EP0881279B1 - Procédé de préparation de granules contenant un tensioactif cationique - Google Patents

Procédé de préparation de granules contenant un tensioactif cationique Download PDF

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Publication number
EP0881279B1
EP0881279B1 EP98108983A EP98108983A EP0881279B1 EP 0881279 B1 EP0881279 B1 EP 0881279B1 EP 98108983 A EP98108983 A EP 98108983A EP 98108983 A EP98108983 A EP 98108983A EP 0881279 B1 EP0881279 B1 EP 0881279B1
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EP
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Prior art keywords
weight
granules
granulation
cationic surfactant
cationic surfactants
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
EP98108983A
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German (de)
English (en)
Other versions
EP0881279A3 (fr
EP0881279B2 (fr
EP0881279A2 (fr
Inventor
Rene-Andres Dr. Dipl.-Chem. Artiga Gonzalez
Monika Dr. Dipl.-Chem. Böcker
Christian Dr. Dipl.-Chem. Block
Stefan Hammelstein
Heinke Jebens
Judith Dr. Dipl.-Chem. Scherler
Berthold Dr. Dipl.-Chem. Schreck
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.)
Cognis IP Management GmbH
Original Assignee
Cognis Deutschland GmbH and Co KG
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Application filed by Cognis Deutschland GmbH and Co KG filed Critical Cognis Deutschland GmbH and Co KG
Publication of EP0881279A2 publication Critical patent/EP0881279A2/fr
Publication of EP0881279A3 publication Critical patent/EP0881279A3/fr
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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
    • C11D17/0034—Fixed on a solid conventional detergent ingredient
    • 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
    • C11D1/38—Cationic compounds
    • C11D1/62—Quaternary ammonium 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
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets

