US20110147962A1 - Spray-Drying Process - Google Patents

Spray-Drying Process Download PDF

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Publication number
US20110147962A1
US20110147962A1 US12/966,319 US96631910A US2011147962A1 US 20110147962 A1 US20110147962 A1 US 20110147962A1 US 96631910 A US96631910 A US 96631910A US 2011147962 A1 US2011147962 A1 US 2011147962A1
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Prior art keywords
spray
detersive surfactant
process according
dried
slurry
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US12/966,319
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Larry Savio Cardozo
Hossam Hassan Tantawy
James Robert Lickiss
Nigel Patrick Somerville Roberts
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Procter and Gamble Co
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Procter and Gamble Co
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Assigned to THE PROCTER & GAMBLE COMPANY reassignment THE PROCTER & GAMBLE COMPANY ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: CARDOZO, LARRY SAVIO, LICKISS, JAMES ROBERT, TANTAWY, HOSSAM HASSAN, SOMERVILLE ROBERTS, NIGEL PATRICK
Publication of US20110147962A1 publication Critical patent/US20110147962A1/en
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    • GPHYSICS
    • G06COMPUTING; CALCULATING OR COUNTING
    • G06FELECTRIC DIGITAL DATA PROCESSING
    • G06F12/00Accessing, addressing or allocating within memory systems or architectures
    • G06F12/02Addressing or allocation; Relocation
    • G06F12/0223User address space allocation, e.g. contiguous or non contiguous base addressing
    • G06F12/023Free address space management
    • G06F12/0253Garbage collection, i.e. reclamation of unreferenced memory
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/12Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/29Sulfates of polyoxyalkylene ethers
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions
    • C11D11/02Preparation in the form of powder by spray drying
    • GPHYSICS
    • G06COMPUTING; CALCULATING OR COUNTING
    • G06FELECTRIC DIGITAL DATA PROCESSING
    • G06F16/00Information retrieval; Database structures therefor; File system structures therefor
    • G06F16/90Details of database functions independent of the retrieved data types
    • G06F16/95Retrieval from the web
    • G06F16/957Browsing optimisation, e.g. caching or content distillation
    • G06F16/9574Browsing optimisation, e.g. caching or content distillation of access to content, e.g. by caching

Definitions

  • the present invention relates to a spray-drying process.
  • Spray-drying is the standard method for manufacturing laundry detergent base powder.
  • detergent ingredients are mixed together to form an aqueous detergent slurry in a mixer, such as a crutcher mixer.
  • This slurry is then transferred through at least one pump to a spray nozzle, and the slurry is sprayed into a spray-drying tower, and spray-dried to form a spray-dried powder.
  • detergent ingredients and/or the combination of detergent ingredients, can be spray-dried in this manner. This is especially true for alkoxylated anionic detersive surfactants. These surfactants tend to form highly viscous phases in the crutcher mixer; such phases are extremely difficult to handle in the manufacturing plant, leading to poor mixing in the crutcher mixer.
  • the Inventors have found that by reducing, or even removing, alkoxylated anionic detersive surfactant from the aqueous detergent slurry formed in the crutcher mixer, and incorporating the surfactant at a later stage in the process, such as after the mixer and before the spray nozzle, the above problems are overcome.
  • a process for preparing a spray-dried detergent powder comprising (i) detersive surfactant; and (ii) other detergent ingredients; wherein the process comprises the steps of: (a) forming an aqueous detergent slurry in a mixer; (b) transferring the aqueous detergent slurry from the mixer through at least one pump to a spray nozzle; (c) contacting alkoxylated anionic detersive surfactant and/or acid precursor thereof to the aqueous detergent slurry after the mixer and before the spray nozzle to form a mixture; (d) spraying the mixture through the spray nozzle into a spray-drying tower; and (e) spray-drying the mixture to form a spray-dried powder.
  • the process for preparing a spray-dried detergent powder typically comprises the steps of: (a) forming an aqueous detergent slurry in a mixer; (b) transferring the aqueous detergent slurry from the mixer through at least one pump to a spray nozzle; (c) contacting alkoxylated anionic detersive surfactant and/or acid precursor thereof to the aqueous detergent slurry after the mixer and before the spray nozzle to form a mixture; (d) spraying the mixture through the spray nozzle into a spray-drying tower; and (e) spray-drying the mixture to form a spray-dried powder.
  • Step (a): the aqueous detergent slurry can be formed by mixing in any suitable vessel, such as mixer, in the standard manner.
  • suitable mixers include vertical mixers, slurry mixers, tank agitators, crutcher mixers and the like.
  • the aqueous detergent slurry is transferred in a pipe.
  • the aqueous slurry is typically transferred though an intermediate storage vessel such as a drop tank, for example when the process is semi-continuous.
  • the process can be a continuous process, in which case no intermediate storage vessel is required.
  • the aqueous detergent slurry is transferred through at least one pump, preferably at least two, or even at least three or more pumps, although one or two, preferably two pumps may be preferred.
  • the first pump is a low pressure pump, such as a pump that is capable of generating a pressure of from 3 ⁇ 10 5 to 1 ⁇ 10 6 Pa
  • the second pump is a high pressure pump, such as a pump that is capable of generating a pressure of from 2 ⁇ 10 6 to 1 ⁇ 10 7 Pa.
  • the aqueous detergent slurry is transferred through a disintegrator, such as disintegrators supplied by Hosakawa Micron.
  • the disintegrator can be position before the pump, or after the pump. If two or more pumps are present, then the disintegrator can also be positioned between the pumps.
  • the pumps, disintegrators, intermediate storage vessels, if present are all in series configuration. However, some equipment may be in a parallel configuration.
  • a suitable spray nozzle is a Spray Systems T4 Nozzle.
  • the mixture formed in step (c) comprises from 20 wt % to 35 wt % water.
  • Step (c) can be carried out in any position after the mixer and before the spray nozzle. However, preferably step (c) is carried out after the aqueous detergent slurry has been transferred through at least one pump, although step (c) may be carried out before the aqueous detergent slurry has been transferred through at least one pump.
  • the aqueous detergent slurry is transferred through at least two pumps, and step (c) is carried out after the aqueous detergent slurry has been transferred through the first pump but before the aqueous detergent slurry enters the second pump.
  • the pipe is at a pressure of from 3 ⁇ 10 5 to 1 ⁇ 10 6 Pa.
  • step (c) it may be preferred for step (c) to be carried out immediately before the spray nozzle.
  • step (c) it may be preferred that additionally sodium chloride is contacted to the aqueous detergent slurry after the mixer and before the spray nozzle.
  • the mixture is at a temperature of from 60° C. to 130° C. when it is sprayed through the spray nozzle into a spray-drying tower.
  • Suitable spray-drying towers are co-current or counter-current spray-drying towers.
  • the mixture is typically sprayed at a pressure of from 6 ⁇ 10 6 Pa to 1 ⁇ 10 7 Pa.
  • the exhaust air temperature is in the range of from 60° C. to 100° C.
