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
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/12—Water-insoluble compounds
  • C11D3/1213—Oxides or hydroxides, e.g. Al2O3, TiO2, CaO or Ca(OH)2
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/02—Anionic compounds
  • C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
  • C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
  • C11D1/146—Sulfuric acid esters
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/02—Anionic compounds
  • C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
  • C11D1/22—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/02—Anionic compounds
  • C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
  • C11D1/29—Sulfates of polyoxyalkylene ethers
• • 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
  • C11D11/02—Preparation in the form of powder by spray drying
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/12—Water-insoluble compounds
  • C11D3/1233—Carbonates, e.g. calcite or dolomite
• • 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
  • C11D3/12—Water-insoluble compounds
  • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
  • C11D3/1246—Silicates, e.g. diatomaceous earth
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
  • C11D2111/10—Objects to be cleaned
  • C11D2111/12—Soft surfaces, e.g. textile

Definitions

• the present invention relates to a process for preparing a particulate, free flowing detergent particle by a slurry making and spray drying technique.
• the spray-dried particle is suitable for use as a solid laundry detergent composition, or for incorporation into a solid laundry detergent composition.
• granular laundry detergent composition is prepared by spray-drying.
• the laundry detergent components such as surfactants and builders are mixed with around 20% to 50% by weight water to form an aqueous slurry, the aqueous slurry is maintained at temperatures ranging from 60°C to 85°C and then spray-dried in a spray-drying tower.
• Carbonate salts and silicate salts provide a wash liquor with desired pH of about 10.5.
• carbonate salt and silicate salt also function as effective builders to sequester calcium and magnesium ions present in water.
• presence of carbonate salt provides good physical attributes to the spray-dried detergent particle. Such physical characteristics include lower caking tendency and good flowability of the powder during extended shelf storage period. Any reduction in the levels of carbonate salt will directly affect the abovementioned properties.
• Silicate salt which is typically a sodium salt of silicate is generally considered a critical ingredient in spray dried particulate detergent compositions and serves to provide stability and integrity to the detergent particles formed during the spray-drying operation. Attempts at reducing or eliminating sodium silicate have caused deterioration of flow properties and the spray-dried particles were found to be prone to caking. Lowering the silicate levels also impact the viscosity and flow behaviour of the slurry and it was observed that the slurry was difficult to pump due to gelation of slurry.
• US 2002/0123450 A1 discloses a process for preparing a base particle which involves a step of spray drying a slurry having zeolite, water soluble salt and a surfactant in an amount of 5 wt.% by weight of the slurry or less.
• the zeolite in the process may be obtained by mixing an aluminium source in presence of an alkaline earth metal compound.
• the spray dried detergent particle according to the present invention incorporates optimum amounts of alkaline builders, particularly alkali metal silicate, alkali metal carbonate or mixtures thereof.
• alkaline builders particularly alkali metal silicate, alkali metal carbonate or mixtures thereof.
• the spray-dried detergent particle has good powder properties and is free-flowing even after extended storage period.
• spray-dried detergent particle has lowered reserve alkalinity levels while maintaining the pH levels required for optimum cleaning performance thereby providing better fabric care benefits.
• the process according to the present invention provides a spray-dried detergent particle which in presence of low levels of carbonate builder provides good storage stability, good powder properties and is less harsh on the hands or on the fabric.
• the low levels of carbonate builder ensures that the spray-dried detergent particle is less harsh on the hands and when prepared according to the process of the present invention having a solubilized aluminium hydrate provides good powder properties in addition to maintaining good cleaning performance.
• the spray-dried particle has low no phosphate builder.
• a process for preparing a spray dried detergent particle comprising the steps of:
• an alkaline builder selected from the group consisting of (i) alkali metal carbonate salt (ii) alkali metal silicate salt or mixtures thereof to form an aqueous slurry; wherein the aqueous slurry comprises a solubilized aluminium hydrate, detersive surfactant, and alkaline builder; and wherein the alkali builder comprises from 3 wt.% to 25 wt.% alkali metal carbonate salt and wherein the aqueous slurry has a pH ranging from 10 to 12,
• the reserve alkalinity of the spray-dried detergent particle to pH 10 is from 1.5 to 5 grams NaOH/100g. Preferably less than 5.0 grams NaOH/100g, preferably less than 4 grams NaOH/100g, still preferably 3.5 grams NaOH/100g, further preferably less than 2 grams NaOH/100g.
