EP0550086B1 - Verfahren zur Herstellung einer granulierten Waschmittelzusammensetzung - Google Patents

Verfahren zur Herstellung einer granulierten Waschmittelzusammensetzung Download PDF

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Publication number
EP0550086B1
EP0550086B1 EP19920203804 EP92203804A EP0550086B1 EP 0550086 B1 EP0550086 B1 EP 0550086B1 EP 19920203804 EP19920203804 EP 19920203804 EP 92203804 A EP92203804 A EP 92203804A EP 0550086 B1 EP0550086 B1 EP 0550086B1
Authority
EP
European Patent Office
Prior art keywords
weight
slurry
granules
spray
granular detergent
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP19920203804
Other languages
English (en)
French (fr)
Other versions
EP0550086A1 (de
Inventor
Feng-Lung Gordon Hsu
Charles Fraser Irwin
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Unilever PLC
Unilever NV
Original Assignee
Unilever PLC
Unilever NV
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Unilever PLC, Unilever NV filed Critical Unilever PLC
Publication of EP0550086A1 publication Critical patent/EP0550086A1/de
Application granted granted Critical
Publication of EP0550086B1 publication Critical patent/EP0550086B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
    • C11D17/065—High-density particulate detergent compositions
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • 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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C11D3/10—Carbonates ; Bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • 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
    • C11D3/128—Aluminium silicates, e.g. zeolites