  • the spray-dried detergent powder typically comprises: (i) detersive surfactant; and (ii) other detergent ingredients.
  • the spray-dried detergent powder comprises: (a) from 0 wt % to 10 wt % zeolite builder; (b) from 0 wt % to 10 wt % phosphate builder; and (c) optionally from 0 wt % to 15 wt % silicate salt.
  • the spray-dried detergent powder comprises from 8 wt % to 20 wt % alkoxylated anionic detersive surfactant.
  • the spray-dried detergent powder is suitable for any detergent application, for example: laundry, including automatic washing machine laundering and hand laundering, and even bleach and laundry additives; hard surface cleaning; dish washing, especially automatic dish washing; carpet cleaning and freshening.
  • the spray-dried detergent powder is a spray-dried laundry detergent powder.
  • the spray-dried detergent powder can be a fully formulated detergent product, such as a fully formulated laundry detergent product, or it can be combined with other particles to form a fully formulated detergent product, such as a fully formulated laundry detergent product.
  • the spray-dried laundry detergent particles may be combined with other particles such as: enzyme particles; perfume particles including agglomerates or extrudates of perfume microcapsules, and perfume encapsulates such as starch encapsulated perfume accord particles; surfactant particles, such as non-ionic detersive surfactant particles including agglomerates or extrudates, anionic detersive surfactant particles including agglomerates and extrudates, and cationic detersive surfactant particles including agglomerates and extrudates; polymer particles including soil release polymer particles, cellulosic polymer particles; filler particles including sulphate salt particles, especially sodium sulphate particles; buffer particles including carbonate salt and/or silicate salt particles, preferably a particle comprising carbonate salt and
  • the spray-dried detergent powder comprises: (a) from 15 wt % to 30 wt % detersive surfactant; (b) from 0 wt % to 4 wt % zeolite builder; (c) from 0 wt % to 4 wt % phosphate builder; and (d) optionally from 0 wt % to 15 wt % silicate salt, and wherein in step (c) the alkoxylated anionic detersive surfactant comprises C 8-18 alkyl ethoxylated sulphate having an average degree of ethoxylation of from 0.5 to 3 and/or acid precursor thereof.
  • the spray-dried powder typically comprises from 0 wt % to 7 wt %, preferably from 1 wt % to 5 wt %, and preferably from 2 wt % to 3 wt % water.
  • the spray-dried particle is typically flowable, typically having a cake strength of from 0 N to 20 N, preferably from 0 N to 15 N, more preferably from 0 N to 10 N, most preferably from 0 N to 5 N.
  • the method to determine the cake strength is described in more detail elsewhere in the description.
  • a smooth plastic cylinder of internal diameter 6.35 cm and length 15.9 cm is supported on a suitable base plate.
  • a 0.65 cm hole is drilled through the cylinder with the centre of the hole being 9.2 cm from the end opposite the base plate.
  • a metal pin is inserted through the hole and a smooth plastic sleeve of internal diameter 6.35 cm and length 15.25 cm is placed around the inner cylinder such that the sleeve can move freely up and down the cylinder and comes to rest on the metal pin.
  • the space inside the sleeve is then filled (without tapping or excessive vibration) with the spray-dried powder such that the spray-dried powder is level with the top of the sleeve.
  • a lid is placed on top of the sleeve and a 5 kg weight placed on the lid. The pin is then pulled out and the spray-dried powder is allowed to compact for 2 minutes. After 2 minutes the weight is removed, the sleeve is lowered to expose the powder cake with the lid remaining on top of the powder.
  • a metal probe is then lowered at 54 cm/min such that it contacts the centre of the lid and breaks the cake.
  • the maximum force required to break the cake is recorded and is the result of the test.
  • a cake strength of 0 N refers to the situation where no cake is formed.
  • the aqueous detergent slurry typically comprises detergent ingredients, such as alkalinity source, polymer, builder, detersive surfactant, filler salts and mixtures thereof. However, it may be especially preferred for the aqueous detergent slurry to comprise low levels, or even be free, of detersive surfactant.
  • the aqueous detergent slurry comprises from 0 wt %, or from above 0 wt %, and to 10.2 wt %, preferably to 9 wt %, or to 8 wt %, or to 7 wt %, or to 6 wt %, or to 5 wt %, or to 4 wt %, or to 3 wt %, or to 2 wt %, or to 1 wt % detersive surfactant. It may even be preferred for the aqueous detergent slurry to be essentially free of detersive surfactant. By essentially free of it is typically meant herein to mean: “comprises no deliberately added”.
  • the aqueous detergent slurry may comprise low levels, or even be completely free, of detersive surfactants that are difficult to process when in slurry form and exposed to the residence time and process conditions typically experienced by an aqueous detergent slurry during a conventional spray-drying process, for example in the mixer of step (a), such as a crutcher mixer.
  • detersive surfactants include alkoxylated anionic detersive surfactants which have a tendency to form an undesirable phase when incorporated into an aqueous detergent slurry and exposed to pro-longed residence times.
  • the aqueous detergent slurry formed in step (a) comprises from 0 wt % to 2 wt %, preferably to lwt % alkoxylated anionic detersive surfactant.
  • the aqueous detergent slurry formed in step (a) is essentially free from alkoxylated anionic detersive surfactant. By essentially free from, it is typically meant herein to mean: “comprises no deliberately added”.
  • aqueous detergent slurry may also be especially preferred for the aqueous detergent slurry to comprise low levels, or even be free, of builder.
  • the aqueous detergent slurry comprises from 0 wt % to 10 wt %, or to 9 wt %, or to 8 wt %, or to 7 wt %, or to 6 wt %, or to 5 wt %, or to 4 wt %, or to 3 wt %, or to 2 wt %, or to 1 wt % zeolite builder.
  • the aqueous detergent slurry is essentially free of zeolite builder.
  • the aqueous detergent slurry comprises from 0 wt % to 10 wt %, or to 9 wt %, or to 8 wt %, or to 7 wt %, or to 6 wt %, or to 5 wt %, or to 4 wt %, or to 3 wt %, or to 2 wt %, or to 1 wt % phosphate builder.
  • the aqueous detergent slurry is essentially free of phosphate builder.
  • the aqueous detergent slurry is alkaline.
  • the aqueous detergent slurry has a pH of greater than 7.0, preferably greater than 7.7, or greater than 8.1, or even greater than 8.5, or greater than 9.0, or greater than 9.5, or greater than 10.0, or even greater than 10.5, and preferably to 14, or to 13, or to 12.
  • Suitable detersive surfactants include anionic detersive surfactants, non-ionic detersive surfactant, cationic detersive surfactants, zwitterionic detersive surfactants and amphoteric detersive surfactants.
  • Preferred anionic detersive surfactants include sulphate and sulphonate detersive surfactants.
  • Preferred sulphonate detersive surfactants include alkyl benzene sulphonate, preferably C 10-13 alkyl benzene sulphonate.