• a process for preparing a spray-dried detergent particle comprising the steps as described herein below.
• the first aspect of the present invention disclosed is a process of solubilizing aluminium hydrate by contacting the aluminium hydrate with an alkaline source in an aqueous mixture.
• aluminium hydrate is preferably preformed or formed in-situ. Aluminium hydrate is commercially available in solid form from various suppliers, the preformed aluminium hydrate comprises 99 wt.% to 100 wt.% aluminium hydrate. Aluminium hydrate may also be available in the form of a pre-dissolved solution.
• the alkaline source is an alkali metal hydroxide, alkali metal silicate, alkali metal carbonate or mixtures thereof.
• the alkaline source is an alkali metal hydroxide, still preferably sodium hydroxide.
• the sodium hydroxide is in the form of an aqueous solution having a solid content ranging from 30 wt.% to 50 wt.%.
• Sodium Hydroxide may also be in solid form which can be pre diluted to form a solution of Sodium hydroxide before addition to the aqueous mixture.
• aluminium hydrate is solubilized in an aqueous mixture by adding an alkaline source wherein the pH of the aqueous mixture after addition of the alkaline source ranges from 12 to 14. It is essential that the pH of the aqueous mixture is from 12 to 14 for solubilizing the aluminium hydrate in the aqueous mixture.
• Aqueous mixture :
• the aqueous mixture comprises a detersive surfactant.
• Suitable detersive surfactant includes anionic, nonionic, cationic, amphoteric, zwitterionic detersive surfactant or mixtures thereof.
• Suitable detersive surfactant may be linear or branched, substituted or un-substituted.
• the detersive surfactant may be derived from petrochemical material or is bioderived.
• the detersive surfactant present in the aqueous mixture is an anionic surfactant.
• Anionic detersive surfactant The aqueous mixture preferably includes an anionic detersive surfactant.
• the partly neutralized anionic surfactant is preferably prepared by a neutralization process which involves the step of mixing a liquid acid form of the anionic surfactant and a neutralizing agent to form a partially neutralized solution; preferably the neutralizing agent is an alkali metal hydroxide, more preferably sodium hydroxide, wherein the amount of alkali metal hydroxide neutralizing agent is sufficient to react with a portion of liquid acid anionic surfactant precursor to form in-situ anionic surfactant salt.
• the neutralizing agent is an alkali metal hydroxide, more preferably sodium hydroxide, wherein the amount of alkali metal hydroxide neutralizing agent is sufficient to react with a portion of liquid acid anionic surfactant precursor to form in-situ anionic surfactant salt.
• the neutralized anionic surfactant formed by neutralizing the acid form with the alkali metal hydroxide neutralizing agent preferably contributes from 28 parts to 98 parts of the total anionic surfactant by weight present in the spray-dried particle.
• the remaining unreacted acid form of the anionic surfactant reacts with the alkaline source to form fully neutralized salt form of the anionic surfactant.
• a fully neutralized anionic surfactant is added to the aqueous mixture.
• the liquid acid anionic surfactant precursor is reacted with an alkali metal hydroxide to form fully neutralized anionic surfactant salt before addition to the aqueous mixture.
• the liquid acid precursor of the anionic surfactant is partly or fully neutralized in-situ. It is most preferred that the detersive surfactant is present when the aluminium hydrate is solubilized by adding an alkaline source. The order of addition is to contact the preneutralized detersive surfactant or the acid detersive surfactant precursor with water followed by adding the alkaline source and then adding the aluminium hydrate.
• the part or full neutralization may be carried out in the same vessel by contacting the acid precursor form of the anionic surfactant with an aqueous solution of neutralizing agent (alkali metal hydroxide) to form the neutralized anionic surfactant salt.
• the detersive surfactant is an anionic surfactant.
• Suitable anionic detersive surfactant include sulphonate and sulphate surfactant.
• Suitable sulphonate surfactant include methyl ester sulphonate, alpha olefin sulphonate, alkyl benzene sulphonate, especially alkyl benzene sulphonate, preferably C10 to C14 alkyl benzene sulphonate.
• Suitable sulphate surfactant includes alkyl sulphate, preferably Cs to C18 alkyl sulphate, or predominantly C12 to C18 alkyl sulphate.
