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
  • 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
  • C11D11/0088—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 the liquefied ingredients being sprayed or adsorbed onto solid 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
  • 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
• • 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

Definitions

• the present invention generally relates to a process for producing a low density detergent composition More particularly, the invention is directed to a process dunng which low density detergent agglomerates are produced by feeding a surfactant paste or liquid acid precursor of anionic surfactant and dry starting detergent matenal sequentially into two high speed mixers followed by a fluid bed dryer which has an optimally selected nozzle height for spraying on a binder
• the process produces a free flowing, low density detergent composition which can be commercially sold as a conventional non-compact detergent composition or used as an admix in a low dosage, "compact" detergent product BACKGROUND OF THE INVENTION
• the first type of process involves spray-drying an aqueous detergent slurry in a spray-drying tower to produce highly porous detergent granules.
• the va ⁇ ous detergent components are dry mixed after which they are agglomerated with a binder such as a nonionic or anionic surfactant.
• a binder such as a nonionic or anionic surfactant.
• Marume ⁇ zer® This apparatus comprises a substantially horizontal, roughened, rotatable table positioned withm and at the base of a substantially vertical, smooth walled cylinder
• This process is essentially a batch process and is therefore less suitable for the large scale production of detergent powders
• other attempts have been made to provide continuous processes for increasing the density of "post-tower” or spray d ⁇ ed detergent granules
• such processes require a first apparatus which pulve ⁇ zes or g ⁇ nds the granules and a second apparatus which increases the density of the pulve ⁇ zed granules by agglomeration While these processes achieve the desired increase in density by treating or densifying "post tower” or spray d ⁇ ed granules, they do not provide a process which has the flexibility of providing lower density granules.
• Patent No. 4,900,466 (Lever); France et al, U.S. Patent No. 5,576,285 (Procter & Gamble); and Dhalewadika et al, PCT WO 96/04359 (Unilever).
• the present invention meets the aforementioned needs in the art by providing a process which produces a low density (below about 600 g/1) detergent composition directly from a surfactant paste and dry starting detergent ingredients.
• the process involves agglomerating the starting detergent ingredients in a high speed mixer followed by a second high speed mixer. Thereafter, the agglomerates formed in the high speed mixers are agglomerated and dried in a fluid bed dryer in which a liquid binder is sprayed onto the agglomerates from one or more nozzles at a selected height from the distribution plate of the fluid bed dryer.
• the process does not use the conventional spray drying towers currently used and is therefore more efficient, economical and flexible with regard to the variety of detergent compositions which can be produced in the process. Moreover, the process is more amenable to environmental concerns in that it does not use spray drying towers which typically emit particulates and volatile organic compounds into the atmosphere.
• agglomerates refers to particles formed by agglomerating detergent granules or particles which typically have a smaller median particle size than the formed agglomerates.
• median particle size it is meant the particle size diameter value above which 50% of the particles have a larger particle size and below which 50% of particles have a smaller particle size. All percentages used herein are expressed as “percent-by-weight" on an anhydrous basis unless indicated otherwise.
• a process for preparing low density detergent agglomerates comprises the steps of: (a) agglomerating a detergent surfactant paste or precursor thereof and dry starting detergent material in a first high speed mixer to obtain agglomerates; (b) mixing the agglomerates in a second high speed mixer to obtain built-up agglomerates; and (c) feeding the built-up agglomerates into a fluid bed dryer in which a binder is sprayed via a nozzle having a height of from about 25 cm to about 60 cm from the distributor plate of the fluid bed dryer such that the built-up agglomerates are dried and agglomerated to form the low detergent agglomerates having a density in a range from about 300 g/1 to about 550 g/1
• another process for prepa ⁇ ng low density detergent agglomerates is provided The process comp ⁇ ses the steps of (a) agglomerating a detergent surfact
• the present invention is directed to a process m which low density agglomerates are produced by a three step process, the last of which involves a fluid bed dryer containing one or more nozzles positioned at a selected height from the distnbution plate of the dryer.
• the process forms free flowing, low density detergent agglomerates which can be used alone as the detergent product or as an admixture with conventional spray-dned detergent granules and/or high density detergent agglomerates in a final commercial detergent product.