  • Suitable alkyl benzene sulphonate (LAS) is obtainable, preferably obtained, by sulphonating commercially available linear alkyl benzene (LAB);
  • suitable LAB includes low 2-phenyl LAB, such as those supplied by Sasol under the tradename Isochem® or those supplied by Petresa under the tradename Petrelab®, other suitable LAB include high 2-phenyl LAB, such as those supplied by Sasol under the tradename Hyblene®.
  • a suitable anionic detersive surfactant is alkyl benzene sulphonate that is obtained by DETAL catalyzed process, although other synthesis routes, such as HF, may also be suitable.
  • Preferred sulphate detersive surfactants include alkyl sulphate, preferably C 8-18 alkyl sulphate, or predominantly C 1-2 alkyl sulphate.
  • alkyl alkoxylated sulphate preferably alkyl ethoxylated sulphate, preferably a C 8-18 alkyl alkoxylated sulphate, preferably a C 8-18 alkyl ethoxylated sulphate, preferably the alkyl alkoxylated sulphate has an average degree of alkoxylation of from 0.5 to 20, preferably from 0.5 to 10, preferably the alkyl alkoxylated sulphate is a C 8-18 alkyl ethoxylated sulphate having an average degree of ethoxylation of from 0.5 to 10, preferably from 0.5 to 7, more preferably from 0.5 to 5 and most preferably from 0.5 to 3.
  • alkyl sulphate, alkyl alkoxylated sulphate and alkyl benzene sulphonates may be linear or branched, substituted or un-substituted.
  • the detersive surfactant may be a mid-chain branched detersive surfactant, preferably a mid-chain branched anionic detersive surfactant, more preferably a mid-chain branched alkyl sulphate and/or a mid-chain branched alkyl benzene sulphonate, most preferably a mid-chain branched alkyl sulphate.
  • the mid-chain branches are C 1-4 alkyl groups, preferably methyl and/or ethyl groups.
  • Suitable non-ionic detersive surfactants are selected from the group consisting of: C 8 -C 18 alkyl ethoxylates, such as, NEODOL® non-ionic surfactants from Shell; C 6 -C 12 alkyl phenol alkoxylates wherein preferably the alkoxylate units are ethyleneoxy units, propyleneoxy units or a mixture thereof; C 12 -C 18 alcohol and C 6 -C 12 alkyl phenol condensates with ethylene oxide/propylene oxide block polymers such as Pluronic® from BASF; C 14 -C 22 mid-chain branched alcohols; C 14 -C 22 mid-chain branched alkyl alkoxylates, preferably having an average degree of alkoxylation of from 1 to 30; alkylpolysaccharides, preferably alkylpolyglycosides; polyhydroxy fatty acid amides; ether capped poly(oxyalkylated) alcohol surfactants; and mixtures thereof.
  • Preferred non-ionic detersive surfactants are alkyl polyglucoside and/or an alkyl alkoxylated alcohol.
  • Preferred non-ionic detersive surfactants include alkyl alkoxylated alcohols, preferably C 8-18 alkyl alkoxylated alcohol, preferably a C 8-18 alkyl ethoxylated alcohol, preferably the alkyl alkoxylated alcohol has an average degree of alkoxylation of from 1 to 50, preferably from 1 to 30, or from 1 to 20, or from 1 to 10, preferably the alkyl alkoxylated alcohol is a C 8-18 alkyl ethoxylated alcohol having an average degree of ethoxylation of from 1 to 10, preferably from 1 to 7, more preferably from 1 to 5 and most preferably from 3 to 7.
  • the alkyl alkoxylated alcohol can be linear or branched, and substituted or un-substituted.
  • Suitable cationic detersive surfactants include alkyl pyridinium compounds, alkyl quaternary ammonium compounds, alkyl quaternary phosphonium compounds, alkyl ternary sulphonium compounds, and mixtures thereof.
  • Preferred cationic detersive surfactants are quaternary ammonium compounds having the general formula:
  • R is a linear or branched, substituted or unsubstituted C 6-18 alkyl or alkenyl moiety
  • R 1 and R 2 are independently selected from methyl or ethyl moieties
  • R 3 is a hydroxyl, hydroxymethyl or a hydroxyethyl moiety
  • X is an anion which provides charge neutrality
  • preferred anions include: halides, preferably chloride; sulphate; and sulphonate.
  • Preferred cationic detersive surfactants are mono-C 6-18 alkyl mono-hydroxyethyl di-methyl quaternary ammonium chlorides.
  • Highly preferred cationic detersive surfactants are mono-C 8-10 alkyl mono-hydroxyethyl di-methyl quaternary ammonium chloride, mono-C 10-12 alkyl mono-hydroxyethyl di-methyl quaternary ammonium chloride and mono-C 10 alkyl mono-hydroxyethyl di-methyl quaternary ammonium chloride.
  • alkoxylated anionic detersive surfactant and/or acid precursor thereof is contacted to the aqueous detergent slurry.
  • the alkoxylated anionic detersive surfactant comprises alkyl ethoxylated sulphate and/or acid precursor thereof.
  • the alkoxylated anionic detersive surfactant comprises C 8-18 alkyl ethoxylated sulphate having an average degree of ethoxylation of from 0.5 to 20, preferably to 10, or to 5, preferably from 0.5 to 3 and/or acid precursor thereof. It may be preferred that in step (c) the alkoxylated anionic detersive surfactant comprises acid precursor of an alkyl ethoxylated sulphate.
  • Suitable zeolite builder includes include zeolite A, zeolite P and zeolite MAP. Especially suitable is zeolite 4 A.
  • a typical phosphate builder is sodium tri-polyphosphate.
  • a suitable silicate salt is sodium silicate, preferably 1.6 R and/or 2.0 R sodium silicate.
  • the composition typically comprises other detergent ingredients.
  • Suitable detergent ingredients include: transition metal catalysts; imine bleach boosters; enzymes such as amylases, carbohydrases, cellulases, laccases, lipases, bleaching enzymes such as oxidases and peroxidases, proteases, pectate lyases and mannanases; source of peroxygen such as percarbonate salts and/or perborate salts, preferred is sodium percarbonate, the source of peroxygen is preferably at least partially coated, preferably completely coated, by a coating ingredient such as a carbonate salt, a sulphate salt, a silicate salt, borosilicate, or mixtures, including mixed salts, thereof; bleach activator such as tetraacetyl ethylene diamine, oxybenzene sulphonate bleach activators such as nonanoyl oxybenzene sulphonate, caprolactam bleach activators, imide bleach activators such as N-nonanoyl-N
  • Aqueous slurry Component (parts) Sodium Silicate 8.5 Acrylate/maleate copolymer 3.2 Hydroxyethane di(methylene phosphonic acid) 0.6 Sodium carbonate 8.8 Sodium sulphate 42.9 Water 19.7 Miscellaneous, such as magnesium sulphate, and one 1.7 or more stabilizers Aqueous alkaline slurry parts 85.4
  • An alkaline aqueous slurry having the composition as described above is prepared in a slurry making vessel (crutcher).
