EP0876469A1 - Procede de preparation de detergents et de nettoyants granulaires ou constituants utilises pour les preparer - Google Patents

Procede de preparation de detergents et de nettoyants granulaires ou constituants utilises pour les preparer

Info

Publication number
EP0876469A1
EP0876469A1 EP96938109A EP96938109A EP0876469A1 EP 0876469 A1 EP0876469 A1 EP 0876469A1 EP 96938109 A EP96938109 A EP 96938109A EP 96938109 A EP96938109 A EP 96938109A EP 0876469 A1 EP0876469 A1 EP 0876469A1
Authority
EP
European Patent Office
Prior art keywords
granules
weight
acid
cleaning agents
components
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.)
Withdrawn
Application number
EP96938109A
Other languages
German (de)
English (en)
Inventor
Manfred Greger
Karl-Martin Faeser
Volker Bauer
Norbert Kühne
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.)
Henkel AG and Co KGaA
Original Assignee
Henkel AG and Co KGaA
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 Henkel AG and Co KGaA filed Critical Henkel AG and Co KGaA
Publication of EP0876469A1 publication Critical patent/EP0876469A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/22—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by pressing in moulds or between rollers
    • 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

Definitions

  • Homogenizing devices conventional granulating devices, for example pellet press extruders with one or two shafts, planetary roller extruders and other apparatuses, can be used.
  • a continuously operating twin-screw extruder is preferred.
  • the premix which is plasticized in the extruder, emerges in the form of fine strands through a perforated die plate.
  • the extrudate is then removed by means of a rotating cutting knife into almost spherical to cylindrical granules and this still plastic PMR granulate preferably rounded off in a conventional rounding machine, if necessary using small amounts of dry powder.
  • other active ingredients in particular temperature-sensitive recipe components, can be added to the dried-on granulate, or sprayed on and sprayed on formed grain can be mixed to form a multigrain mixture
  • the extrusion is carried out by means of a circular plate provided with nozzle bores.
  • the hole nozzles can be arranged vertically or horizontally.
  • the fine strands of approximately 0.5 to 5 mm, typically of 0.8, emerging through the hole shapes mm to 2.0 mm diameter are in a hot cut from a single or multi-bladed Rotating cutter head crushed into almost spherical to cylindrical granules.
  • the knife sheaths of the cut-off day device either lie on the nozzle plate with a low contact pressure or form a gap with the plate that is very small compared to the diameter of the perforated nozzles.
  • the homogeneous and solid, ⁇ eselfahiges premix must be of such consistency that it is plastically softened and extrudable under the pressure or under the entry of specific work, but that at the time of the exit from the hole shape, at which no more shear forces act on the system , the viscosity of the system is suddenly reduced in such a way that the extruded strand can be cut, to be precise cut to predetermined dimensions
  • a disadvantage of this prior art method is that energy losses in the form of temperature increases occur under the high working pressure, so that the extruder housing, including the extruder pelletizing head, normally has to be cooled in order to prevent the viscosity of the premix from being so already during the extrusion drops sharply that an actual extrusion is no longer possible. Too high temperature increases also lead to the fact that temperature-sensitive ingredients, for example bleaching agents such as perborate or percarbonate, could not be used without cooling the housing
  • gear press rolls are commercially available.For example, they can be purchased as granulate molding machines, in particular of the G series from Bepex GmbH, Leingart, Federal Republic of Germany.
  • the granulate molding by means of a gear press roll takes place in such a way that the feed material is drawn in by the toothed rolls and through which Nozzle holes are pressed as part of this Press rollers use hollow gears with nozzle holes in the tooth base. Scraper blades fitted inside the wheel cut off the emerging pellets.
  • the compression that can be achieved in addition to shaping is determined by the number of nozzles, the nozzle pressure and the ratio of nozzle diameter to nozzle length.
  • the gear wheels used in the press roll according to the invention for molding the granules are hollow and have nozzle bores in the tooth base.
  • a pressure of 10 to 200 bar, preferably 10 to 130 bar, in particular 30 to 60 bar, builds up within the press rolls, and the scraper blades present in the interior of the wheel or in the outlet of the press roll produce a granulate content of 0.5 to 10 mm, preferably 1 to 5 mm.