• the process desc ⁇ bed herein can be operated continuously or in a batch mode depending upon the particularly desired application.
• One major advantage of the present process is that it utilizes equipment which can be operated differently from the present process parameters to obtain high density detergent compositions.
• a single large-scale commercial detergent manufactunng facility can be built to produce high or low density detergent compositions depending upon the local consumer demand and its inevitable fluctuations between compact and non- compact detergent products.
• a detergent surfactant paste or precursor thereof as set forth in more detail hereinafter and dry starting detergent matenal is inputted and agglomerated in a high speed mixer
• the dry starting matenal can include only those relatively inexpensive detergent materials typically used in modern granular detergent products
• Such ingredients include but are not limited to, builders, fillers, dry surfactants, and flow aides
• the builder includes aluminosi cates, crystalline layered silicates, phosphates, carbonates and mixtures thereof which is the essential dry starting detergent ingredient within the scope of the current process Relatively expensive materials such as Burkeite (Na2S ⁇ 4 «Na2C ⁇ 3) and the various silicas are not necessary to achieve the desired low density agglomerates produced by the process Rather, by selecting the binder and nozzle height through which the binder is sprayed onto the agglomerates in the fluid bed dryer as descnbed in more detail hereinafter, the present process achieve
• the first step of the process it is preferable to include from 1% to about 40% by weight of undersized detergent particles or "fines" in the first step of the process. This can be conveniently accomplished by screening the detergent particles formed subsequent to the fluid bed dryer to a median particle size range of from about 10 microns to about 150 microns and feeding these "fines" back into the first high speed mixer.
• the high speed mixer can be any one of a vanety of commercially available mixers such as a Lodige CB 30 mixer or similar brand mixer.
• These types of mixers essentially consist of a honzontal, hollow static cylinder having a centrally mounted rotating shaft around which several shovel and rod-shaped blades are attached which have a tip speed of from about 5 m/s to about 30 m/s, more preferably from about 6 m/s to about 26 m/s
• the shaft rotates at a speed of from about 100 rpm to about 2500 rpm, more preferably from about 300 rpm to about 1600 rpm.
• the mean residence time of the detergent ingredients in the high speed mixer is preferably m range from about 2 seconds to about 45 seconds, and most preferably from about 5 seconds to about 15 seconds.
• This mean residence time is conveniently measured by dividing the weight of the mixer at steady state by throughput (kg/hr) flow.
• Another suitable mixer is any one of the vanous Flexomix models available from Schugi (Netherlands) which are vertically positioned high speed mixers. This type of mixer is preferably operated at a Froude Index of from about 13 to about 32. See U.S. Patent 5,149,455 to Jacobs et al (issued September 22, 1992) for a detailed discussion of this well-known Froude Index which is a dimensionless number that can be optimally selected by those skilled in the art.
• a liquid acid precursor of an anionic surfactant is inputted with the dry starting detergent matenal which at least includes a neutralizing agent such as sodium carbonate
• the preferred liquid acid surfactant precursor is C ⁇ ⁇ _ ⁇ g linear alkylbenzene sulfonate surfactant ("HLAS"), although any acid precursor ot an anionic surfactant may be used m the process
• a more preferred embodiment involves feeding a liquid acid precursor of C i2-14 linear alkylbenzene sulfonate surfactant with a Xo-18 a lkyl ethoxylated sulfate (“AS”) surfactant into the first high speed mixer, preferably in a weight ratio of from about 5 1 to about 1 5, and most preferably, in a range of from about 1 1 to about 3 1 (HLAS AS)
• the result of such mixing is a "dry neutralization" reaction between the HLAS and the sodium carbonate embodied in the dry starting detergent material, all of which forms agglomer
• the built-up agglomerates are inputted into a fluid bed dryer in which the agglomerates are dned and agglomerated to a median particle size of from about 300 microns to about 700 microns, more preferably from about 325 microns to about 450 microns
• the density of the agglomerates formed is from about 300 g/1 to about 550 g/1, more preferably from about 350 g/1 to about 500 g/1, and even more preferably from about 400 g/1 to about 480 g/1 All of these densities are generally below that of typical detergent compositions formed of dense agglomerates or most typical spray-dned granules.