  • the alkaline aqueous slurry is shear thinning and has a viscosity in the range of from 0.5 to 30 Pas at a temperature of 70° C. and at a shear rate of 50 s ⁇ 1 .
  • the moisture content of the above slurry is 23.1%. Any ingredient added above in liquid form is heated to 70° C., such that the aqueous slurry is never at a temperature below 70° C.
  • Saturated steam at a pressure of 6.0 ⁇ 10 5 Pa is injected into the crutcher to raise the temperature to 90° C.
  • the slurry is then pumped into a low pressure line (having a pressure of 5.0 ⁇ 10 5 Pa).
  • a low pressure line having a pressure of 5.0 ⁇ 10 5 Pa.
  • 1.14 parts of ethoxylated C 12-18 alkyl alcohol sulphate anionic detersive surfactant having an average degree of ethoxylation of 1 (AE 1 S), 10.26 parts of C 8 -C 24 alkyl benzene sulphonic acid (HLAS), and 3.2 parts of a 50w/w % aqueous sodium hydroxide solution are pumped into the low pressure line.
  • the viscosity of the alkaline slurry increases.
  • the resultant mixture is then pumped by a high pressure pump into a high pressure line (having an exit pressure of 8.0 ⁇ 10 6 Pa).
  • the mixture is then sprayed at a rate of 1,640 kg/hour at a pressure of 8.0 ⁇ 10 6 Pa and at a temperature of 90° C.+/ ⁇ 2° C. through a spray pressure nozzle into a counter current spray-drying tower with an air inlet temperature of 300° C.
  • the mixture is atomised and the atomised slurry is dried to produce a solid mixture, which is then cooled and sieved to remove oversize material (>1.8 mm) to form a spray-dried powder, which is free-flowing.
  • Fine material ( ⁇ 0.15 mm) is elutriated with the exhaust the exhaust air in the spray-drying tower and collected in a post tower containment system.
  • the spray-dried powder has a moisture content of 2.5 wt %, a bulk density of 510 g/l and a particle size distribution such that greater than 80 wt % of the spray-dried powder has a particle size of from 150 to 710 micrometers.
  • the composition of the spray-dried powder is given below.
  • the above laundry detergent composition was prepared by dry-mixing all of the above particles (all except the AE7) in a standard batch mixer.
  • the AE7 in liquid form is sprayed on the particles in the standard batch mixer.
  • the AE7 in liquid form is sprayed onto the spray-dried powder of example 1.
  • the resultant powder is then mixed with all of the other particles in a standard batch mixer.

Abstract

A process for preparing a spray-dried detergent powder having (i) detersive surfactant; and (ii) other detergent ingredients; wherein the process comprises the steps of: (a) forming an aqueous detergent slurry in a mixer; (b) transferring the aqueous detergent slurry from the mixer through at least one pump to a spray nozzle; (c) contacting alkoxylated anionic detersive surfactant and/or acid precursor thereof to the aqueous detergent slurry after the mixer and before the spray nozzle to form a mixture; (d) spraying the mixture through the spray nozzle into a spray-drying tower; and (e) spray-drying the mixture to form a spray-dried powder.

Description

    FIELD OF THE INVENTION
  • The present invention relates to a spray-drying process.
  • BACKGROUND OF THE INVENTION
  • Spray-drying is the standard method for manufacturing laundry detergent base powder. Typically, detergent ingredients are mixed together to form an aqueous detergent slurry in a mixer, such as a crutcher mixer. This slurry is then transferred through at least one pump to a spray nozzle, and the slurry is sprayed into a spray-drying tower, and spray-dried to form a spray-dried powder.
  • However, there are limitation on which detergent ingredients, and/or the combination of detergent ingredients, can be spray-dried in this manner. This is especially true for alkoxylated anionic detersive surfactants. These surfactants tend to form highly viscous phases in the crutcher mixer; such phases are extremely difficult to handle in the manufacturing plant, leading to poor mixing in the crutcher mixer.
  • The Inventors have found that by reducing, or even removing, alkoxylated anionic detersive surfactant from the aqueous detergent slurry formed in the crutcher mixer, and incorporating the surfactant at a later stage in the process, such as after the mixer and before the spray nozzle, the above problems are overcome.
  • SUMMARY OF THE INVENTION
  • A process for preparing a spray-dried detergent powder comprising (i) detersive surfactant; and (ii) other detergent ingredients; wherein the process comprises the steps of: (a) forming an aqueous detergent slurry in a mixer; (b) transferring the aqueous detergent slurry from the mixer through at least one pump to a spray nozzle; (c) contacting alkoxylated anionic detersive surfactant and/or acid precursor thereof to the aqueous detergent slurry after the mixer and before the spray nozzle to form a mixture; (d) spraying the mixture through the spray nozzle into a spray-drying tower; and (e) spray-drying the mixture to form a spray-dried powder.
  • DETAILED DESCRIPTION OF THE INVENTION Process for Preparing a Spray-Dried Detergent Powder
  • The process for preparing a spray-dried detergent powder typically comprises the steps of: (a) forming an aqueous detergent slurry in a mixer; (b) transferring the aqueous detergent slurry from the mixer through at least one pump to a spray nozzle; (c) contacting alkoxylated anionic detersive surfactant and/or acid precursor thereof to the aqueous detergent slurry after the mixer and before the spray nozzle to form a mixture; (d) spraying the mixture through the spray nozzle into a spray-drying tower; and (e) spray-drying the mixture to form a spray-dried powder.
  • Step (a): the aqueous detergent slurry can be formed by mixing in any suitable vessel, such as mixer, in the standard manner. Suitable mixers include vertical mixers, slurry mixers, tank agitators, crutcher mixers and the like.
  • Step (b): the aqueous detergent slurry is transferred from the mixer through at least one pump to a spray nozzle. Typically, the aqueous detergent slurry is transferred in a pipe. The aqueous slurry is typically transferred though an intermediate storage vessel such as a drop tank, for example when the process is semi-continuous. Alternatively, the process can be a continuous process, in which case no intermediate storage vessel is required. The aqueous detergent slurry is transferred through at least one pump, preferably at least two, or even at least three or more pumps, although one or two, preferably two pumps may be preferred. Typically, when two or more pumps are used, the first pump is a low pressure pump, such as a pump that is capable of generating a pressure of from 3×105 to 1×106 Pa, and the second pump is a high pressure pump, such as a pump that is capable of generating a pressure of from 2×106 to 1×107 Pa. Optionally, the aqueous detergent slurry is transferred through a disintegrator, such as disintegrators supplied by Hosakawa Micron. The disintegrator can be position before the pump, or after the pump. If two or more pumps are present, then the disintegrator can also be positioned between the pumps. Typically, the pumps, disintegrators, intermediate storage vessels, if present, are all in series configuration. However, some equipment may be in a parallel configuration. A suitable spray nozzle is a Spray Systems T4 Nozzle.