Definitions

  • the present invention relates to a process for making a granular detergent composition.
  • Granular detergents produced by spray-drying have good solubility but tend to be of low bulk density and therefore, have large packing volumes.
  • High bulk density granular detergent compositions have several advantages over low bulk density compositions.
  • the packing volume of the granules is lower, meaning that packaging can be smaller which facilitates storage and transport of products.
  • non-automatic washing machine powders be produced by a process of spray-cooling.
  • U.S. Patent 4,466,897 discloses a process for making a detergent powder for use in a non-automatic washing machine by impregnating spray-dried or spray-cooled washing powder comprising a sodium soap as the principal organic detergent-active species, with a finely divided, water soluble sodium salt.
  • British Patent Specification 1, 344, 253 discloses a process for producing an enzymatic adjunct for use in detergent compositions by suspending enzyme particles in a molten nonionic surfactant and solidifying the mixture by spray-cooling. The production of detergent compositions comprising anionic surfactants is not disclosed.
  • the invention provides a process for the manufacture of a granular detergent composition comprising the steps of
  • the advantages of this process are that it uses existing equipment since most granular detergents are produced by spray-drying and this same apparatus can be used for spray-cooling, operating costs are low since no drying gas is used in the process and nonionic surfactants can be used in the compositions without undesirable emissions.
  • the process also gives the advantage of bulk density flexibility since high or low bulk density granules can be produced.
  • a solid component which can comprise detergency builders such as water-soluble alkaline inorganic materials (for example sodium carbonate seeded with calcium carbonate), zeolite, sodium tripolyphosphate, other watersoluble inorganic materials, for example, sodium bicarbonate or silicate, fluorescers, polycarboxylate polymers, antiredeposition agents, and fillers, is mixed with a carrier component which, in addition to a non-soap surfactant can comprise water, silicate solution, liquid polymer components, polyethylene glycols, perfumes, enzymes and other materials.
  • detergency builders such as water-soluble alkaline inorganic materials (for example sodium carbonate seeded with calcium carbonate), zeolite, sodium tripolyphosphate, other watersoluble inorganic materials, for example, sodium bicarbonate or silicate, fluorescers, polycarboxylate polymers, antiredeposition agents, and fillers
  • a carrier component which, in addition to a non-soap surfactant can comprise water
  • the process is very flexible with respect to the chemical composition of the starting materials. Phosphate as well as zeolite based compositions and compositions having low or high surfactant contents may be made. The process is also suitable for preparing calcite/carbonate containing compositions.
  • the solid component is preferably particulate with particle size of 1 to 400 microns (as measured by Rosin Rammler), more preferably 1 to 350 microns, most preferably 10 to 300 microns.
  • the solid component comprises from 5 to 95% by weight of detergent builders, preferably from 10 to 80%, more preferably from 20 to 60%.
  • the carrier comprises from 5% to 95% by weight of non-soap surfactants, preferably from 15% to 80% by weight, more preferably from 20% to 70% by weight.
  • the carrier component comprises a mixture of surfactants for example, anionic, nonionic or zwitterionic.
  • the anionic surfactant may be selected from linear alkyl benzene sulphate or sulphonate preferably C 12 to C 18 linear alkyl benzene sulphate, alpha-olefin sulphate or sulphonate, internal olefin sulphate or sulphonate, fatty acid ester sulphate or sulphonate and primary and secondary alcohol sulphates or sulphonates.
  • non-soap anionic surfactant any anionic surfactant except the water-soluble salts of C 8 to C 24 fatty acids.
  • the nonionic surfactant may be selected from those compounds produced by the condensation of alkylene oxide groups with an organic hydrophobic compound for example alkyl phenols or alcohols.
  • Preferred nonionics are the water soluble condensation products of aliphatic alcohols with 8 to 30 carbon atoms in the molecule with 3 to 15 moles of ethylene oxide per mole of alcohol.
  • Other nonionics include water soluble amine oxides containing one alkyl moiety of about 10 to 18 carbon atoms and 2 moieties selected from the groups of alkyl and hydroxyalkyl moieties with from 1 to 3 carbon atoms and those nonionics derived from sugars such as alkyl poly glycoside.
  • the zwitterionic surfactants include derivatives of aliphatic quaternary ammonium phosphonium and sulphonium compounds in which one of the aliphatic substituents contains an anionic water-solubilizing group.
  • the carrier comprises a mixture of surfactants for example a mixture of linear alkylbenzene sulphonate containing from 11 to 14 carbon atoms and a C 12 to C 15 primary alcohol ethoxylated with 3 to 7 moles of ethylene oxide per mole of alcohol in a weight ratio of anionic to nonionic of 3 to 1 or a mixture of a C 14 to C 17 secondary alcohol sulphate with a C 12 to C 15 primary alcohol ethoxylated with 7 moles of ethylene oxide per mole of alcohol in a weight ratio of from 2 to 1.