• a binder as descnbed previously is preferably added dunng this step to enhance formation of the desired agglomerates
• a particularly preferred binder is liquid sodium silicate in an amount of from about 0 1% to about 20% by weight of the final low density composition
• the nozzle height through which the binder is added is preferably from about 25 cm to about 60 cm, more preferably from about 30 cm to about 60 cm, most preferably from about 40 cm to about 60 cm, and even more preferably at 40 cm, from the dist ⁇ bution plate of the fluid bed dryer
• Preferably all of the nozzles used in the fluid bed drying apparatus have such a height arrangement
• the benefits of the process in this regard can be enhanced by maintaining the spray-on flux of the binder in the fluid bed to be from about 0.02 kg. c ⁇ Xhr to about 0.06 kg/cm ⁇ /hr, more preferably from about 0.04 kg/cnXhr to about 0.05 kg/cm ⁇ /hr.
• the air inlet temperature in the fluid bed dryer is from about 100°C to about 200°C, more preferably from about 110°C to about 130°C.
• the unfluidized bed height in fluid bed dryer is preferably from about 5 cm to about 20 cm.
• the process benefits can be enhanced by maintaining the fluidized air flux in the fluid bed dryer is from about 0.6 kg/m ⁇ /s to about 0.8 kg/m ⁇ /s. It has also been found beneficial to add the binder simultaneously at more than one location in one or more of the steps of the process.
• the liquid silicate can be added at two locations in the fluid bed dryer, e.g., at or near the inlet port and at or near the exit port.
• the median binder droplet diameter is from about 20 microns to about 150 microns, a parameter which enhances formation of the desired built-up agglomerates.
• the ratio of the median binder droplet diameter to built-up agglomerate (exiting the second high speed mixer) particle diameter is preferably from about 0.1 to about 0.6.
• the process may involve adding the binder to both the second high speed mixer as well as the fluid bed dryer. It has also been found beneficial to add the binder simultaneously at more than one location in one or more of the steps of the process.
• the liquid silicate can be added at two locations in the fluid bed dryer, e.g., at or near the inlet port and at or near the exit port.
• the agglomerates are built-up from smaller sizes to large sized particles having a high degree of intraparticle porosity.
• the degree of intraparticle porosity is preferably from about 20% to about 40%, and most preferably from about 25% to about 35%.
• the intraparticle porosity can be conveniently measured by standard mercury porosimetry testing.
• optional steps contemplated by the present process include screening the oversized detergent agglomerates in a screening apparatus which can take a variety of forms including but not limited to conventional screens chosen for the desired particle size of the finished detergent product.
• Other optional steps include conditioning of the detergent agglomerates by subjecting the agglomerates to additional drying and/or cooling by way of apparatus discussed previously.
• Another optional step of the instant process entails finishing the resulting detergent agglomerates by a variety of processes including spraying and/or admixing other conventional detergent ingredients.
• the finishing step encompasses spraying perfumes, brighteners and enzymes onto the finished agglomerates to provide a more complete detergent composition.
• Such techniques and ingredients are well known in the art.
• the liquid acid precursor of anionic surfactant is used in the first step of the process, and in optional embodiments, as a liquid binder in the second and/or third essential steps of the process
• This liquid acid precursor will typically have a viscosity measured at 30°C of from about 500 cps to about 5,000 cps
• the liquid acid is a precursor for the anionic surfactants desc ⁇ bed in more detail hereinafter
• a detergent surfactant paste can also be used m the process and is preferably in the form of an aqueous viscous paste, although other forms are also contemplated by the invention
• This so-called viscous surfactant paste has a viscosity of from about 5,000 cps to about 100,000 cps, more preferably from about 10,000 cps to about 80,000 cps, and contains at least about 10% water, more preferably at least about 20% water
• the viscosity is measured at 70°C and at shear rates of about 10 to 100 sec "' Furthermore, the sur
• the surfactant itself, in the viscous surfactant paste, is preferably selected from anionic, nonionic, zwitte ⁇ onic, ampholytic and cationic classes and compatible mixtures thereof
• Detergent surfactants useful herein are descnbed m U S. Patent 3,664,961, Norns, issued May 23, 1972, and m U S. Patent 3,919,678, Laughlm et al., issued December 30, 1975, both of which are incorporated herein by reference.
