EP0882126A1 - Procede pour la production d'une composition detergente - Google Patents

Procede pour la production d'une composition detergente

Info

Publication number
EP0882126A1
EP0882126A1 EP97901008A EP97901008A EP0882126A1 EP 0882126 A1 EP0882126 A1 EP 0882126A1 EP 97901008 A EP97901008 A EP 97901008A EP 97901008 A EP97901008 A EP 97901008A EP 0882126 A1 EP0882126 A1 EP 0882126A1
Authority
EP
European Patent Office
Prior art keywords
bulk density
process according
detergent
low
granules
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.)
Granted
Application number
EP97901008A
Other languages
German (de)
English (en)
Other versions
EP0882126B1 (fr
Inventor
Reiner Jumao-As Abdul Wahab Al-Ghamdi Crisologo
Marcelito Abad Abdul Wahab Al-Ghamdi Garcia
David Alan Jordan
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
Family has litigation
First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=10787857&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=EP0882126(A1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Unilever PLC, Unilever NV filed Critical Unilever PLC
Publication of EP0882126A1 publication Critical patent/EP0882126A1/fr
Application granted granted Critical
Publication of EP0882126B1 publication Critical patent/EP0882126B1/fr
Anticipated expiration legal-status Critical
Revoked legal-status Critical Current

Links

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
    • 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
    • C11D11/04—Special methods for preparing compositions containing mixtures of detergents by chemical means, e.g. by sulfonating in the presence of other compounding ingredients followed by neutralising