  • surfactants for example a mixture of linear alkylbenzene sulphonate containing from 11 to 14 carbon atoms and a C 12 to C 15 primary alcohol ethoxylated with 3 to 7 moles of ethylene oxide per mole of alcohol in a weight ratio of anionic to nonionic of 3 to 1 or a mixture of a C 14 to C 17 secondary alcohol sulphate with a C 12 to C 15 primary alcohol ethoxy
  • the carrier component is prepared by neutralizing a non-soap sulphonic acid with a mixture of nonionic surfactant and concentrated aqueous alkali metal hydroxide in an amount stoichiometric to the sulphonic acid.
  • the sulphonic acid may also be under or over neutralized. The heat generated by the exothermic neutralization allows the carrier to be mixed with the solid component and pumped directly to the spray-cooling apparatus without further heating.
  • the surfactant comprises less than 20% by weight of water, more preferably less than 10% and most preferably less than 5% by weight and is made by the method described in US-A-4,923,636 (Blackburn) or US-A-4,826,632 (Blackburn) incorporated herein by reference.
  • Preferred surfactant mixtures contain 20 to 80% by weight of anionic surfactant and 20 to 80% by weight of nonionic surfactant and no water.
  • the carrier component comprises less than 30% by weight of water, more preferably between 25% and 0%, most preferably between 10% and 0%.
  • the carrier component preferably comprises from 1% to 20% of a solidification aid such as a fatty acid (which can be neutralized to form a salt in situ) or a polymer with a melting point between 40°C and 85°C (for example a polyethylene glycol or polypropylene glycol of molecular weight between 1400 and 20,000.)
  • a solidification aid such as a fatty acid (which can be neutralized to form a salt in situ) or a polymer with a melting point between 40°C and 85°C (for example a polyethylene glycol or polypropylene glycol of molecular weight between 1400 and 20,000.)
  • Preferred solidification aids are polyethylene glycol of molecular weight 3350 and stearic acid.
  • the carrier component preferably comprises from 2 to 10% by weight of a solidification aid.
  • the spray-cooling apparatus used to carry out the process consists essentially of a slurry mixer, pump and spray nozzle inside a cylindrical vessel fed with counter current air.
  • the carrier may be prepared by any suitable method which maintains the total water content below 30% by weight of the carrier. It is preferred to mix any nonionic surfactant with concentrated aqueous sodium hydroxide solution in an amount stoichiometric to the anionic sulphonic acid, mix with the sulphonic acid and add a solidification aid such as fatty acid.
  • the carrier thus obtained is mixed with the solid component to form a slurry.
  • the slurry is then atomized into droplets and solidified into granules either by reduction of temperature below the melting point of the slurry or by neutralization of any fatty acid present by coating the droplets with soda ash.
  • the solidified droplets can be coated with a flow aid such as zeolite to improve their powder properties.
  • the resulting granules are preferably from 300 to 1200 microns in diameter and are generally spherical with little or no internal porosity, especially if atomized without the aid of air injection.
  • the ratio by weight of carrier to solid component in the slurry is preferably from 1:2 to 4:1 by weight, more preferably 1:1 to 2:1.
  • the slurry temperature is preferably from 50°C to 100°C.
  • LAS Sodium salt of C 11 -C 15 alkylbenzene sulphonate acid (stephan Bio-Soft S-100) PEG 3350 Polyethylene glycol (mw 3350) Carbowax PEG 3350 ex Union Carbide Zeolite Zeolite 4A PQ Corp., Valfor 100 DSA dense soda ash, FMC, Grade 260 NI13EO nonionic surfactant (ethoxylated C 12 -C 15 alcohol) 13 moles of ethylene oxide per mole of alcohol.
  • Alkylbenzene sulphonic acid was neutralized with a mixture of nonionic surfactant and a stoichiometric amount of concentrated aqueous sodium hydroxide.
  • Polyethylene glycol of molecular weight 3350 and zeolite were added to this mixture. Due to the neutralization reaction the slurry temperature was raised to about 80°C.
  • the slurry was then pumped through a gear pump to a two fluid nozzle isolated in an Aeromatic fluid bed model STREA-1 and atomized into droplets. Dense soda ash and zeolite were fluidized in the bed to coat the droplets which solidified in the bed.
  • a slurry was produced as in Examples 1 and 2 by mixing in a spray pot. The slurry was then atomized into droplets using air pressure in place of the pump in Examples 1 and 2. It can be seen that this reduces the bulk density from the 845 and 852 g/l of Examples 1 and 2 to 750 g/l in Example 3.
  • a slurry was prepared as in Example 3 and atomized using air pressure as in Example 3.
  • the slurry was atomized into a cooling tower, the droplets landing on a bed of zeolite.
  • a slurry was prepared as in Examples 1 and 2 and sprayed via a single fluid nozzle into a cooling tower. Light soda ash was blown into the bottom of the tower to form a cloud of soda ash which coated the falling particles.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Detergent Compositions (AREA)