  • plasticized premixes are supplied to the gear press rolls, which are 2 to 100% by weight, preferably 10 to 45% by weight and in particular above 10% by weight, for example 15 to 40% by weight .-% returned shares. It is not necessary to grind the coarse particles into smaller grains beforehand.
  • plasticizers and / or lubricants used as auxiliaries can be solid, flowable, gel-like or pasty at room temperature without the need to use an additional liquid phase.
  • Preferred plasticizers and / or lubricants are preparations based on surfactant components and / or based on water-soluble or water-emulsifiable or water-dispersible
  • plasticizers and / or lubricants examples include numerous types of the nonionic surfactants commonly used in detergents and cleaning agents.
  • Substances with a low melting point for example higher molecular weight polyethylene glycol ethers with molecular weights between 4,000 and 20,000 can be used as plasticizers and / or lubricants which are solid at room temperature
  • the pastes are preferably used in amounts not exceeding 12% by weight, in particular in amounts between 0.5 and 10% by weight, and with particular advantage between 3 and 8% by weight, based on the total mixture. At least 30 are particularly suitable % By weight, preferably 40% by weight pastes and gels
  • the surfactant components so formed form in which the granules formed dry Binder-like top and intermediate layers, which are jointly responsible for the cohesion of the grains can be anionic surfactant salts, in particular sulfates and sulfonates, from the wide range of compounds proposed here for detergents and cleaning agents, optionally in admixture with customary, nonionic compounds Particular importance is to be taken as an example in the production of textile detergents, a feed mixture of at least two solid components (spray-dried granules / fatty alkyl sulfate compound) with or without the addition of sodium piperborate (monohydrate and / or tetrahydrate) with the addition of 2 to 5% by weight of water and 4 to 8% by weight of a 55 to 65% Cg to C 3 alkylbenzenesulfonate paste (ABS paste) instead of the aforementioned combination of spray-dried granules and a fatty alkyl
  • ABS paste 55 to 65% C
  • APG alkyl polyglycoside
  • polymer compounds are distinguished by a pronounced lubricating character, which provides the decisive processing aid in the processes according to the invention.
  • these polymer components dry out in the formation of the granulate granules according to the invention into polymer films which, on the one hand, promote the connection of the grain and, on the other hand, easily return to the state of the solution or emulsification or dispersion when aqueous media are added.
  • the granules can then be fed to a rounding step as in international patent application WO-A-91/02047.
  • Usual rounding devices such as Marumerizer, but also sieve mills, as are commercially available from Bepex GmbH, for example, can be used here.
  • Sieve mills of this type have the advantage that any coarse particles that may have occurred are reduced to a maximum grain size limit and the fractions of finer granules that are produced in this way can also be returned to the premix.
  • the finally formed granulate granulate is preferably fed to a drying step, for example a fluidized bed dryer, in which, at moderately raised supply air temperatures, in particular up to a maximum of 80 ° C., correspondingly moderate final product temperatures of, for example, between 55 to 60 ° C. are set, but then not exceeded become.
  • a drying step for example a fluidized bed dryer, in which, at moderately raised supply air temperatures, in particular up to a maximum of 80 ° C., correspondingly moderate final product temperatures of, for example, between 55 to 60 ° C. are set, but then not exceeded become.
  • the product is cooled with cold air, for example.
  • the content of free water in the granulate can be reduced.
  • Preferred residual contents of unbound water are about 1% by weight, preferably in the range of about 0.1 to 0.5% by weight.
  • the resulting, very low-dust product can be classified, for example sieved, to remove small coarse particles.
  • the "internal drying" of the granules is also possible: by using moisture-binding components in the premix in the short processing time, the plasticizing effect of the liquid components presented can be used. Then, by binding at least partial components of these liquid components through the mixed-in components, the granules are dried "from the inside out", so that the external drying can be shortened or omitted entirely.
  • Components which are able to bind water in the form of stall water are, for example, sodium sulfate and / or sodium carbonate in anhydrous or low-water form or else a zeolite which has been partially freed from water of crystallization
  • granule systems are used which represent a combination of granules of different compositions.This way, the storage-stable combination of potentially reactive or at least only partially compatible components is achieved.