• Useful cationic surfactants also include those descnbed in U.S. Patent 4,222,905, Cockrell, issued September 16, 1980, and m U S. Patent 4,239,659, Murphy, issued December 16, 1980, both of which are also incorporated herein by reference.
• amonics and nomonics are preferred and amonics are most preferred.
• Nonhmitmg examples of the preferred anionic surfactants useful in the surfactant paste, or from which the liquid acid precursor descnbed herein denves include the conventional C ⁇ ⁇ -C ⁇ alkyl benzene sulfonates ("LAS"), p ⁇ mary, branched-chain and random CI Q-C20 alkyl sulfates ("AS"), the CJQ-CI g secondary (2,3) alkyl sulfates of the formula CH 3 (CH2) x (CHOS0 3 " M + ) CH 3 and CH 3 (CH 2 ) y (CHOS0 3 " M + ) CH 2 CH 3 where x and (y + 1) are integers of at least about 7, preferably at least about 9, and M is a 510 water-solubilizmg cation, especially sodium, unsaturated sulfates such as oleyl sulfate, and the Cio-Ci g alkyl alkoxy sulfates ("AE X S"; especially
• exemplary surfactants useful m the paste of the invention include and C10-C18 alkyl alkoxy carboxylates (especially the EO 1-5 ethoxycarboxylates), the ClO-18 gly cer ol ethers, the CI Q-CI. g alkyl polyglycosides and their corresponding sulfated polyglycosides, and C12-C1 g alpha-sulfonated fatty acid esters.
• the conventional nonionic and amphotenc surfactants such as the Ci 2-C1 g alkyl ethoxylates ("AE") including the so-called narrow peaked alkyl ethoxylates and alkyl phenol alkoxylates (especially ethoxylates and mixed ethoxy/propoxy), C12-C 1 g betaines and sulfobetaines ("sultames”), I Q-C I g amine oxides, and the like, can also be included in the overall compositions.
• the Cj -C ⁇ N-alkyl polyhydroxy fatty acid amides can also be used. Typical examples include the C ⁇ -Cj N-methylglucamides. See WO 9,206,154.
• sugar-derived surfactants include the N-alkoxy polyhydroxy fatty acid amides, such as X0-C1 8 N-(3-methoxypropyl) glucamide.
• the N-propyl through N-hexyl C ⁇ -C j glucamides can be used for low sudsing.
• C 10X20 conventional soaps may also be used. If high sudsing is desired, the branched-chain C J Q-C I g soaps may be used. Mixtures of anionic and nonionic surfactants are especially useful.
• Other conventional useful surfactants are listed m standard texts.
• the starting dry detergent material of the present process preferably compnses a builder and other standard detergent ingredients such as sodium carbonate, especially when a liquid acid precursor of a surfactant is used as it is needed as a neutralizing agent in the first step of the process.
• preferable starting dry detergent matenal includes sodium carbonate and a phosphate or an alummosi cate builder which is referenced as an alummosilicate ion exchange material.
• a preferred builder is selected from the group consisting of aluminosihcates, crystalline layered silicates, phosphates, carbonates and mixtures thereof.
• Preferred phosphate builders include sodium t ⁇ polyphosphate, tetrasodium pyrophosphate and mixtures thereof.
• inorganic phosphate builders are sodium and potassium tnpolyphosphate, pyrophosphate, polymenc metaphosphate having a degree of polymerization of from about 6 to 21, and orthophosphates.
• polyphosphonate builders are the sodium and potassium salts of ethylene diphosphonic acid, the sodium and potassium salts of ethane 1-hydroxy-l, 1 -diphosphonic acid and the sodium and potassium salts of ethane, 1 , 1 ,2-t ⁇ phosphon ⁇ c acid.
• Other phosphorus builder compounds are disclosed in U.S. Patents 3,159,581; 3,213,030; 3,422,021; 3,422,137; 3,400,176 and 3,400,148, all of which are incorporated herein by reference.