• a preferred sulphate detersive surfactant is alkyl alkoxylated sulphate, preferably alkyl ethoxylated sulphate, preferably a Cs to Cis alkyl alkoxylated sulphate, preferably a Cs to Cis 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 Cs to Cis alkyl ethoxylated sulphate having an average degree of ethoxylation of from 0.5 to 10, preferably from 0.5 to 5, more preferably from 0.5 to 3 and most preferably from 0.5 to 1.5.
• the alkyl sulphate, alkyl alkoxylated sulphate and alkyl benzene sulphonate may be linear or branched, substituted or un-substituted and may be derived from petrochemical material or biomaterial.
• suitable anionic detersive surfactants include, soaps, alkyl ether carboxylates.
• suitable anionic detersive surfactants may be in salt form, suitable counter-ions include sodium, calcium, magnesium, amino alcohols, and any combinations thereof. A preferred counterion is sodium.
• One or more anionic surfactant may be present in the spray-dried detergent particle.
• Suitable non-ionic detersive surfactants are selected from the group consisting of: Cs to Cis alkyl ethoxylates, such as, NEODOL® non-ionic surfactants from Shell; Cs to C12 alkyl phenol alkoxylates wherein preferably the alkoxylate units are ethyleneoxy units, propyleneoxy units or a mixture thereof; C12 to C18 alcohol and Ce to C12 alkyl phenol condensates with ethylene oxide/propylene oxide block polymers such as Pluronic® from BASF; alkyl polysaccharides, preferably alkyl polyglycosides; methyl ester ethoxylates; polyhydroxy fatty acid amides; ether capped poly(oxyalkylated) alcohol surfactants and mixtures thereof.
• Cs to Cis alkyl ethoxylates such as, NEODOL® non-ionic surfactants from Shell
• Cs to C12 alkyl phenol alkoxylates wherein preferably
• Suitable non-ionic detersive surfactants are alkyl polyglucoside and/or an alkyl alkoxylated alcohol.
• Suitable non-ionic detersive surfactants include alkyl alkoxylated alcohols, preferably Cs to Cis alkyl alkoxylated alcohol, preferably a Cs to Cis 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 Cs to Cis 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 nonionic detersive surfactants include secondary alcohol-
• Zwitterionic surfactant Suitable zwitterionic detersive surfactants include amine oxides and/or betaines.
• One or more detersive surfactant may be present in the spray-dried particle according to the present invention.
• the surfactant preferably includes those which are thermally stable during processing conditions of a spray-drying tower with inlet air temperature ranging from 250°C to 500°C and those which are chemically stable at the pH conditions typically present in a spray-drying slurry.
• Non-limiting examples of the anionic surfactant includes the ones mentioned above.
• the aqueous slurry includes LAS.
• the detersive surfactant present in the aqueous slurry is a combination of LAS and alkyl ether sulphate, still preferably a combination of LAS and SLES (1 EO to 3EO).
• the aqueous mixture may also preferably include a combination of anionic surfactant and non-ionic surfactant as the co-surfactant.
• the aqueous mixture includes i) preferably 5 wt.% to 45 wt.% detersive surfactant; ii) 0.8 wt.% to 4.8 wt.% aluminium hydrate; iii) preferably 7 wt.% to 31 wt.% alkali metal silicate salt; iv) 0 wt.% carbonate salt; v) 50 wt.% to 60 wt.% water.
• the aqueous mixture includes aluminium hydrate in solubilized form.
• the solubility of aluminium hydrate in the aqueous mixture is more than 0.0001 g/mL under room conditions.
• aluminium hydrate is solubilized in the aqueous mixture by adding an alkaline source wherein the pH of the aqueous mixture after addition of the alkaline source is in the range from 12 to 14.
• the pH range from 12 to 14 provides for solubilizing the aluminium hydrate in the aqueous mixture.
• the aqueous mixture includes less than 3 wt.% organic acid
• organic acid include those selected from the group consisting of hydroxycarboxylic acid, polycarboxylic acid or mixtures thereof. More preferably the aqueous mixture includes less than 1 wt.% organic acid, still preferably 0 wt.% organic acid.
• the organic acid generally used in laundry composition includes tartaric acid, citric acid, malic acid, glycolic acid or lactic acid, more commonly the organic acid is citric acid.