Definitions

  • the present invention relates to a process for the production of a detergent composition.
  • the invention is concerned with a process for the production of a detergent composition having a medium bulk density without the use of a spray-drying step involving a high shear mixing step and a very low shear mixing step and to detergent compositions thereby produced.
  • detergent compositions have been produced by a spray-drying process in which the components of the composition are mixed with water to form an aqueous crutcher slurry which is then sprayed into a spray-drying tower and contacted with hot air to remove water whereby detergent particles, often referred to as a "base" powder are obtained.
  • the particles so obtained have a high porosity.
  • powders produced by this method typically have a bull- density of 300 to 550 g/1 or even up to 650 g/1.
  • Spray-dried powders generally provide good powder delivery characteristics such as dispensing and dissolution. However, the capital and operating costs of the spray-drying process are high. Nevertheless there remains a significant consumer demand for such low density powders.
  • detergent powders having a high bulk density have been produced by mechanical mixing processes. Bulk densities of 700 to 900 g/1 and even higher have been obtained. Typically such powders are produced by densifying a spray-dried base powder in one or more mechanical mixers, optionally with the addition of further components, or by mixing the components of the composition in a continuous or batch mixing process without the use of a spray-drying step.
  • EP 367 339 discloses a process for the production of a detergent composition having a high bulk density in which a particulate starting material is treated in a high speed mixer, a moderate speed mixer wherein the material is brought into or maintained in a deformable state, and then dried and/or cooled.
  • the starting material may be a spray-dried base powder or the components of the composition may be employed without a prior spray-drying step in the detergent production process.
  • Powders having a high bulk density have a low packing volume which is advantageous for storage and distribution operations and also for the consumer. Furthermore, if a spray-drying step is not employed, the capital and operating costs are typically much lower and the process uses less energy and so provides an environmental benefit. The avoidance of a spray-drying step in the detergent production process is therefore desirable.
  • EP 544 365 (Unilever) is concerned with the production of a high bulk density detergent composition and refers to the bulk density of a detergent powder being dependent upon the bulk density of the starting materials in the case of a mixing process.
  • Treating a porous spray-dried material in a mechanical mixing process typically leads to an increase in bulk density as the powder porosity is reduced.
  • a powder having a surprisingly low bulk density for example less than 700 g/1, may be obtained by a process in which a spray-drying step is not employed, involving a high shear mixing step and a very low shear mixing step if a component having a low bulk density is incorporated in the very low shear mixing step. Further, such a powder exhibits good powder properties.
  • a first aspect of the invention provides a process for the production of a detergent composition or component having a bulk density of less than 700 g/1 which does not comprise a spray-drying step and which process comprises mixing a particulate starting material with a liquid binder in a mixer granulator, preferably having both a stirring and a cutting action, to form granules wherein the starting material and/or binder comprises a non-soap detergent active or a precursor thereof, feeding the said granules to a very low shear mixing zone and contacting the granules with a particulate material having a bulk density of not more than 700g/l to produce a detergent composition or component having a bulk density of less than 700 g/1.
  • a second aspect of the invention provides a detergent composition or component having a bulk density of less than 700 g/1 obtainable by a process which does not comprise a spray-drying step and which comprises mixing a particulate starting material with a liquid binder in a mixer/granulator, preferably having both a stirring and cutting action, to form granules and feeding the said granules to a very low shear mixing zone and contacting the granules with a particulate material having a bulk density of not more than 700g/l.
  • % figures are on a weight basis and based on the total weight of the detergent composition or component prior to the optional addition of post-dosed ingredients .
  • the detergent composition has a bulk density of 400 to 680 g/1, preferably 450 to 680 g/1 and more preferably 500 to less than 650 g/1. It is further preferred that the detergent composition has a particle porosity of at least 0.2 and more preferably at least 0.25. The porosity may be determined by a mercury porosimetry method.
  • the component incorporated in the very low shear zone has a bulk density of not more than 700 g/1, and suitably has a bulk density of 200 to 600 g/1, preferably 250 to 550 g/1 and especially 350 to 500 g/1.
  • This low bulk density component is desirably an aluminosilicate, for example zeolite 4A or zeolite A24 or a salt, preferably an inorganic salt. Salts, preferably sodium, of phosphates, for example tripolyphosphate, carbonate, bicarbonate and sulphate are especially suitable. Desirably the low bulk density component constitutes the detergency builder, or part thereof in the composition. If desired, this component may be a non-builder material, in which case the particulate starting material will suitably comprise a builder.
  • the low bulk density component comprises sodium tripolyphosphate having a bulk density of 380 to 500 g/1. This compares to a typical bulk density of 800 to 1000 g/1 for tripolyphosphate conventionally employed in detergent compositions.
  • the level of the low bulk density component is selected according to the desired density of the detergent composition. Preferably it is present at a level of 5 to 65 wt %, preferably 10 to 40 wt % and optimally 10 to 30 wt % of the composition.
  • part of the low bulk density component may be introduced into the high speed mixer/granulator.
  • the level of this component in the very low shear mixing zone is at least 10% by ' weight based on the detergent composition and additionally up to 80% of the total amount of the low bulk density component may be dosed into the high speed mixer/granulator although it is preferred that up to 60%, more preferably 5 to 50%, especially 20 to 45% of the low density material (as a percentage of the total amount of this material) be dosed into the high speed mixer granulator.
  • the process may be continuous but is preferably batch- wise.