Definitions

  • the invention is in the field of the production of cationic surfactant-containing granules, such as for example in special detergents and cleaning agents, but also in Fabric softeners are used.
  • Cationic surfactants are used in special detergents and cleaning agents, but especially in Laundry post-treatment agents such as fabric softeners are used to achieve the appropriate agents treated textiles a soft, fluffy feel and to give pleasant wearing properties. It also makes it easier on the textiles applied cationic surfactant ironing and leads to an antistatic effect that in turn, the wearing properties improved.
  • the cationic surfactants are usually in the form of dispersions in the liquid to pasty agent incorporated.
  • German published patent application DE 32 43 983 (Degussa AG) describes a free-flowing plasticizer concentrate which consists of one or more cationic surfactants which, if appropriate in a mixture with one or more solubilizers, are applied to synthetic silica.
  • the agents are prepared by mixing a melt or a solution of the cationic surfactant in isopropanol with the precipitated and spray-dried silica.
  • Powdery fabric softening detergents which contain cationic surface-active substances adsorbed on highly absorbent silica are also described in German Offenlegungsschrift DE 34 02 437 (REWO Chemische Werke GmbH).
  • the cationic surfactants are applied as a melt or solution in isopropanol to the silica in the mixer and then granulated under shear.
  • German patent DE 43 08 794 (Henkel KGaA) describes special solid cationic surfactant preparation forms which are obtained by alkylation of triethanolamine esters in the presence of suitable dispersants (in particular fatty alcohols).
  • suitable dispersants in particular fatty alcohols.
  • the products obtained in this way have a flake-like structure and low bulk densities.
  • the first two methods have the disadvantage that the cationic surfactant is applied to an insoluble carrier in the form of its isopropanol solution or as a melt.
  • extensive occupational health and safety measures are required, and the isopropanol must also be removed again later by evaporation, since alcohols have a negative effect on the powder properties of detergent compositions.
  • energy is required to melt the cationic surfactant.
  • silica in large amounts also leads to the formation of residues in the treated textiles when used in detergents and fabric softeners. All processes of the prior art have the disadvantage in common that they deliver products which are only poorly soluble or not soluble without residues. The latter process also provides products with an undesirable low bulk density.
  • the object of the invention was to provide a method for manufacturing to provide cationic surfactant-containing granules which the process and Overcomes product disadvantages.
  • the invention further relates to a process for the preparation of cationic surfactants Granules, in which a solid carrier is placed in a mixer under low Energy input with a cationic surfactant and then with the addition of Water or an aqueous solution of one or more granulating aids under high Granular energy input.
  • the cationic surfactant can be added directly to the mixer in its delivery form, or in the form of a liquid to pasty cationic surfactant preparation form on the solid Carriers are injected.
  • Such forms of cationic surfactants can be for example by mixing commercially available cationic surfactants with auxiliaries such as Manufacture non-ionic surfactants, polyethylene glycols or polyols. Even lower ones Alcohols such as ethanol and isopropanol can be used, the amount of such lower alcohols in the liquid cationic surfactant preparation form from the reasons mentioned above should be below 10 wt .-%.
  • Solid cationic surfactants are simply added and act on the carrier in the course of the granulation; Cationic delivery forms other physical states are added, poured in or depending on the viscosity atomized.
  • Carriers from the group of alkali metal sulfates, carbonates, silicates, citrates, aluminum silicates and citric acid are preferred. Are particularly preferred water-soluble carriers and in particular sodium sulfate.
  • cellulose and Starch and its derivatives preferred carrier materials.
  • These include in particular cellulose and starch itself, however also cellulose and starch derivatives, which are obtained from cellulose by polymer-analogous reactions or starch are available.
  • Such chemically modified celluloses or starches include, for example, products from esterifications or etherifications in which Hydroxy hydrogen atoms have been substituted.
  • celluloses or starches in which the hydroxy groups versus functional groups that do not have a Oxygen atoms are bound, have been replaced, can be used as a carrier material.
  • alkali celluloses CMC
  • CMS Carboxymethyl cellulose
  • cellulose and starch esters and ethers as well as aminocelluloses and starches.