• the next step involves adding an alkaline builder to the aqueous mixture to form an aqueous slurry comprising the solubilized aluminium hydrate, alkaline builder and a detersive surfactant.
• the alkaline builder is selected from the group consisting of alkali metal carbonate, alkali metal silicate or mixtures thereof.
• Alkali metal carbonate builder
• the aqueous slurry includes from 3 wt.% to 15 wt.% alkali metal carbonate builder, still preferably from 3 wt.% to 13 wt.% alkali metal carbonate builder.
• the amount of alkali metal carbonate builder in the aqueous slurry is not less than 3 wt.%, still preferably not less than 5 wt.%, more preferably not less than 8 wt.%, still more preferably not less than 10 wt.%, but typically not more than 14 wt.%, preferably not more than 13.5 wt.% or still preferably not more than 13 wt.%.
• the alkaline builder may be an alkali metal silicate salt builder.
• the alkali metal silicate is a soluble silicate. Soluble silicates are common ingredients in the laundry detergent compositions.
• the alkali metal silicate salt preferably has a weight ratio of SiC ⁇ /hO, within the range of 1.6 to 3.3 more preferably 1.6 to 2.4, and most preferably 2.0 to 2.85 wherein M is an alkali metal.
• the alkali metal silicate salt employed is in the form of an aqueous solution, generally having 30 wt.% to 45 wt.% solid content.
• the alkali metal silicate salt may be selected from the group consisting of sodium silicate, potassium silicate, sodium-potassium double silicate or mixtures thereof.
• the alkali metal silicate salt is water-soluble.
• the alkali metal silicate salt employed is sodium silicate.
• the sodium silicate has a weight ratio, SiO2:Na2O within the range of 1.6 to 3.3 more preferably 1.6 to 2.4, and most preferably 2.0 to 2.85.
• the aqueous slurry includes from 4 wt.% to 15 wt.% alkali metal silicate salt builder, still preferably from 4 wt.% to 13.5 wt.% alkali metal silicate salt builder.
• an alkaline builder selected from the group consisting of: preferably from 4 wt.% to 15 wt.% alkali metal silicate, 3 wt.% to 15 wt.% alkali metal carbonate builder or mixtures thereof; and,
• the amount of solubilized aluminium hydrate in the aqueous slurry is not less than 0.08 wt.%, still preferably not less than 1 wt.%, more preferably not less than 1.5 wt.%, still more preferably not less than 2 wt.%, but typically not more than 3.5 wt.%, preferably not more than 3 wt.% or still preferably not more than 2.5 wt.%.
• the amount of water in the aqueous slurry is not less than 22 wt.%, still preferably not less than 24 wt.%, more preferably not less than 25 wt.%, but typically not more than 34 wt.%, preferably not more than 38 wt.% or still preferably not more than 37 wt.%.
• Inorganic phosphate builders for example sodium orthophosphate, pyrophosphate and tripolyphosphate, hexametaphosphate are preferably present at relatively low levels, for example less than 5 wt.%, still preferably less than 3 wt.%, further preferably less than 1 wt.%.
• the aqueous slurry includes 0 wt.% phosphate builder.
• the spray-dried detergent particle prepared from the process according to the first aspect of the present invention is substantially free of inorganic phosphate builder. By substantially free it is meant that the spray dried detergent particle prepared according to the process of the first aspect does not include any deliberately added inorganic phosphate builder.
• Zeolite builders used in most commercial particulate detergent compositions is zeolite A.
• aluminium zeolite P zeolite MAP
• zeolite MAP is an alkali metal aluminosilicate of the P type having a silicon to aluminium ratio not exceeding 1.33, preferably not exceeding 1.15, and more preferably not exceeding 1.07.
• Zeolite builders are preferably present at relatively low levels, for example less than 5 wt.%, still preferably less than 3 wt.%, further preferably less than 1 wt.% in the aqueous slurry.
• the aqueous slurry includes 0 wt.% zeolite builder.
• Non-limiting examples of organic builder include polycarboxylate polymers such as polyacrylates, acrylic/maleic copolymers, and acrylic phosphinates; monomeric polycarboxylates such as citrates, gluconates, oxydisuccinates, glycerol mono-, di-and tri succinates, carboxymethyloxysuccinates, carboxymethyloxymalonates, dipicolinates, hydroxyethyliminodiacetates, alkyl- and alkenylmalonates and succinates; and sulphonated fatty acid salts.