  • a preferred type of mixer/granulator for use in the process of the invention is bowl-shaped and preferably has a substantially vertical stirrer axis.
  • mixers of the Fukae (Trade Mark) FS-G series manufactured by Fukae Powtech Kogyo Co. , Japan are essentially in the form of a bowl-shaped vessel accessible via a top port, provided near its base with a stirrer having a substantially vertical axis, and a cutter positioned on a side wall.
  • the stirrer and cutter may be operated independently of one another, and at separately variable speeds.
  • Another mixer found to be suitable for use in the process of the invention is the L ⁇ dige (Trade Mark) FM series batch mixer ex Morton Machine Co. Ltd., Scotland. This differs from the mixers mentioned above in that its stirrer has a horizontal axis.
  • Granulation is preferably effected by running the mixer using both stirrer and cutter; a relatively short residence time (for example, 5-8 minutes for a 35 kg batch) is generally sufficient.
  • the final bulk density can be controlled by choice of residence time.
  • the stirrer is operated at a rate of 25 to 80 rpm, preferably 30 to 75 rpm.
  • the cutter is suitably operated at a rate of 200 to 2500 rpm, preferably 300 to 2200 rpm.
  • a batch process typically involves pre- mixing of solid components, addition of liquids, granulation, optional addition of a layering material suitable for controlling the granulation end-point, and product discharge.
  • the rate of stirring and/or cutting is suitably adjusted according to the stage of the process.
  • the binder comprises one or more of the following: liquid detergent-active compound(s) , precursors thereof, water, solutions, non-aqueous or aqueous, of other ingredients or mixtures thereof. If water is employed the level is desirably controlled so that the moisture content of the detergent composition is not more than 10% by weight and preferably not more than 6%.
  • the mixing step is preferably carried out at a controlled temperature somewhat above ambient, preferably above 30°C.
  • the temperature is within the range 30 to 55°C although higher temperatures may be suitable, for example, where heat of reaction is generated by in situ neutralisation.
  • the very low shear mixing zone may be located within the same apparatus as the high speed mixer granulation but desirably is in a separate apparatus for example a rotating bowl mixer and preferably a fluid bed.
  • the fluid bed is suitably operated at a temperature of 30 to 90°C and at a superficial air velocity of about 0.25 to 1.2 ms "1 .
  • Suitable fluid beds are available from, for example NIRO.
  • the air flow in the fluid bed may be adjusted according to the desired level of shear and agitation of the low bulk density component.
  • the low bulk density component is dosed into the bed and gently agitated using a small air flow which is then increased prior to feeding in the granules from the high speed mixer/granulator.
  • the detergent composition suitably comprises anionic detergent active.
  • anionic detergent active This may be incorporated as a pre- neutralised material, desirably as a component of the particulate starting material, or may be neutralised in situ.
  • the acid precursor of the active is preferably neutralised using a solid neutralising agent, for example carbonate (preferably sodium carbonate) , which is desirably a component of the particulate starting material.
  • the detergent active material present in the composition may be selected from anionic, ampholytic, zwitterionic or nonionic detergent active materials or mixtures thereof.
  • suitable synthetic anionic detergent compounds are sodium and potassium (C 9 -C 20 ) benzene sulphonates, particularly sodium linear secondary alkyl (C 10 -C 15 ) benzene sulphonates; sodium or potassium alkyl sulphates; and sodium alkyl glyceryl ether sulphates, especially those ethers of the higher alcohols derived from tallow or coconut oil and synthetic alcohols derived from petroleum.
  • Suitable nonionics which may be employed include, in particular the reaction products of compounds having a hydrophobic group and a reactive hydrogen atom, for example, aliphatic alcohols, acids, amides or alkyl phenols with alkylene oxides, especially ethylene oxide either alone or with propylene oxide.
  • Specific nonionic detergent compounds are alkyl (C 6 - C 22 ) phenol ethylene oxide condensates, generally having 5 to 25 EO, ie 5 to 25 units of ethylene oxide per molecule, and the condensation products of aliphatic (C 8 -C 18 ) primary or secondary linear or branched alcohols with ethylene oxide, generally 5 to 40 EO.
  • the level of detergent active material present in the composition may be in the range from 1 to 50% by weight depending on the desired applications.
  • Nonionic material may be present in the particulate starting material at a level which is preferably less than 10% by weight, more preferably less than 5% by weight and/or employed as the liquid binder optionally with another liquid component, for example water.
  • the particulate starting material comprises one or more of a carbonate salt at a level of 5 to 60 wt %, a zeolite at a level of 5 to 60 wt % and, if present as the low bulk density component, a phosphate salt at a level of 5 to 20% by weight of the total quantity of starting material.
  • the particulate starting material constitutes 30 to 70% of the detergent composition.
  • a layering material may be employed during the high speed mixing step to control granule formation and reduce or prevent over-agglomeration.
  • a layering material is introduced into the very low shear mixing step.
  • Suitable materials include aluminosilicates, for example zeolite 4A and A24.
  • the layering material is suitability present at a level of 1 to 4 wt % based on the composition.
  • the composition may be used as a complete composition in its own right or may be mixed with other components or mixtures and thus may form a major or minor part of a final product.
  • the composition may be blended with for example a spray-dried base powder.
  • a detergent composition was prepared by dosing the following components into a Fukae FS3500 mixer (in the following sequence) :
  • the mixer was operated at a temperature of 30-35°C.
  • the mixer was operated for sufficient time to effect granulation in the granulation step (end point 60 amps) and the product was discharged over 240 seconds.
  • 130kg of sodium tripolyphosphate (bd 400-440g/l) was dosed into a NIRO fluid bed and 'bubbled' at a low air velocity. Prior to discharge of the granules from the Fukae mixer, the air flow was increased to about 11000 m 3 /hr and the granules were fed into the fluid bed. 20kg of zeolite 4A was then dosed into the fluid bed as a layering material. The detergent composition was then discharged from the fluid bed at a temperature below 30°C.