• the aluminosilicate ion exchange materials used herein as a detergent builder preferably have both a high calcium ion exchange capacity and a high exchange rate. Without intending to be limited by theory, it is believed that such high calcium ion exchange rate and capacity are a function of several interrelated factors which denve from the method by which the aluminosilicate ion exchange material is produced.
• the aluminosilicate ion exchange materials used herein are preferably produced in accordance with Corkill et al, U.S. Patent No. 4,605,509 (Procter & Gamble), the disclosure of which is incorporated herein by reference.
• the aluminosilicate ion exchange material is in "sodium" form since the potassium and hydrogen forms of the instant aluminosilicate do not exhibit the as high of an exchange rate and capacity as provided by the sodium form.
• the aluminosilicate ion exchange material preferably is in over dned form so as to facilitate production of c ⁇ sp detergent agglomerates as described herein.
• the aluminosilicate ion exchange materials used herein preferably have particle size diameters which optimize their effectiveness as detergent builders.
• particle size diameter represents the average particle size diameter of a given aluminosilicate ion exchange material as determined by conventional analytical techniques, such as microscopic determination and scanning electron microscope (SEM).
• the preferred particle size diameter of the aluminosilicate is from about 0.1 micron to about 10 microns, more preferably from about 0.5 microns to about 9 microns. Most preferably, the particle size diameter is from about 1 microns to about 8 microns.
• the aluminosilicate ion exchange matenal has the formula Na z [(A10 2 ) z .(Si ⁇ 2) y ]xH 2 0 wherein z and y are integers of at least 6, the molar ratio of z to y is from about 1 to about 5 and x is from about 10 to about 264. More preferably, the aluminosilicate has the formula
• aluminosilicates are available commercially, for example under designations Zeolite A, Zeolite B and Zeolite X.
• Naturally-occurnng or synthetically derived aluminosilicate ion exchange materials suitable for use herein can be made as descnbed in Krummel et al, U.S. Patent No. 3,985,669, the disclosure of which is incorporated herein by reference.
• the aluminosilicates used herein are further charactenzed by their ion exchange capacity which is at least about 200 mg equivalent of CaC0 3 hardness/gram, calculated on an anhydrous basis, and which is preferably in a range from about 300 to 352 mg equivalent of CaC0 3 hardness/gram.
• the instant aluminosilicate ion exchange materials are still further charactenzed by their calcium ion exchange rate which is at least about 2 grains Ca "H" /gallon/m ⁇ nute/-gram gallon, and more preferably in a range from about 2 grains Ca "H 7gallon/minute/-gram/gallon to about 6 grains Ca ++ /gallon minute/-gram/gallon .
• Adjunct Detergent Ingredients The starting dry detergent material in the present process can include additional detergent ingredients and/or, any number of additional ingredients can be incorporated in the detergent composition during subsequent steps of the present process.
• adjunct ingredients include other detergency builders, bleaches, bleach activators, suds boosters or suds suppressors, anti-tarnish and anticorrosion agents, soil suspending agents, soil release agents, germicides, pH adjusting agents, non-builder alkalinity sources, chelatmg agents, smectite clays, enzymes, enzyme-stabilizing agents and perfumes See U S Patent 3,936,537, issued February 3, 1976 to Baskerville, Jr et al , incorporated herein by reference
• Other builders can be generally selected from the va ⁇ ous borates, polyhydroxy sulfonates, polyacetates, carboxylates, citrates, tartrate mono- and di-succinates, and mixtures thereof Preferred are the alkali metal, especially sodium, salts of the above In companson with amorphous sodium silicates, crystalline layered sodium silicates exhibit a clearly increased calcium and magnesium ion exchange capacity In addition, the layered sodium silicates prefer magnesium ions over calcium ions, a feature necessary to insure that substantially all of the "hardness" is removed from the wash water These crystalline layered sodium silicates, however, are generally more expensive than amorphous silicates as well as other builders. Accordingly, in order to provide an economically feasible laundry detergent, the proportion of crystalline layered sodium silicates used must be determined judiciously
• the crystalline layered sodium silicates suitable for use herein preferably have the formula NaMS ⁇ x 0 2x + ⁇ yH 2 0 wherein M is sodium or hydrogen, x is from about 1.9 to about 4 and y is from about 0 to about 20. More preferably, the crystalline layered sodium silicate has the formula
• nonphosphorus, inorganic builders are tetraborate decahydrate and silicates having a weight ratio of S ⁇ Ofact to alkali metal oxide of from about 0.5 to about 4 0, preferably from about 1.0 to about 2.4.