• polycarboxylate polymers such as polyacrylates, acrylic/maleic copolymers, and acrylic phosphinates
• monomeric polycarboxylates such as citrates, gluconates, oxydisuccinates, glycerol mono-, di-and tri succinates, carboxymethyloxysuccinates, carboxymethyloxymalonates, dipicolinates, hydroxyethyliminodiacetates
• Preferred supplementary organic builders are suitably used in amounts of from 0.1 wt.% to 30 wt.%, preferably from 10 wt.% to 25 wt.%; and acrylic polymers, more especially acrylic/maleic copolymers, suitably used in amounts of from 0.5 wt.% to 15 wt.%, preferably from 1 wt.% to 10 wt.%.
• Powder flow properties may be improved by the incorporation of a small amount of a powder structurant, for example, a fatty acid (or fatty acid soap), a sugar, an acrylate or acrylate/maleate polymer.
• a powder structurant for example, a fatty acid (or fatty acid soap), a sugar, an acrylate or acrylate/maleate polymer.
• a powder structurant is fatty acid soap, suitably present in an amount of from 1 wt.% to 5 wt.%.
• the spray-drying is carried out using any of the conventional spray drying system known in the art.
• the aqueous slurry is transferred through a pipe system to a pump system consisting of one or more pump and then further to a spray nozzle through which the slurry is released under pressure into a drying tower.
• a typical spray-drying process involves the step of transferring the aqueous slurry through a pipe system leading to a first pump and then through a second pump and from a second pump to a plurality of spray nozzles.
• the first pump is typically a low- pressure pump, such as a pump that can generate a pressure of from 1x10 5 Nov 2 to 1x10 6 Nm -2 , which ensures proper flooding of the second pump.
• the second pump is a high-pressure pump, such as a pump can generate a pressure ranging from 2x10 6 Nm -2 to 2x10 7 Nm -2 .
• the aqueous slurry may be transferred through bolt catchers, magnetic filters, lump breakers, disintegrators such as the Ritz Mill, during the transfer of the aqueous slurry through the pipe system downstream the pump system/mixer in which the aqueous slurry is formed.
• the disintegrator is preferably positioned between the pumps.
• the flow rate of the aqueous slurry along the pipes is typically in the range from 800 Kg/hour to more than 50,000 Kg/hour.
• the spray drying system may include a deaeration system.
• the deaeration system is preferably a vacuum assisted de-aerator, which is preferably fed by a transfer pump.
• the deaeration system remove air bubbles formed during the slurry preparation, thus increasing the bulk density of the spray-dried detergent particle.
• Deaeration of the slurry may also be carried out by other mechanical means or chemical de-aeration means using antifoams or de-foamers.
• the inlet hot air/hot steam temperature introduced into the spray drying tower is the range from 250°C to 500°C depending on the evaporation capacity and sizing of the tower.
• the tower exhaust air temperature can range from, 60°C to 200°C, more preferably 80°C to 200°C, still more preferably 80°C to 100°C depending on the loading of the tower.
• the aqueous slurry introduced into the spray nozzle of the spray drying tower is preferably at a temperature ranging from 60°C to 95°C.
• the spray drying tower may be a co-current spray drying tower, but these are less common.
• the spray-dried detergent particle existing the tower is maintained at a temperature less than 150°C, still preferably less than 100°C.
• the amount of alkali metal carbonate in the spray-dried detergent particle is not less than 6 wt.%, still preferably not less than 8 wt.%, more preferably not less than 10 wt.%, but typically not more than 18 wt.%, preferably not more than 16 wt.% or still preferably not more than 15 wt.%.
• the amount of filler in the spray-dried detergent particle is not less than 10 wt.%, still preferably not less than 15 wt.%, more preferably not less than 20 wt.%, but typically not more than 65 wt.%, preferably not more than 60 wt.% or still preferably not more than 55 wt.%.
• the spray dried detergent particle may preferably include from 0 wt.% to 4 wt.% polymer selected from antiredeposition polymer, soil release polymer, structuring polymer or mixtures thereof.
• the polymer is a polymeric carboxylate, preferably polyacrylate or a copolymer of acrylic acid and maleic acid.