Landscapes

  • 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)
  • Detergent Compositions (AREA)

Abstract

Cette invention se rapporte à un procédé qui permet de produire une composition détergente à masse volumique en vrac basse à moyenne, en mélangeant un liant liquide et un matériau de départ particulaire dans un mélangeur/granulateur à haute vitesse, afin de former des granulés qui sont ensuite mis en contact avec un matériau particulaire ayant une masse volumique en vrac ne dépassant pas 700g/l dans une zone de mélange à faible cisaillement, tel qu'un lit fluidisé. Les compositions produites par ce procédé sont également présentées.
EP97901008A 1996-01-31 1997-01-06 Procede pour la production d'une composition detergente Revoked EP0882126B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
GB9601920 1996-01-31
GBGB9601920.3A GB9601920D0 (en) 1996-01-31 1996-01-31 Process for the production of a detergent composition
PCT/EP1997/000118 WO1997028246A1 (fr) 1996-01-31 1997-01-06 Procede pour la production d'une composition detergente

Publications (2)

Publication Number Publication Date
EP0882126A1 true EP0882126A1 (fr) 1998-12-09
EP0882126B1 EP0882126B1 (fr) 2000-04-19

Family

ID=10787857

Family Applications (1)

Application Number Title Priority Date Filing Date
EP97901008A Revoked EP0882126B1 (fr) 1996-01-31 1997-01-06 Procede pour la production d'une composition detergente

Country Status (16)

Country Link
EP (1) EP0882126B1 (fr)
CN (1) CN1191351C (fr)
AR (1) AR005576A1 (fr)
AU (1) AU1440997A (fr)
BR (1) BR9707474A (fr)
CA (1) CA2242420C (fr)
DE (1) DE69701731T2 (fr)
EA (1) EA001314B1 (fr)
ES (1) ES2145567T3 (fr)
GB (1) GB9601920D0 (fr)
HU (1) HUP9901180A3 (fr)
IN (1) IN188387B (fr)
PL (1) PL184656B1 (fr)
TR (1) TR199801444T2 (fr)
WO (1) WO1997028246A1 (fr)
ZA (1) ZA97255B (fr)