  • Step (c): alkoxylated anionic detersive surfactant and/or acid precursor thereof is contacted to the aqueous detergent slurry after the mixer and before the spray nozzle to form a mixture. Preferably, the mixture formed in step (c) comprises from 20 wt % to 35 wt % water. Step (c) can be carried out in any position after the mixer and before the spray nozzle. However, preferably step (c) is carried out after the aqueous detergent slurry has been transferred through at least one pump, although step (c) may be carried out before the aqueous detergent slurry has been transferred through at least one pump. In a preferred embodiment, the aqueous detergent slurry is transferred through at least two pumps, and step (c) is carried out after the aqueous detergent slurry has been transferred through the first pump but before the aqueous detergent slurry enters the second pump. Preferably, during step (c) the pipe is at a pressure of from 3×105 to 1×106 Pa. However, it may be preferred for step (c) to be carried out immediately before the spray nozzle.
  • In step (c), it may be preferred that additionally sodium chloride is contacted to the aqueous detergent slurry after the mixer and before the spray nozzle.
  • Step (d): the mixture formed in step (c) is sprayed through the spray nozzle into a spray-drying tower. Preferably, the mixture is at a temperature of from 60° C. to 130° C. when it is sprayed through the spray nozzle into a spray-drying tower. Suitable spray-drying towers are co-current or counter-current spray-drying towers. The mixture is typically sprayed at a pressure of from 6×106 Pa to 1×107 Pa.
  • Step (e): the mixture is spray-dried to form a spray-dried powder. Preferably, the exhaust air temperature is in the range of from 60° C. to 100° C.
  • Spray-Dried Detergent Powder
  • The spray-dried detergent powder typically comprises: (i) detersive surfactant; and (ii) other detergent ingredients. Highly preferably, the spray-dried detergent powder comprises: (a) from 0 wt % to 10 wt % zeolite builder; (b) from 0 wt % to 10 wt % phosphate builder; and (c) optionally from 0 wt % to 15 wt % silicate salt. Most preferably, the spray-dried detergent powder comprises from 8 wt % to 20 wt % alkoxylated anionic detersive surfactant.
  • The spray-dried detergent powder is suitable for any detergent application, for example: laundry, including automatic washing machine laundering and hand laundering, and even bleach and laundry additives; hard surface cleaning; dish washing, especially automatic dish washing; carpet cleaning and freshening. However, highly preferably, the spray-dried detergent powder is a spray-dried laundry detergent powder.
  • The spray-dried detergent powder can be a fully formulated detergent product, such as a fully formulated laundry detergent product, or it can be combined with other particles to form a fully formulated detergent product, such as a fully formulated laundry detergent product. The spray-dried laundry detergent particles may be combined with other particles such as: enzyme particles; perfume particles including agglomerates or extrudates of perfume microcapsules, and perfume encapsulates such as starch encapsulated perfume accord particles; surfactant particles, such as non-ionic detersive surfactant particles including agglomerates or extrudates, anionic detersive surfactant particles including agglomerates and extrudates, and cationic detersive surfactant particles including agglomerates and extrudates; polymer particles including soil release polymer particles, cellulosic polymer particles; filler particles including sulphate salt particles, especially sodium sulphate 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, especially coated percarbonate particles, including carbonate and/or sulphate coated percarbonate, silicate coated percarbonate, borosilicate coated percarbonate, sodium perborate coated percarbonate; bleach catalyst particles, such as transition metal catalyst bleach particles, and imine bleach boosting particles; performed peracid particles; hueing dye particles; and any mixture thereof.
  • In a highly preferred embodiment of the present invention, the spray-dried detergent powder comprises: (a) from 15 wt % to 30 wt % detersive surfactant; (b) from 0 wt % to 4 wt % zeolite builder; (c) from 0 wt % to 4 wt % phosphate builder; and (d) optionally from 0 wt % to 15 wt % silicate salt, and wherein in step (c) the alkoxylated anionic detersive surfactant comprises C8-18 alkyl ethoxylated sulphate having an average degree of ethoxylation of from 0.5 to 3 and/or acid precursor thereof.
  • The spray-dried powder typically comprises from 0 wt % to 7 wt %, preferably from 1 wt % to 5 wt %, and preferably from 2 wt % to 3 wt % water.
  • The spray-dried particle is typically flowable, typically having a cake strength of from 0 N to 20 N, preferably from 0 N to 15 N, more preferably from 0 N to 10 N, most preferably from 0 N to 5 N. The method to determine the cake strength is described in more detail elsewhere in the description.
  • Method for Measuring Cake Strength
  • A smooth plastic cylinder of internal diameter 6.35 cm and length 15.9 cm is supported on a suitable base plate. A 0.65 cm hole is drilled through the cylinder with the centre of the hole being 9.2 cm from the end opposite the base plate.
  • A metal pin is inserted through the hole and a smooth plastic sleeve of internal diameter 6.35 cm and length 15.25 cm is placed around the inner cylinder such that the sleeve can move freely up and down the cylinder and comes to rest on the metal pin. The space inside the sleeve is then filled (without tapping or excessive vibration) with the spray-dried powder such that the spray-dried powder is level with the top of the sleeve. A lid is placed on top of the sleeve and a 5 kg weight placed on the lid. The pin is then pulled out and the spray-dried powder is allowed to compact for 2 minutes. After 2 minutes the weight is removed, the sleeve is lowered to expose the powder cake with the lid remaining on top of the powder.
  • A metal probe is then lowered at 54 cm/min such that it contacts the centre of the lid and breaks the cake. The maximum force required to break the cake is recorded and is the result of the test. A cake strength of 0 N refers to the situation where no cake is formed.
  • Aqueous Detergent Slurry
  • The aqueous detergent slurry typically comprises detergent ingredients, such as alkalinity source, polymer, builder, detersive surfactant, filler salts and mixtures thereof. However, it may be especially preferred for the aqueous detergent slurry to comprise low levels, or even be free, of detersive surfactant. Preferably, the aqueous detergent slurry comprises from 0 wt %, or from above 0 wt %, and to 10.2 wt %, preferably to 9 wt %, or to 8 wt %, or to 7 wt %, or to 6 wt %, or to 5 wt %, or to 4 wt %, or to 3 wt %, or to 2 wt %, or to 1 wt % detersive surfactant. It may even be preferred for the aqueous detergent slurry to be essentially free of detersive surfactant. By essentially free of it is typically meant herein to mean: “comprises no deliberately added”.
  • It may be highly advantageous for the aqueous detergent slurry to comprise low levels, or even be completely free, of detersive surfactants that are difficult to process when in slurry form and exposed to the residence time and process conditions typically experienced by an aqueous detergent slurry during a conventional spray-drying process, for example in the mixer of step (a), such as a crutcher mixer. Such detersive surfactants include alkoxylated anionic detersive surfactants which have a tendency to form an undesirable phase when incorporated into an aqueous detergent slurry and exposed to pro-longed residence times. Preferably, the aqueous detergent slurry formed in step (a) comprises from 0 wt % to 2 wt %, preferably to lwt % alkoxylated anionic detersive surfactant. Preferably, the aqueous detergent slurry formed in step (a) is essentially free from alkoxylated anionic detersive surfactant. By essentially free from, it is typically meant herein to mean: “comprises no deliberately added”.