• other polymers may also be suitable such as polyamines (including the ethoxylated variants thereof), polyethylene glycol and polyesters.
• Polymeric soil suspending aids and polymeric soil release agents are particularly suitable.
• the spray dried detergent particle includes from 0 wt.% to 4 wt.% carboxylate polymer, still preferably from 0 wt.% to 2.5 wt.% carboxylate polymer, more preferably from 0 wt.% to 1 wt.% carboxylate polymer.
• the antiredeposition polymer may be a sodium carboxymethyl cellulose which may be used in an amount ranging from 0 wt.% to 4 wt.%.
• the spray-dried detergent particle preferably comprises from 7 wt.% to 40 wt.% anionic surfactants, which is preferably a C to C20 linear alkyl benzene sulphonate, still C10 to C13 linear alkyl benzene sulphonate preferably and which is substantially neutralized with little or no acid residues. It is also preferred that the anionic surfactant is a combination of alkyl benzene sulphonate and either or both alkyl sulphate surfactant and alkyl ethoxylated sulphate.
• the spray-dried particle is typically post dosed with ingredients that are incompatible with the spray-drying process conditions to form a fully formulated laundry detergent composition.
• a fully formulated laundry detergent composition includes from 20 wt.% to 95 wt.% of the spray-dried particle according to the first aspect.
• the other laundry ingredients are post dosed by dry mixing the spray-dried particle with other laundry ingredients. These laundry ingredients and generally those that are not thermally stable.
• Non-limiting example of the other post dosed laundry ingredients includes enzymes, shading dye, fragrance, antifoams, cleaning polymers, care polymers, foam boosters, visual cues, chelating agents and mixtures thereof.
• These components may be incompatible for many reasons including heat sensitivity, pH sensitivity or degradation in aqueous systems.
• the spray dried detergent particle may be used for preparing a unit dose product where the spray-dried detergent particle is enclosed in a pouch, preferably a water-soluble pouch, more preferably a water-soluble pouch comprising a film forming polymer selected from polyvinyl alcohol, polyvinylpyrrolidone and other known film forming polymer.
• the spray-dried particle mixed with layering agents is also known as base powder and is preferably formulated into a finished detergent composition by dry mixing heat sensitive ingredients into the base powder.
• heat sensitive ingredients some amount of alkalinity may be added back into the base powder by addition of alkaline ingredients, additionally other acidic or neutral may also be added to formulate the finished detergent composition.
• the spray-dried detergent particle may be used as a fully formulated laundry detergent composition or may be additionally combined with other optional laundry ingredients to form a fully formulated laundry detergent composition.
• the optional post-dosed laundry ingredients includes but is not limited to enzymes, antiredeposition polymers, perfumes, additional surfactant selected from amphoteric surfactant, zwitterionic surfactant, cationic surfactant and non-ionic surfactant, optical brighteners, antifoaming agent, foam boosters, fabric softeners such as smectite clays, amine softeners and cationic softeners; bleach and bleach activators; dyes or pigments, fillers, fluorescers, salts, soil release polymers, antiredeposition polymer dye transfer inhibitors.
• the antiredeposition polymer may be a sodium carboxymethyl cellulose which may be used in an amount ranging from 0 wt.% to 4 wt.%. These optional ingredients are well known to be used in a laundry detergent composition and added preferably by post-dosing.
• the laundry detergent composition includes from 5 wt.% to 100 wt.% spray-dried detergent particle obtainable according to the first aspect of the present invention. More preferably from 30 wt.% to 95 wt.% of the spray-dried detergent particle obtainable according to the first aspect of the present invention.
• Suitable fluorescent brighteners include dis-styryl biphenyl compounds example Tinopal® CBS-X, di-amino stilbene di-sulfonic acid compounds, e.g. Tinopal® DMS pure Xtra and Blankophor® HRH, and Pyrazoline compounds, e.g. Blankophor® SN, and coumarin compounds, e.g. Tinopal® SWN.
• Preferred brighteners are: sodium 2 (4- styry)-3-sulfophenyl)-2H-napthol(1,2-d]triazole, disodium 4,4’bis ⁇ [4-anilino-6-(N methyl- N-2 hydroxyethyl)amino 1,3,5- triazin-2-yl)]amino]stilbene-2-2' disulfonate, disodium 4,4’bis([(4-anilino-6-morpholino-l,3,5-triazin-2-yl)]amino ⁇ stilbene-2-2'disulfonate, and disodium 4,4’- bis(2-sulfostyryl)biphenyl.