  • this is conventional textile detergents, but now in this preparation form at least two Using granulate types in a mixture with one another
  • the bleaching agent component in particular perborate or sodium carbonate containing water from the water, is pelletized with the use of a proportion of the plasticizers and / or lubricants.
  • the material densities in the grain and thus also the bulk density of the granules are largely determined by the working pressures used in pressing the homogenized material through the perforated plates.
  • Bulk densities in the range from 850 to 980 g / l can be set on the basis of commercially available textile detergent formulations, with good flowability and a preferably high, uniform, spherical grain structure.
  • free-flowing granules in the dry state with uniform bulk densities of 950 to 980 g / l were achieved with an average particle size of the spherical granules in the range of, for example, about 1 mm.
  • the method according to the invention is characterized by a very low proportion of returned goods.
  • This portion of the return material after sieving the granules through a 1.6 mm sieve was in each case in the range of at most 10% by weight.
  • sensitive formulation components for example activators for bleaching agents, enzymes, defoamers, in particular silicone defoamers, perfume and the like, can be added to the granules. Even then, detergent products with bulk densities in the range of about 900 g / l are still obtained.
  • the textile detergents which are customary on the market today in the form of free-flowing powders and / or granules generally contain a combination of anionic-surfactant and non-surfactant active detergent components.
  • the anionic surfactant components make up the largest proportion and the nonionic surfactants make up the smaller proportion of the surfactant mixture.
  • textile detergent concentrates with surfactant contents can be up to 35% by weight and preferably in the range from about 15 to 25% by weight.
  • nonionic surfactants usually used in detergents and cleaning agents are no problem, the pluming effects occurring in the spray drying, see definition in Rompp chemical lexicon, 4 edition, volume 5, page 3488, are omitted.
  • the nonionic surfactants are easily added by incorporation into the mixture of substances before the press step, they can even provide valuable process help in the manner described here as a highly concentrated, aqueous gel or paste
  • the invention relates to universal detergents for textiles which are present in this form of the free-flowing granules with bulk densities above 750 g / l, in particular above 800 g / l, for example in the range from 850 to 950 g / l and in a particularly important one Embodiment are characterized by a uniform particle shape and size.
  • the preferred particle shape is spherical. Preferred particle sizes here are in the range from 0.5 to 10 mm ball diameter, in particular in the range from approximately 1 to 5 mm.
  • the formulation components can correspond to the textile detergents that are commonly used today.
  • Suitable anionic surfactants are, for example, those of the sulfonate and sulfate type.
  • the surfactants of the sulfonate type are alkylbenzenesulfonates (Cg to C 13 alkyl), olefin sulfonates, ie mixtures of alkene and hydroxyalkanesulfonates and disulfonates, such as those obtained from C 2 to C 18 monoolefins with a terminal or internal double bond by sulfonation Gaseous sulfur trioxide and subsequent alkaline or acidic hydrolysis of the sulfonation products.
  • alkanesulfonates which are obtainable from C1 2 - to Ciralkanes by sulfochlorination or sulfoxidation and subsequent hydrolysis or neutralization or by bisulfite addition to olefins, and in particular the esters of ⁇ -sulfofatty acids (ester sulfonates), for.
  • esters of ⁇ -sulfofatty acids esters of ⁇ -sulfofatty acids (ester sulfonates)
  • B. the ⁇ -sulfonated methyl esters of hydrogenated coconut, palm kernel or tallow fatty acids for.
  • Suitable surfactants of the sulfate type are the sulfuric acid monoesters from primary alcohols of natural or synthetic origin, in particular from fatty alcohols, e.g. B. from coconut fatty alcohol, tallow fatty alcohol, oleyl alcohol, lauryl, myristyl, cetyl or stearyl alcohol or the C 10 -C 2 o-oxo alcohols, and those secondary alcohols of this chain length.
  • the sulfuric acid monoesters with 1 to 6 moles of ethylene oxide ethoxylated alcohols, such as 2-methyl-branched C 9 -Cn alcohols with an average of 3.5 moles of ethylene oxide, are also suitable.
  • Preferred fatty alkyl sulfates are derived from fatty alcohol mixtures obtained from coconut oil, palm and palm kernel oil, which additionally contain proportions of unsaturated alcohols, e.g. B. oleyl alcohol, may contain. Mixtures in which the proportion of the alkyl radicals is 30 to 70 find a preferred use % By weight on C 12 to 18 to 30% by weight on C 14 , 5 to 15% by weight on C 16 , less than 3% by weight on C 10 and 0 to 40% by weight on C 18 are distributed. Sulfated fatty acid monoglycerides are also suitable.