Families Citing this family (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB9513327D0 (en) * 1995-06-30 1995-09-06 Uniliver Plc Process for the production of a detergent composition
GB9526097D0 (en) * 1995-12-20 1996-02-21 Unilever Plc Process
US6211137B1 (en) 1996-10-04 2001-04-03 The Procter & Gamble Company Process for making a detergent composition by non-tower process
US6121229A (en) * 1996-10-04 2000-09-19 The Procter & Gamble Company Process for making a detergent composition by non-tower process
US6211138B1 (en) 1996-10-04 2001-04-03 The Procter & Gamble Company Process for making a detergent composition by non-tower process
US6150323A (en) * 1996-10-04 2000-11-21 The Procter & Gamble Company Process for making a detergent composition by non-tower process
US6143711A (en) * 1996-10-04 2000-11-07 The Procter & Gamble Company Process for making a detergent composition by non-tower process
US6391844B1 (en) 1996-10-04 2002-05-21 The Procter & Gamble Company Process for making a detergent composition by non-tower process
US6136777A (en) * 1996-10-04 2000-10-24 The Procter & Gamble Company Process for making a detergent composition by non-tower process
US6172034B1 (en) 1996-10-04 2001-01-09 The Procter & Gamble Process for making a detergent composition by non-tower process
GB9712583D0 (en) 1997-06-16 1997-08-20 Unilever Plc Production of detergent granulates
GB9712580D0 (en) * 1997-06-16 1997-08-20 Unilever Plc Production of detergent granulates
GB9713748D0 (en) * 1997-06-27 1997-09-03 Unilever Plc Production of detergent granulates
DE69904499T2 (de) 1998-10-26 2003-10-30 The Procter & Gamble Company, Cincinnati Verfahren zur herstellung eines granularen waschmittels mit verbessertem aussehen und erhöhter löslichkeit
JP2002533532A (ja) * 1998-12-22 2002-10-08 ザ、プロクター、エンド、ギャンブル、カンパニー 凝集による低かさ密度洗剤組成物の製造方法
US6596683B1 (en) 1998-12-22 2003-07-22 The Procter & Gamble Company Process for preparing a granular detergent composition
US6858572B1 (en) 1999-03-09 2005-02-22 The Procter & Gamble Company Process for producing coated detergent particles
GB9913544D0 (en) * 1999-06-10 1999-08-11 Unilever Plc Process for preparing granular detergent compositions
GB9913546D0 (en) 1999-06-10 1999-08-11 Unilever Plc Granular detergent component containing zeolite map and laundry detergent compositions containing it
US6894018B1 (en) 1999-06-21 2005-05-17 The Procter & Gamble Company Process for making granular detergent in a fluidized bed granulator having recycling of improperly sized particles
CN102471740A (zh) * 2009-07-09 2012-05-23 宝洁公司 用于制备衣物洗涤剂组合物的连续方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59157198A (ja) * 1983-02-28 1984-09-06 ライオン株式会社 嵩密度の小さい洗剤ビルダ−造粒物の製造法
JPS6072999A (ja) * 1983-09-30 1985-04-25 花王株式会社 超濃縮粉末洗剤の製法
JPS6072998A (ja) * 1983-09-30 1985-04-25 花王株式会社 粉末物性に優れた界面活性剤粉体組成物の製造法
JPH06128594A (ja) * 1992-10-16 1994-05-10 Lion Corp 界面活性剤粉粒体組成物の製造方法
CZ286742B6 (en) * 1993-07-02 2000-06-14 Unilever Nv Process for preparing detergent
JPH0813000A (ja) * 1994-06-28 1996-01-16 Lion Corp 高嵩密度粒状洗剤組成物の製造方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO9728246A1 *

Also Published As

Publication number Publication date
EA199800668A1 (ru) 1999-02-25
HUP9901180A2 (hu) 1999-08-30
PL328022A1 (en) 1999-01-04
CA2242420A1 (fr) 1997-08-07
ES2145567T3 (es) 2000-07-01
EA001314B1 (ru) 2001-02-26
DE69701731T2 (de) 2000-08-10
CA2242420C (fr) 2005-08-30
WO1997028246A1 (fr) 1997-08-07
PL184656B1 (pl) 2002-11-29
EP0882126B1 (fr) 2000-04-19
IN188387B (fr) 2002-09-14
AU1440997A (en) 1997-08-22
BR9707474A (pt) 1999-07-27
AR005576A1 (es) 1999-06-23
TR199801444T2 (xx) 1998-10-21
CN1209835A (zh) 1999-03-03
CN1191351C (zh) 2005-03-02
DE69701731D1 (de) 2000-05-25
HUP9901180A3 (en) 2002-04-29
GB9601920D0 (en) 1996-04-03
ZA97255B (en) 1998-07-14

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