  • the amount of solid carrier in the resulting granules 50 to 80 wt .-% of the weight of the resulting granules.
  • Cationic surfactants used for the process according to the invention are all customary surface-active substances into consideration, with cationic surfactants with fabric softening Effect are clearly preferred.
  • Cationic surfactants used for the process according to the invention are all customary surface-active substances into consideration, with cationic surfactants with fabric softening Effect are clearly preferred.
  • the granules are produced by placing the solid support in a mixer and then applied the cationic surfactant with low energy input. Then one or more granulation aids in the form of an aqueous Solution added and the mixture wet granulated with high energy input.
  • Low energy input means in the sense of the method according to the invention slow-running mixing tools or the omission of additional Chopping units.
  • This low energy input is further characterized by that the agitator shaft of the mixer does not swirl the mix, but rather a kind "Pile mixing” is carried out. where the mix in the mixer in Direction of rotation is raised.
  • High energy input means in the sense of inventive method a rapid rotation of the mixing tools or Use of additional shredding units.
  • particles from the Gutbed swirled into the free mixing room and the mixture more and more fluidized. In this state, the particles fill the mixer in the form of a cloud, the so-called “mechanically generated fluidized bed”. With further increasing speeds the product is finally placed on the mixer wall in the form of a mix hurled that rotates there.
  • the method according to the invention can be used both in high intensity and in slow-speed mixers are performed, the high-intensity mixers in the first process stage to be operated slowly and the second Process stage required energy input in the slow-running mixers Additional units such as knife wreaths are provided.
  • high-speed mixers are the Lödige® CB 30 recycler, the Schugi® granulator, the Eirich® mixer type R or the Drais® K-TTP 80
  • examples of slow-running Mixing granulators are the Drais® K-T 160 and the Lödige® KM 300. The latter becomes often referred to as "Lödige ploughshare mixers".
  • aqueous solutions Solutions of carboxymethyl cellulose (CMC), water glass or citric acid are all auxiliary substances commonly used in wet granulation used.
  • CMC carboxymethyl cellulose
  • the process according to the invention particularly advantageously uses aqueous solutions Solutions of carboxymethyl cellulose (CMC), water glass or citric acid.
  • CMC carboxymethyl cellulose
  • the aqueous solutions have a dependency on the particular granulation aid different concentrations of the substances used. This is how CMC for example in 0.2 to 5% by weight aqueous solutions, water glass in the form 10 to 40 wt .-% warmer solutions and citric acid than 5 to 30 wt .-% aqueous Solution used.
  • the method according to the invention can also be used as pure water without dissolved ingredients Use granulating aids without losing their advantages.
  • the water or the aqueous solutions of the granulation aids are used in amounts of 1 to 5, preferably from 2 to 4% by weight, based on the weight of the resulting granules, added in the second process stage.
  • the granulated particles which arise in the process according to the invention can subjected to customary post-treatment steps for detergents and cleaning agents become.
  • drying of the granules in the fluidized bed is possible Connection to the granulation preferred.
  • powdering, rounding or a different surface treatment can be applied directly to the granulation or to a connect any drying
  • the cationic surfactant-containing granules according to the invention contain 5 to 40% by weight of one or several textile softening agents of the above formulas I, II or III, 50 up to 90% by weight of a solid carrier from the group of alkali metal sulfates and carbonates, silicates, citrates and aluminum silicates and citric acid as well as natural polysaccharides and their derivatives as well as 0 to 5, preferably 0.1 to 5 wt .-% of one or more granulation aids, each based on the Weight of the granulate.
  • a solid carrier from the group of alkali metal sulfates and carbonates, silicates, citrates and aluminum silicates and citric acid as well as natural polysaccharides and their derivatives as well as 0 to 5, preferably 0.1 to 5 wt .-% of one or more granulation aids, each based on the Weight of the granulate.
  • Granules containing cationic surfactants are preferred in which the Cationic surfactant component a) is a quaternized triethanolamine ester.
  • preferred Granules containing cationic surfactants contain sodium sulfate as solid carrier component b).
  • Granulation aids c) are preferably one or more substances selected from the Group of cellulose derivatives, water glasses or organic salts used.