  • the anionic surfactants can be present in the form of their sodium, potassium or ammonium salts and as soluble salts of organic bases, such as mono-, di- or triethanolamine.
  • the anionic surfactants are preferably present in the form of their sodium or potassium salts.
  • the content of anionic surfactants or anionic surfactant mixtures in detergents according to the invention is preferably 5 to 40% by weight, in particular 8 to 30% by weight.
  • Addition products of 1-40, preferably 2-20 moles of ethylene oxide to one mole of an aliphatic compound having essentially 10-20 carbon atoms from the group of alcohols, carboxylic acids, fatty amines, carboxamides and alkanesulfonamides can be used as nonionic surfactants.
  • bleach activators are N.N.N'.N'-tetraacetylethylene diamine, 1,4-diacetyl-2,4-dioxo-hexahydro-1,3,5-triazine, furthermore carboxylic acid anhydrides and esters of polyols, such as glucose pentaacetate.
  • Suitable substitutes or partial substitutes for phosphates and zeolite are crystalline, layered silicates of the general formula NaMSi x O 2 _ * ⁇ yH 2 O, where M is sodium or hydrogen, x is a number from 1, 9 - 4 and y is a number from 0 - 20 is.
  • Layered silicates of this type are described, for example, in European patent application 0164514.
  • both ⁇ - and ⁇ -sodium disilicates Na 2 Si 2 ⁇ 5 • yH 2 O are preferred.
  • Further builder substances are amorphous silicates with secondary washing power, for example those according to DE-P44 00 024.3, DE-P44 19 745.4 and DE-P44 46 363.4.
  • zeolite and / or the crystalline sheet silicate and / or the amorphous silicate are preferably used either alone or with a zeolite to crystalline layered silicate or amorphous silicate weight ratio with secondary washing power of 10: 1 to 1: 3 and in particular 3: 1 to 1: 1.
  • Copolymers of acrylic acid with maleic acid which contain 50 to 90% by weight of acrylic acid and 50 to 10% by weight of maleic acid, have proven to be particularly suitable.
  • Their relative molecular weight, based on free acids, is generally 5,000 to 200,000, preferably 10,000 to 120,000 and in particular 50,000 to 100,000.
  • biodegradable polymers for example those which, according to DE-A-43 00 772, are salts of monomers acrylic acid and maleic acid as well as vinyl alcohols or vinyl alcohol derivatives or according to DE-C-42 21 381 as monomers salts of acrylic acid and 2-alkyiallylsulfonic acid and sugar derivatives.
  • copolymers are those which are described in German patent applications DE-A-43 03 320 and P 44 17 734.8 and which preferably contain acrolein and acrylic acid / acrylic acid salts or acrolein and vinyl acetate as monomers.
  • phosphate can also be used, in particular pentasodium triphosphate, optionally also pyrophosphates such as orthophosphates, which act primarily as precipitants for lime salts.
  • pentasodium triphosphate optionally also pyrophosphates such as orthophosphates, which act primarily as precipitants for lime salts.
  • the phosphate content based on pentasodium triphosphate, is below 30% by weight.
  • agents without a phosphate content are preferably used here.
  • Suitable non-active foam inhibitors are, for example, organopolysiloxanes and mixtures thereof with microfine, optionally silanized silica and also paraffins, waxes, Mikrok ⁇ stallinwachse and mixtures thereof with silanized silica also of C 12 - to C ⁇ o-alkylamines and Cr to C ⁇ .
  • Bisacylamides derived from dicarboxylic acids can be used.
  • Mixtures of various foam inhibitors for example those of silicones, paraffins or waxes, are also advantageously used.
  • the foam inhibitors are preferably bound to a granular, water-soluble or dispersible carrier substance or are admixed with the plasticizers and / or lubricants
  • the agents can contain enzyme stabilizers.
  • enzyme stabilizers For example, 0.5 to 1% by weight sodium formate can be used. It is also possible to use proteases with soluble calcium salts and a calcium content of preferably about 1.2 % By weight, based on the enzyme, are stabilized.
  • boron compounds for example boric acid, boron oxide, borax and other alkali metal borates, such as the salts of orthoboric acid (H 3 BO 3 ), metaboric acid (HBO 2 ) and pyrobic acid (tetraboric acid H 2 B 4 O 7 ), is particularly advantageous. .
  • the present invention relates to washing and cleaning agents containing granules of the aforementioned type, which are characterized in that they contain a surfactant content of up to 35% by weight, preferably 15 to 25% by weight.
  • the solid components were placed in a batch mixer of 130 l, which was equipped with a cutter head shredder, and then with the mixer running, the premixed nonionic surfactant / PEG 400 mixture and then the carboxylate solution were added and the mixture was mixed for 30 seconds.