  • It may also be especially preferred for the aqueous detergent slurry to comprise low levels, or even be free, of builder.
  • Preferably, the aqueous detergent slurry comprises from 0 wt % to 10 wt %, or to 9 wt %, or to 8 wt %, or to 7 wt %, or to 6 wt %, or to 5 wt %, or to 4 wt %, or to 3 wt %, or to 2 wt %, or to 1 wt % zeolite builder. Preferably, the aqueous detergent slurry is essentially free of zeolite builder.
  • Preferably, the aqueous detergent slurry comprises from 0 wt % to 10 wt %, or to 9 wt %, or to 8 wt %, or to 7 wt %, or to 6 wt %, or to 5 wt %, or to 4 wt %, or to 3 wt %, or to 2 wt %, or to 1 wt % phosphate builder. Preferably, the aqueous detergent slurry is essentially free of phosphate builder.
  • Preferably the aqueous detergent slurry is alkaline. Preferably, the aqueous detergent slurry has a pH of greater than 7.0, preferably greater than 7.7, or greater than 8.1, or even greater than 8.5, or greater than 9.0, or greater than 9.5, or greater than 10.0, or even greater than 10.5, and preferably to 14, or to 13, or to 12.
  • Detersive Surfactant
  • Suitable detersive surfactants include anionic detersive surfactants, non-ionic detersive surfactant, cationic detersive surfactants, zwitterionic detersive surfactants and amphoteric detersive surfactants.
  • Preferred anionic detersive surfactants include sulphate and sulphonate detersive surfactants.
  • Preferred sulphonate detersive surfactants include alkyl benzene sulphonate, preferably C10-13 alkyl benzene sulphonate. Suitable alkyl benzene sulphonate (LAS) is obtainable, preferably obtained, by sulphonating commercially available linear alkyl benzene (LAB); suitable LAB includes low 2-phenyl LAB, such as those supplied by Sasol under the tradename Isochem® or those supplied by Petresa under the tradename Petrelab®, other suitable LAB include high 2-phenyl LAB, such as those supplied by Sasol under the tradename Hyblene®. A suitable anionic detersive surfactant is alkyl benzene sulphonate that is obtained by DETAL catalyzed process, although other synthesis routes, such as HF, may also be suitable.
  • Preferred sulphate detersive surfactants include alkyl sulphate, preferably C8-18 alkyl sulphate, or predominantly C1-2 alkyl sulphate.
  • Another preferred sulphate detersive surfactant is alkyl alkoxylated sulphate, preferably alkyl ethoxylated sulphate, preferably a C8-18 alkyl alkoxylated sulphate, preferably a C8-18 alkyl ethoxylated sulphate, preferably the alkyl alkoxylated sulphate has an average degree of alkoxylation of from 0.5 to 20, preferably from 0.5 to 10, preferably the alkyl alkoxylated sulphate is a C8-18 alkyl ethoxylated sulphate having an average degree of ethoxylation of from 0.5 to 10, preferably from 0.5 to 7, more preferably from 0.5 to 5 and most preferably from 0.5 to 3.
  • The alkyl sulphate, alkyl alkoxylated sulphate and alkyl benzene sulphonates may be linear or branched, substituted or un-substituted.
  • The detersive surfactant may be a mid-chain branched detersive surfactant, preferably a mid-chain branched anionic detersive surfactant, more preferably a mid-chain branched alkyl sulphate and/or a mid-chain branched alkyl benzene sulphonate, most preferably a mid-chain branched alkyl sulphate. Preferably, the mid-chain branches are C1-4 alkyl groups, preferably methyl and/or ethyl groups.
  • Suitable non-ionic detersive surfactants are selected from the group consisting of: C8-C18 alkyl ethoxylates, such as, NEODOL® non-ionic surfactants from Shell; C6-C12 alkyl phenol alkoxylates wherein preferably the alkoxylate units are ethyleneoxy units, propyleneoxy units or a mixture thereof; C12-C18 alcohol and C6-C12 alkyl phenol condensates with ethylene oxide/propylene oxide block polymers such as Pluronic® from BASF; C14-C22 mid-chain branched alcohols; C14-C22 mid-chain branched alkyl alkoxylates, preferably having an average degree of alkoxylation of from 1 to 30; alkylpolysaccharides, preferably alkylpolyglycosides; polyhydroxy fatty acid amides; ether capped poly(oxyalkylated) alcohol surfactants; and mixtures thereof.
  • Preferred non-ionic detersive surfactants are alkyl polyglucoside and/or an alkyl alkoxylated alcohol.
  • Preferred non-ionic detersive surfactants include alkyl alkoxylated alcohols, preferably C8-18 alkyl alkoxylated alcohol, preferably a C8-18 alkyl ethoxylated alcohol, preferably the alkyl alkoxylated alcohol has an average degree of alkoxylation of from 1 to 50, preferably from 1 to 30, or from 1 to 20, or from 1 to 10, preferably the alkyl alkoxylated alcohol is a C8-18 alkyl ethoxylated alcohol having an average degree of ethoxylation of from 1 to 10, preferably from 1 to 7, more preferably from 1 to 5 and most preferably from 3 to 7. The alkyl alkoxylated alcohol can be linear or branched, and substituted or un-substituted.
  • Suitable cationic detersive surfactants include alkyl pyridinium compounds, alkyl quaternary ammonium compounds, alkyl quaternary phosphonium compounds, alkyl ternary sulphonium compounds, and mixtures thereof.
  • Preferred cationic detersive surfactants are quaternary ammonium compounds having the general formula:

  • (R)(R1)(R2)(R3)N+X
  • wherein, R is a linear or branched, substituted or unsubstituted C6-18 alkyl or alkenyl moiety, R1 and R2 are independently selected from methyl or ethyl moieties, R3 is a hydroxyl, hydroxymethyl or a hydroxyethyl moiety, X is an anion which provides charge neutrality, preferred anions include: halides, preferably chloride; sulphate; and sulphonate. Preferred cationic detersive surfactants are mono-C6-18 alkyl mono-hydroxyethyl di-methyl quaternary ammonium chlorides. Highly preferred cationic detersive surfactants are mono-C8-10 alkyl mono-hydroxyethyl di-methyl quaternary ammonium chloride, mono-C10-12 alkyl mono-hydroxyethyl di-methyl quaternary ammonium chloride and mono-C10 alkyl mono-hydroxyethyl di-methyl quaternary ammonium chloride.
  • Alkoxylated Anionic Detersive Surfactant and/or Acid Precursor Thereof
  • In step (c) of the process, alkoxylated anionic detersive surfactant and/or acid precursor thereof is contacted to the aqueous detergent slurry. Preferably, in step (c) the alkoxylated anionic detersive surfactant comprises alkyl ethoxylated sulphate and/or acid precursor thereof. Preferably, in step (c) the alkoxylated anionic detersive surfactant comprises C8-18 alkyl ethoxylated sulphate having an average degree of ethoxylation of from 0.5 to 20, preferably to 10, or to 5, preferably from 0.5 to 3 and/or acid precursor thereof. It may be preferred that in step (c) the alkoxylated anionic detersive surfactant comprises acid precursor of an alkyl ethoxylated sulphate.