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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)
  • Detergent Compositions (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Glanulating (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Claims (11)

  1. Granulé contenant un agent tensioactif cationique, solide contenant :
    a) de 5 à 40 % en poids d'un ou plusieurs agents assouplissants pour les textiles, cationiques de formule I
    Figure 00180001
    Figure 00180002
    Figure 00180003
    dans lesquelles chaque groupe R1 indépendamment l'un de l'autre est choisi parmi les groupes alkyle en C1-C6, alkényle ou hydroxyalkyle ; chaque groupe R2, indépendamment l'un de l'autre, est choisi parmi les groupes alkyle en C8-C28 ou alkényle ; R3 = R1 ou (CH2)n-T-R2 ; R4 = R1 ou R2 ou (CH2)nT-R2 ; T = -CH2-, -O-CO- ou -CO-O- et n est un nombre entier allant de 0 à 5,
    b) de 50 à 90 % en poids d'un support solide choisi dans le groupe des sulfates, des carbonates, des silicates, des citrates et des aluminosilicates de métal alcalin et l'acide citrique ainsi que des polysaccharides naturels et leurs dérivés,
    c) de 0 à 5 % d'un ou plusieurs auxiliaires de granulation,
    à chaque fois rapporté au poids de granulé.
  2. Granulé contenant un agent tensioactif cationique selon la revendication 1,
    caractérisé en ce que
    le composant d'agent tensioactif cationique a) est un ester de triéthanolamine quaternisé.
  3. Granulé contenant un agent tensioactif cationique selon l'une des revendications 1 ou 2,
    caractérisé en ce que
    le composant de support solide b) est du sulfate de sodium.
  4. Granulé contenant un agent tensioactif cationique selon l'une des revendications 1 à 3,
    caractérisé en ce que
    le composant de support solide b) est choisi parmi les polysaccharides naturels et leurs dérivés parmi lesquels l'amidon est préféré.
  5. Granulé contenant un agent tensioactif cationique selon l'une des revendications 1 à 4,
    caractérisé en ce que
    l'auxiliaire de granulation c) est une ou plusieurs des substances choisies dans le groupe des dérivés de la cellulose, des silicates solubles ou des sels organiques et est mis en oeuvre en quantités allant de 0,1 à 5 % en poids.
  6. Procédé de préparation de granulés contenant un agent tensioactif cationique,
    caractérisé en ce qu'
    on met en contact un support solide dans un mélangeur avec faible introduction d'énergie, avec un agent tensioactif cationique et ensuite on granule en ajoutant de l'eau ou une solution aqueuse d'un ou plusieurs auxiliaires de granulation sous introduction élevée d'énergie.
  7. Procédé selon la revendication 6,
    caractérisé en ce que
    le support solide représente de 50 à 80 % en poids du poids du granulé qui a été formé.
  8. Procédé selon l'une des revendications 6 ou 7,
    caractérisé en ce que
    la mise en contact avec l'agent tensioactif cationique s'effectue par pulvérisation d'une forme de préparation liquide à pâteuse d'agent tensioactif cationique.
  9. Procédé selon l'une des revendications 6 à 8,
    caractérisé en ce que
    la solution aqueuse d'un ou plusieurs auxiliaires de granulation est ajoutée en quantités de 1 à 5, de préférence de 2 à 4 % en poids rapporté au poids du granulé qui s'est formé.
  10. Procédé selon l'une des revendications 6 à 9,
    caractérisé en ce qu'
    à la suite de la granulation, on effectue un séchage du granulé en lit fluidisé.
  11. Procédé selon l'une des revendications 6 à 10,
    caractérisé en ce que
    les granulés formés sont retraités à la suite de la granulation par saupoudrage, mise en forme arrondie ou traitement en surface d'un autre type.
EP98108983A 1997-05-26 1998-05-18 Granules contenant un tensioactif cationique Expired - Lifetime EP0881279B2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19721885A DE19721885A1 (de) 1997-05-26 1997-05-26 Verfahren zur Herstellung kationtensidhaltiger Granulate
DE19721885 1997-05-26

Publications (4)

Publication Number Publication Date
EP0881279A2 EP0881279A2 (fr) 1998-12-02
EP0881279A3 EP0881279A3 (fr) 1999-06-16
EP0881279B1 true EP0881279B1 (fr) 2003-01-02
EP0881279B2 EP0881279B2 (fr) 2007-04-18

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ID=7830469

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EP98108983A Expired - Lifetime EP0881279B2 (fr) 1997-05-26 1998-05-18 Granules contenant un tensioactif cationique

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EP (1) EP0881279B2 (fr)
AT (1) ATE230431T1 (fr)
DE (2) DE19721885A1 (fr)
ES (1) ES2189034T5 (fr)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB0207483D0 (en) 2002-03-28 2002-05-08 Unilever Plc Fabric conditioning compositions
GB0207484D0 (en) 2002-03-28 2002-05-08 Unilever Plc Solid fabric conditioning compositions
EP1502942A1 (fr) * 2003-07-29 2005-02-02 Clariant International Ltd. Composition adoucissante solide
US11441106B2 (en) * 2017-06-27 2022-09-13 Henkel Ag & Co. Kgaa Particulate fragrance enhancers
EP4405451A1 (fr) * 2021-09-22 2024-07-31 Unilever IP Holdings B.V. Composition d'adoucissant pour tissu

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Also Published As

Publication number Publication date
DE19721885A1 (de) 1998-12-03
EP0881279A3 (fr) 1999-06-16
ATE230431T1 (de) 2003-01-15
ES2189034T3 (es) 2003-07-01
DE59806786D1 (de) 2003-02-06
EP0881279B2 (fr) 2007-04-18
ES2189034T5 (es) 2007-11-16
EP0881279A2 (fr) 1998-12-02

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