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

Abstract

L'invention concerne un procédé permettant de comprimer des prémix solides coulants, selon lequel le processus peut se dérouler dans des conditions impliquant moins de risques d'altération des produits, comparativement aux procédés similaires classiques. A cette fin, les moules perforés à travers lesquels les prémix sont comprimés, sont disposés dans deux rouleaux de compression à roues dentées tournant en sens contraire et en prise. D'éventuelles fractions à gros grains peuvent le cas échéant être renvoyées sans broyage.
EP96938109A 1995-11-15 1996-11-06 Procede de preparation de detergents et de nettoyants granulaires ou constituants utilises pour les preparer Withdrawn EP0876469A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19542570 1995-11-15
DE1995142570 DE19542570A1 (de) 1995-11-15 1995-11-15 Verfahren zur Herstellung von granularen Wasch- oder Reinigungsmitteln oder Komponenten hierfür
PCT/EP1996/004841 WO1997018290A1 (fr) 1995-11-15 1996-11-06 Procede de preparation de detergents et de nettoyants granulaires ou constituants utilises pour les preparer

Publications (1)

Publication Number Publication Date
EP0876469A1 true EP0876469A1 (fr) 1998-11-11

Family

ID=7777528

Family Applications (1)

Application Number Title Priority Date Filing Date
EP96938109A Withdrawn EP0876469A1 (fr) 1995-11-15 1996-11-06 Procede de preparation de detergents et de nettoyants granulaires ou constituants utilises pour les preparer

Country Status (3)

Country Link
EP (1) EP0876469A1 (fr)
DE (1) DE19542570A1 (fr)
WO (1) WO1997018290A1 (fr)

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1569996A (fr) * 1968-04-23 1969-06-06
US3947938A (en) * 1974-01-22 1976-04-06 Iu Conversion Systems, Inc. Roll-pelletizer and rolls therefor for making uniform particle size pellets
DE3834785C1 (en) * 1988-10-12 1989-05-24 Gebr. Kaiser Maschinenfabrik, 4150 Krefeld, De Apparatus for generating granules or pellets from flowable material
DE4336548C2 (de) * 1992-11-14 1994-11-17 Degussa Verfahren zur Herstellung kugelförmiger Granulate aus pulverförmigen Feststoffen
DE4329064A1 (de) * 1993-08-28 1995-03-02 Henkel Kgaa Gerüststoffkomponente für Wasch- oder Reinigungsmittel
DE4415362A1 (de) * 1994-05-02 1995-11-09 Henkel Kgaa Verfahren zur Herstellung silikatischer Buildergranulate mit erhöhtem Schüttgewicht

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO9718290A1 *

Also Published As

Publication number Publication date
DE19542570A1 (de) 1997-05-22
WO1997018290A1 (fr) 1997-05-22

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