Claims (11)

  1. Verfahren zur Herstellung einer körnigen Waschmittelzusammensetzung, umfassend die Stufen
    (i) des Mischens einer Trägerkomponente, enthaltend von 5 bis 95 Gewichtsprozent eines Nicht-Seife-Surfactants mit einer festen Komponente, enthaltend 5 bis 95 Gewichtsprozent Waschmittel-Builder zur Bildung einer sprühfähigen Aufschlämmung; und
    (ii) Verfestigen der Aufschlämmung zu Körnchen durch Zerstäubungskühlung.
  2. Verfahren nach Anspruch 1, worin die Trägerkomponente weniger als 30 Gewichtsprozent Wasser enthält.
  3. Verfahren nach einem der Ansprüche 1 oder 2, worin das Nicht-Seife-Surfactant von 20 bis 80 Gewichtsprozent an anionischem und von 20 bis 80 Gewichtsprozent an nichtionischem Surfactant enthält.
  4. Verfahren nach einem der Ansprüche 1 bis 3, worin die feste Komponente teilchenförmig mit Teilchengrößen zwischen 1 und 400 Mikron ist.
  5. Verfahren nach einem der Ansprüche 1 bis 4, worin die Trägerkomponente von 1 bis 20 Gewichtsprozent einer Verfestigungshilfe enthält.
  6. Verfahren nach einem der Ansprüche 1 bis 5, worin die Aufschlämmungstemperatur im Bereich von 50° bis 100°C vor dem Sprühen liegt.
  7. Verfahren nach einem der Ansprüche 1 bis 6, worin die resultierenden Körnchen einen Durchmesser von 300 bis 1200 Mikron aufweisen.
  8. Verfahren nach einem der Ansprüche 1 bis 7, worin die Schüttdichte der entstehenden Körnchen größer als 600 g/ℓ ist.
  9. Eine körnige Waschmittelzusammensetzung, hergestellt durch das Verfahren nach einem der Ansprüche 1 bis 8, wobei die körnige Waschmittelzusammensetzung im wesentlichen aus Körnchen mit niedriger innerer Porosität besteht.
  10. Verfahren zur Herstellung einer körnigen Waschmittelzusammensetzung, umfassend die Stufen von:
    (i) Auswählen einer Trägerkomponente, enthaltend von 5 bis 95 Gewichtsprozent eines Nicht-Seife-anionischen Surfactants;
    (ii) Auswählen einer festen Komponente;
    (iii) Mischen des Trägers und der festen Komponenten zur Bildung einer sprühfähigen Aufschlämmung;
    (iv) Verfestigen der Aufschlämmung zu Körnchen durch Zerstäubungskühlung;
    (v) Beschichten der Körnchen mit einem Fließmittel.
  11. Verfahren nach Anspruch 10, worin die Aufschlämmung unter Verwendung von Druckluft durch Zerstäubung gekühlt ist.
EP19920203804 1991-12-31 1992-12-08 Verfahren zur Herstellung einer granulierten Waschmittelzusammensetzung Expired - Lifetime EP0550086B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US81636691A 1991-12-31 1991-12-31
US816366 1991-12-31

Publications (2)

Publication Number Publication Date
EP0550086A1 EP0550086A1 (de) 1993-07-07
EP0550086B1 true EP0550086B1 (de) 1998-03-11

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Application Number Title Priority Date Filing Date
EP19920203804 Expired - Lifetime EP0550086B1 (de) 1991-12-31 1992-12-08 Verfahren zur Herstellung einer granulierten Waschmittelzusammensetzung

Country Status (3)

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EP (1) EP0550086B1 (de)
DE (1) DE69224729T2 (de)
ES (1) ES2113408T3 (de)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB9324127D0 (en) * 1993-05-26 1994-01-12 Unilever Plc Detergent compositions
DE19524464C2 (de) * 1995-07-10 2000-08-24 Cognis Deutschland Gmbh Verfahren zur Herstellung von Zuckertensidgranulaten
GB9711359D0 (en) 1997-05-30 1997-07-30 Unilever Plc Detergent powder composition
GB9711356D0 (en) 1997-05-30 1997-07-30 Unilever Plc Particulate detergent composition
ID29296A (id) 1997-05-30 2001-08-16 Unilever Nv Komposisi deterjen butiran lembut yang bebas mengalir
GB9711350D0 (en) * 1997-05-30 1997-07-30 Unilever Plc Granular detergent compositions and their production
US6627597B1 (en) 1998-10-15 2003-09-30 The Procter & Gamble Company Method for making a nanoporous granular material and a detergent composition
WO2018234056A1 (en) * 2017-06-20 2018-12-27 Unilever N.V. PARTICULATE DETERGENT COMPOSITION COMPRISING A FRAGRANCE

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1344253A (en) * 1970-09-02 1974-01-16 Grindstedvaerket As Enzymatic products for use in detergents
US4466897A (en) * 1981-09-29 1984-08-21 Lever Brothers Company Process for the manufacture of soap powder

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Publication number Publication date
DE69224729D1 (de) 1998-04-16
DE69224729T2 (de) 1998-07-02
EP0550086A1 (de) 1993-07-07
ES2113408T3 (es) 1998-05-01

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