  • Zeolite Builder
  • Suitable zeolite builder includes include zeolite A, zeolite P and zeolite MAP. Especially suitable is zeolite 4 A.
  • Phosphate Builder
  • A typical phosphate builder is sodium tri-polyphosphate.
  • Silicate Salt
  • A suitable silicate salt is sodium silicate, preferably 1.6 R and/or 2.0 R sodium silicate.
  • Other Detergent Ingredients
  • The composition typically comprises other detergent ingredients. Suitable detergent ingredients include: transition metal catalysts; imine bleach boosters; enzymes such as amylases, carbohydrases, cellulases, laccases, lipases, bleaching enzymes such as oxidases and peroxidases, proteases, pectate lyases and mannanases; source of peroxygen such as percarbonate salts and/or perborate salts, preferred is sodium percarbonate, the source of peroxygen is preferably at least partially coated, preferably completely coated, by a coating ingredient such as a carbonate salt, a sulphate salt, a silicate salt, borosilicate, or mixtures, including mixed salts, thereof; bleach activator such as tetraacetyl ethylene diamine, oxybenzene sulphonate bleach activators such as nonanoyl oxybenzene sulphonate, caprolactam bleach activators, imide bleach activators such as N-nonanoyl-N-methyl acetamide, preformed peracids such as N,N-pthaloylamino peroxycaproic acid, nonylamido peroxyadipic acid or dibenzoyl peroxide; suds suppressing systems such as silicone based suds suppressors and/or fatty acid based suds suppressors; brighteners; hueing agents; photobleach; fabric-softening agents such as clay, silicone and/or quaternary ammonium compounds; flocculants such as polyethylene oxide; dye transfer inhibitors such as polyvinylpyrrolidone, poly 4-vinylpyridine N-oxide and/or co-polymer of vinylpyrrolidone and vinylimidazole; fabric integrity components such as oligomers produced by the condensation of imidazole and epichlorhydrin; soil dispersants and soil anti-redeposition aids such as alkoxylated polyamines and ethoxylated ethyleneimine polymers; anti-redeposition components such as polyesters and/or terephthalate polymers, polyethylene glycol including polyethylene glycol substituted with vinyl alcohol and/or vinyl acetate pendant groups; perfumes such as perfume microcapsules, polymer assisted perfume delivery systems including Schiff base perfume/polymer complexes, starch encapsulated perfume accords; soap rings; aesthetic particles including coloured noodles and/or needles; dyes; fillers such as sodium sulphate, although it may be preferred for the composition to be substantially free of fillers; carbonate salt including sodium carbonate and/or sodium bicarbonate; silicate salt such as sodium silicate, including 1.6 R and 2.0 R sodium silicate, or sodium metasilicate; co-polyesters of di-carboxylic acids and diols; cellulosic polymers such as methyl cellulose, carboxymethyl cellulose, hydroxyethoxycellulose, or other alkyl or alkylalkoxy cellulose, and hydrophobically modified cellulose; carboxylic acid and/or salts thereof, including citric acid and/or sodium citrate; and any combination thereof.
  • EXAMPLES Example 1 A Spray-Dried Laundry Detergent Powder and Process of Making it Aqueous Alkaline Slurry Composition.
  • Aqueous slurry
    Component (parts)
    Sodium Silicate 8.5
    Acrylate/maleate copolymer 3.2
    Hydroxyethane di(methylene phosphonic acid) 0.6
    Sodium carbonate 8.8
    Sodium sulphate 42.9
    Water 19.7
    Miscellaneous, such as magnesium sulphate, and one 1.7
    or more stabilizers
    Aqueous alkaline slurry parts 85.4
  • Preparation of a Spray-Dried Laundry Detergent Powder.
  • An alkaline aqueous slurry having the composition as described above is prepared in a slurry making vessel (crutcher). The alkaline aqueous slurry is shear thinning and has a viscosity in the range of from 0.5 to 30 Pas at a temperature of 70° C. and at a shear rate of 50 s−1. The moisture content of the above slurry is 23.1%. Any ingredient added above in liquid form is heated to 70° C., such that the aqueous slurry is never at a temperature below 70° C. Saturated steam at a pressure of 6.0×105 Pa is injected into the crutcher to raise the temperature to 90° C. The slurry is then pumped into a low pressure line (having a pressure of 5.0×105 Pa). Separately, 1.14 parts of ethoxylated C12-18 alkyl alcohol sulphate anionic detersive surfactant having an average degree of ethoxylation of 1 (AE1S), 10.26 parts of C8-C24 alkyl benzene sulphonic acid (HLAS), and 3.2 parts of a 50w/w % aqueous sodium hydroxide solution are pumped into the low pressure line. The viscosity of the alkaline slurry increases. The resultant mixture is then pumped by a high pressure pump into a high pressure line (having an exit pressure of 8.0×106 Pa). The mixture is then sprayed at a rate of 1,640 kg/hour at a pressure of 8.0×106 Pa and at a temperature of 90° C.+/−2° C. through a spray pressure nozzle into a counter current spray-drying tower with an air inlet temperature of 300° C. The mixture is atomised and the atomised slurry is dried to produce a solid mixture, which is then cooled and sieved to remove oversize material (>1.8 mm) to form a spray-dried powder, which is free-flowing. Fine material (<0.15 mm) is elutriated with the exhaust the exhaust air in the spray-drying tower and collected in a post tower containment system. The spray-dried powder has a moisture content of 2.5 wt %, a bulk density of 510 g/l and a particle size distribution such that greater than 80 wt % of the spray-dried powder has a particle size of from 150 to 710 micrometers. The composition of the spray-dried powder is given below.
  • Spray-Dried Laundry Detergent Powder Composition
  • % w/w Spray Dried
    Component Powder
    Ethoxylated C12-18 alkyl alcohol sulphate anionic 1.5
    detersive surfactant having an average degree of
    ethoxylation of 1 (AE1S)
    Sodium silicate salt 10.0
    C8-C24 alkyl benzene sulphonate 13.6
    Acrylate/maleate copolymer 4.0
    Hydroxyethane di(methylene phosphonic acid) 0.7
    Sodium carbonate 11.9
    Sodium sulphate 53.7
    Water 2.5
    Miscellaneous, such as magnesium sulphate, and 2.1
    one or more stabilizers
    Total Parts 100.00
  • A Granular Laundry Detergent Composition.