• Water-soluble, nonphosphorus organic builders useful herein include the vanous alkali metal, ammonium and substituted ammonium polyacetates, carboxylates, polycarboxylates and polyhydroxy sulfonates.
• polyacetate and polycarboxylate builders are the sodium, potassium, lithium, ammonium and substituted ammonium salts of ethylene diamme tetraacetic acid, nit ⁇ lot ⁇ acetic acid, oxydisuccinic acid, mel tic acid, benzene polycarboxy c acids, and cit ⁇ c acid
• Polymenc polycarboxylate builders are set forth in U.S. Patent 3,308,067, Diehl, issued March 7, 1967, the disclosure of which is incorporated herein by reference.
• Such matenals include the water-soluble salts of homo- and copolymers of aliphatic carboxyhc acids such as maleic acid, ltacomc acid, mesaconic acid, fuma ⁇ c acid, acomtic acid, citraconic acid and methylene malomc acid Some of these materials are useful as the water-soluble anionic polymer as hereinafter described, but only if in intimate admixture with the non-soap anionic surfactant
• Other suitable polycarboxylates for use herein are the polyacetal carboxylates desc ⁇ bed in U S Patent 4,144,226, issued March 13, 1979 to Crutchfield et al, and U S Patent 4,246,495, issued March 27, 1979 to Crutchfield et al, both of which are incorporated herein by reference
• These polyacetal carboxylates can be prepared by b ⁇ nging together under polymenzation conditions an ester of glyoxy c acid and a polymerization initiator The resulting polyacetal carb
• Bleaching agents and activators are desc ⁇ bed in U S. Patent 4,412,934, Chung et al., issued November 1, 1983, and in U.S. Patent 4,483,781, Hartman, issued November 20, 1984, both of which are incorporated herein by reference.
• Chelatmg agents are also desc ⁇ bed in U.S. Patent 4,663,071, Bush et al., from Column 17, line 54 through Column 18, line 68, incorporated herein by reference.
• Suds modifiers are also optional ingredients and are descnbed in U.S. Patents 3,933,672, issued January 20, 1976 to Bartoletta et al., and 4,136,045, issued January 23, 1979 to Gault et al., both incorporated herein by reference.
• Suitable smectite clays for use herein are descnbed m U.S. Patent 4,762,645,
• EXAMPLE This Example illustrates the process invention in which a low density agglomerated detergent composition is prepared.
• a Lodige CB 30 high speed mixer is charged with a mixture of powders, namely sodium carbonate (median particle size 15 microns) and sodium t ⁇ polyphosphate ("STPP") with a median particle size of 25 microns
• the mixer is operated at 1600 rpm and the sodium carbonate, STPP, HLAS and AES are formed into agglomerates having a median particle size of about 110 microns after a mean residence time in the Lodig
• a HLAS binder is inputted into the Schugi (Model # FX160) mixer dunng this step which results in built-up agglomerates having a median particle size of about 180 microns being formed Thereafter, the built-up agglomerates are passed through a four-zone fluid bed dryer which is operated at an air inlet temperature of about 125°C and a nozzle height of 40 cm from the distribution plate m the first and fourth zones of the fluid bed
• the spray-on flux of the sodium silicate in 0.04 kg/cm ⁇ /hr, the unfluidized bed height is 10 cm, and the fluidized air flux is 0.6 kg/ ⁇ Xs.
• fines are also added to the Lodige CB 30 mixer.
• liquid sodium silicate is fed into the fluid bed dryer resulting in the finished detergent agglomerates having a density of about 485 g/1 and a median particle size of about 360 microns.
• the finished agglomerates have excellent physical properties in that they are free flowing as exhibited by their supenor cake strength grades.
• the composition of the agglomerates are given below in Table I.
• the agglomerates embody about 14% of fines (less than 150 microns) which are recycled from the fluid bed back into the Lodige CB 30 which enhances production of the agglomerates produced by the process.

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