• a suitable fluorescent brightener is S C.l. Fluorescent Brightener 260, which may be used in its beta or alpha crystalline forms, or a mixture of these forms.
• the composition of the present invention preferably includes an enzyme. It may preferably include one or more enzymes. Preferred examples of the enzymes include those which provide cleaning performance and/or fabric care benefits.
• Suitable enzymes include, but are not limited to, hemicellulases, peroxidases, proteases, cellulases, xylanases, lipases, xyloglucanase, phospholipases, esterases, cutinases, pectinases, mannanases, pectate lyases, keratinases, reductases, oxidases, phenoloxidases, lipoxygenases, ligninases, pullulanases, tannases, pentosanases, mannanases, G-glucanases, arabinosidases, hyaluronidase, chondroitinase, laccase, and amylases, or mixtures thereof.
• a typical combination is an enzyme combination that includes a protease and lipase in conjunction with one or more of amylase, mannanase and cellulase.
• the enzymes When present in a detergent composition, the enzymes may be present at levels from about 0.00001% to about 2%, from about 0.0001% to about 1 % or from 0.001 % to about 0.5% enzyme protein by weight of the detergent composition.
• a packaged article comprising a flexible container enclosing a laundry detergent composition having a spray dried detergent particle prepared according to the first aspect of the present invention.
• the flexible container is preferably made from a packaging material suitable for packaging laundry detergent composition and but not limited to polyolefin film, laminates, paper based films or laminates, multilayered structures include two or more flexible structures and other materials known to a person skilled in the art.
• the flexible container includes polyethylene films having polymer selected from HDPE, LLDPE, mLLDPE, LDPE or combination thereof.
• the flexible films may be made of monomaterial or combination of different materials.
• the flexible packaging container is a flexible pouch or a bag.
• the flexible container may preferably include a measurement means which may be supplied with the package either as a part of the closure of the container or as an integrated system or a separate dosing measure may be provided along with the package.
• the laundry detergent composition comprising the spray dried detergent particle of the present invention may be packaged as unit dose product enclosed within a polymeric film, wherein the polymeric film is water soluble or disintegrates upon addition to the wash water.
• the spray-dried detergent particle or a laundry detergent composition including the spray-dried particle of the invention may be supplied in multidose plastics packs with a top or bottom closure, may be enclosed in a flexible container.
• the packaging material suitable for packaging may include but not limited to multilayer polyethylene film, laminate, paper based, and other materials known to a person skilled in the art.
• the packaging material is selected from material which are biodegradable or recyclable.
• aqueous detergent slurry was spray dried in a counter-current spray drying tower.
• the aqueous detergent slurry was heated to 80°C and pumped under pressure (7.5x106 Nm- 2 ), into a counter current spray-drying tower with an air inlet temperature ranging from between 250°C to 330°C.
• the inlet fan was set to provide a tower inlet airflow of 187,500 kgtr 1 .
• the exhaust fan was controlled to create a negative pressure in the tower of -200 Nm -2 (typically the outlet air flow rate through the exhaust fan is between 220,000 kgh' 1 to 240,000 kgtr 1 , this includes the evaporated water from the slurry).
• the temperature of the spray-dried detergent particle exiting the tower has a temperature of below 150°C.
• the composition of the spray- dried detergent particle obtained by spray-drying the aqueous detergent slurry is given below.
• the composition of the spray dried powder is provided in Table 2 below.
• a control spray-dried particle with the formulation as provided in table 3 was prepared under similar spraying conditions as the inventive Ex 1 was then similarly stored.
• the % caking was measured after 12 week and the values were noted and provided in table 3 below.

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• 2022
  • 2022-09-12 EP EP22786761.1A patent/EP4402233B1/de active Active
  • 2022-09-12 WO PCT/EP2022/075230 patent/WO2023041467A1/en not_active Ceased
  • 2022-09-12 CN CN202280062056.2A patent/CN117940543A/zh active Pending
• 2024
  • 2024-03-07 ZA ZA2024/01939A patent/ZA202401939B/en unknown

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