  • % w/w granular laundry
    Component detergent composition
    Spray-dried powder of example 1 (described above) 59.38
    91.6 wt % active linear alkyl benzene sulphonate flake supplied 0.22
    by Stepan under the tradename Nacconol 90G ®
    Citric acid 5.00
    Sodium percarbonate (having from 12% to 15% active AvOx) 14.70
    Photobleach particle 0.01
    Lipase (11.00 mg active/g) 0.70
    Amylase (21.55 mg active/g) 0.33
    Protease (56.00 mg active/g) 0.43
    Tetraacetyl ethylene diamine agglomerate (92 wt % active) 4.35
    Suds suppressor agglomerate (11.5 wt % active) 0.87
    Acrylate/maleate copolymer particle (95.7 wt % active) 0.29
    Green/Blue carbonate speckle 0.50
    Sodium Sulphate 9.59
    Solid perfume particle 0.63
    Ethoxylated C12-C18 alcohol having an average degree of 3.00
    ethoxylation of 7 (AE7)
    Total Parts 100.00
  • The above laundry detergent composition was prepared by dry-mixing all of the above particles (all except the AE7) in a standard batch mixer. The AE7 in liquid form is sprayed on the particles in the standard batch mixer. Alternatively, the AE7 in liquid form is sprayed onto the spray-dried powder of example 1. The resultant powder is then mixed with all of the other particles in a standard batch mixer.
  • The dimensions and values disclosed herein are not to be understood as being strictly limited to the exact numerical values recited. Instead, unless otherwise specified, each such dimension is intended to mean both the recited value and a functionally equivalent range surrounding that value. For example, a dimension disclosed as “40 mm” is intended to mean “about 40 mm”.
  • Every document cited herein, including any cross referenced or related patent or application, is hereby incorporated herein by reference in its entirety unless expressly excluded or otherwise limited. The citation of any document is not an admission that it is prior art with respect to any invention disclosed or claimed herein or that it alone, or in any combination with any other reference or references, teaches, suggests or discloses any such invention. Further, to the extent that any meaning or definition of a term in this document conflicts with any meaning or definition of the same term in a document incorporated by reference, the meaning or definition assigned to that term in this document shall govern.
  • While particular embodiments of the present invention have been illustrated and described, it would be obvious to those skilled in the art that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.

Claims (13)

1. A process for preparing a spray-dried detergent powder comprising
(i) detersive surfactant; and
(ii) other detergent ingredients;
wherein the process comprises the steps of:
(a) forming an aqueous detergent slurry in a mixer;
(b) transferring the aqueous detergent slurry from the mixer through at least one pump to a spray nozzle;
(c) contacting alkoxylated anionic detersive surfactant and/or acid precursor thereof to the aqueous detergent slurry after the mixer and before the spray nozzle to form a mixture;
(d) spraying the mixture through the spray nozzle into a spray-drying tower; and
(e) spray-drying the mixture to form a spray-dried powder.
2. A process according to claim 1, wherein in step (c) the alkoxylated anionic detersive surfactant comprises alkyl ethoxylated sulphate and/or acid precursor thereof.
3. A process according to claim 1, wherein in step (c) the alkoxylated anionic detersive surfactant comprises C8-18 alkyl ethoxylated sulphate having an average degree of ethoxylation of from about 0.5 to about 3 and/or an acid precursor thereof.
4. A process according to claim 1, wherein in step (c) the alkoxylated anionic detersive surfactant comprises acid precursor of an alkyl ethoxylated sulphate.
5. A process according to claim 1, wherein in step (c) additionally sodium chloride is contacted to the aqueous detergent slurry after the mixer and before the spray nozzle.
6. A process according to claim 1, wherein the aqueous detergent slurry comprises from about 0 wt % to about 5 wt % detersive surfactant.
7. A process according to claim 1, wherein the spray-dried detergent powder comprises:
(a) from about 0 wt % to about 10 wt % zeolite builder;
(b) from about 0 wt % to about 10 wt % phosphate builder; and
(c) optionally from about 0 wt % to about 15 wt % silicate salt.
8. A process according to claim 1, wherein the aqueous detergent slurry formed in step (a) comprises from about 0 wt % to about 2 wt % alkoxylated anionic detersive surfactant.
9. A process according to claim 1, wherein the spray-dried detergent powder comprises from about 8 wt % to about 20 wt % alkoxylated anionic detersive surfactant.
10. A process according to claim 1, wherein in step (d) the mixture is at a temperature of from about 60° C. to about 130° C. when it is sprayed through the spray nozzle into a spray-drying tower.
11. A process according to claim 1, wherein the mixture formed in step (c) comprises from about 20 wt % to about 35 wt % water.
12. A process according to claim 1, wherein the spray-dried detergent powder is spray-dried laundry detergent powder.
13. A process according to claim 1, wherein the spray-dried detergent powder comprises
(a) from about 15 wt % to about 30 wt % detersive surfactant;
(b) from about 0 wt % to about 4 wt % zeolite builder;
(c) from about 0 wt % to about 4 wt % phosphate builder; and
(d) optionally from about 0 wt % to about 15 wt % silicate salt,
wherein in step (c) the alkoxylated anionic detersive surfactant comprises C8-18 alkyl ethoxylated sulphate having an average degree of ethoxylation of from about 0.5 to about 3 and/or an acid precursor thereof.
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US7842657B2 (en) * 2008-06-25 2010-11-30 The Procter & Gamble Company Spray-drying process
US7811980B1 (en) * 2009-06-09 2010-10-12 The Procter & Gamble Company Spray-drying process
US20110146099A1 (en) * 2009-12-18 2011-06-23 Larry Savio Cardozo Spray-Drying Process
US20110147964A1 (en) * 2009-12-18 2011-06-23 Larry Savio Cardozo Spray-Drying Process
US20110147963A1 (en) * 2009-12-18 2011-06-23 Larry Savio Cardozo Spray-Drying Process

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* Cited by examiner, † Cited by third party
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US20110147963A1 (en) * 2009-12-18 2011-06-23 Larry Savio Cardozo Spray-Drying Process
US20110147964A1 (en) * 2009-12-18 2011-06-23 Larry Savio Cardozo Spray-Drying Process
US20110146099A1 (en) * 2009-12-18 2011-06-23 Larry Savio Cardozo Spray-Drying Process
US8361357B2 (en) 2009-12-18 2013-01-29 The Procter & Gamble Company Spray-drying process
US8435936B2 (en) 2009-12-18 2013-05-07 The Procter & Gamble Company Spray-drying process
US8568629B2 (en) 2009-12-18 2013-10-29 The Procter & Gamble Company Spray-Drying process
US20130320575A1 (en) * 2012-06-01 2013-12-05 The Procter & Gamble Company Spray-drying process
US8901065B2 (en) * 2012-06-01 2014-12-02 The Procter & Gamble Company Spray-drying process
CN104364007A (en) * 2012-06-01 2015-02-18 宝洁公司 Spray-drying process
CN104364007B (en) * 2012-06-01 2017-02-22 宝洁公司 Spray-drying process
WO2022243343A1 (en) 2021-05-19 2022-11-24 Unilever Ip Holdings B.V. Process for preparing a spray dried detergent particle

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US9582418B2 (en) 2017-02-28
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