EP1257628B1 - Agglomeres contenant du mineral en feuillets et des tensioactifs non ioniques - Google Patents

Agglomeres contenant du mineral en feuillets et des tensioactifs non ioniques Download PDF

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Publication number
EP1257628B1
EP1257628B1 EP01919340A EP01919340A EP1257628B1 EP 1257628 B1 EP1257628 B1 EP 1257628B1 EP 01919340 A EP01919340 A EP 01919340A EP 01919340 A EP01919340 A EP 01919340A EP 1257628 B1 EP1257628 B1 EP 1257628B1
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Prior art keywords
agglomerates
weight
relation
bentonite
component
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German (de)
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EP1257628A1 (fr
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Ulrich Sohling
Norbert Schall
Wolfgang Heininger
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Sued Chemie AG
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Sued Chemie AG
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    • 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
    • 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
    • C11D1/66—Non-ionic 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
    • C11D1/66—Non-ionic compounds
    • C11D1/74—Carboxylates or sulfonates esters of polyoxyalkylene glycols
    • 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
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0047—Detergents in the form of bars or tablets
    • C11D17/0065—Solid detergents containing builders
    • C11D17/0073—Tablets
    • C11D17/0086—Laundry tablets
    • 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
    • C11D3/1253—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite
    • C11D3/126—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite in solid compositions

Definitions

  • the invention relates to layer silicate-containing agglomerates nonionic surfactants, a process for their preparation and their use as detergent additive.
  • Nonionic surfactants are increasingly being used in powder detergents used. The reasons are first in their good Washing properties even at low temperatures. This is possible This is in line with the trend towards lower washing temperatures in European countries and those already used for a long time low washing temperatures in America and Asia. Farther become the washing properties of nonionic surfactants not or only slightly influenced by a high water hardness. Also have nonionic surfactants to anionic Surfactants better cleaning properties for fatty Dirt as well as for synthetic fiber fabrics on.
  • nonionic surfactants Due to its liquid to waxy consistency that is Penetration of nonionic surfactants in larger quantities in powdered detergents, however, with some difficulty connected. This is how the use of nonionic surfactants leads in washing powders produced by a spraying process Be easy to gluing even during spray drying of the nozzles and to a swelling of the powder the evaporation of volatile contaminants in the nonionic surfactants.
  • the nonionic surfactants usually applied to the powder only after spray drying.
  • it allows the absorption capacity of not obtained from the spray-drying process, larger Apply or incorporate amounts of nonionic surfactants.
  • JP 0009087699 AA describes a granular nonionic A detergent composition containing a nonionic Surfactant, a clay mineral, such as montmorillonite, an oil-absorbing Carrier, such as amorphous silica, and a silicone. It may contain further additives, such as sodium silicate as a builder organic polyacrylate salt, also as builder, an optical one Brightener, an enzyme, a bleach and an extender present be. The ingredients are kneaded and extruded and then crushed. So it does not find a simple one Agglomeration instead.
  • JP 0011310791 describes a granular, nonionic Detergent composition containing a nonionic surfactant, a clay mineral and an oil-absorbing carrier. The Ingredients are mixed, kneaded, extruded and then crushed. A simple agglomeration process is not described.
  • US-A-4,861,510 describes porous detergent granules, containing sodium sulfate and synthetic phyllosilicates.
  • the granules are prepared by spray drying, wherein a porous granulate is formed, which acts on liquid surfactants can be.
  • the liquid absorption capacity is between 2 and 50 wt .-%, preferably up to 35 wt .-%.
  • the surfactant content is over 50%, and the Agglomerates are not produced by spray drying.
  • Tenside contents are calculated from the examples (based on anhydrous alcohol ethoxylate) from 10 to 20.5 Wt .-%.
  • the surfactant content is therefore well below 50 wt .-%.
  • There the surfactant uptake capacity of zeolite A is only 26% by weight, it is not possible on the basis of zeolite as sole carrier material granules with surfactant contents of produce more than 50%. This is not possible with Carrier mixtures of bentonites and zeolites, as bentonite granules absorb only a maximum of about 40 wt .-% surfactants can.
  • EP-A-0 690 123 describes a process for the preparation a powdered detergent, wherein (1) a builder (soda, Zeolite, STPP, trisodium nitrilotriacetate, citrates or Sulfates or mixtures thereof) with a nonionic surfactant (2) a barrier material (amorphous silicates / precipitated silicas) is added and (3) a further processing done with the builder to the final granules.
  • the total content of surfactant is 5 to 50 wt .-%, is therefore below the upper limit of the invention. Farther the products of the invention are only in maximum made two steps.
  • the inventive Agglomerates containing montmorillonite-containing phyllosilicates are only in maximum made two steps.
  • the object of the invention was therefore agglomerates with a high content to provide nonionic surfactants. not are sticky, do not "bleed” and release more quickly allow the nonionic surfactants in the wash liquor. Furthermore, in the release of nonionic Surfactants often observed to reduce gel effect as possible become. The resulting gel phases have a high Viscosity, which prevents rapid dissolution of the surfactants and may cause sticking of the particles upon dissolution cause.
  • inventive Agglomerates with the above composition very can absorb high levels of nonionic surfactants without that they become sticky or "bleed".
  • the agglomerates according to the invention can be particularly advantageous Washing powders are admixed, the above-mentioned Gelation effect on the one hand only on the agglomerates remains limited and not the entire detergent composition recorded, and on the other hand, surprisingly low fails.
  • the rapid Dissolution of agglomerate particles and rapid release ensures the non-ionic surfactants in the wash liquor, while avoiding incrustations on the laundry can be.
  • montmorillonite-containing silicates such as bentonite, as well as attapulgite, hectorite and / or beidellite in particular provide advantageous results.
  • natural or synthetic bentonites preferably Na bentonite
  • attapulgites preferably Na bentonite
  • Attapulgites preferably Na bentonite
  • Attapulgites preferably Na bentonite
  • Attapulgites preferably Na bentonite
  • synthetic phyllosilicates are used, for example synthetic hectorite.
  • a previous activation in particular an alkaline activation of the phyllosilicates, positive for the properties of the agglomerates according to the invention effect.
  • a particularly preferred embodiment is for example activated bentonite, in particular soda-activated bentonite used.
  • the amount of precipitated Silica in the agglomerates according to the invention adjusted that, on the one hand, they are at least 12% by weight, preferably at least 14% by weight, and in particular at least 16 wt .-%, based on the total amount of Support materials.
  • the layered silicate used in the manner of a "house of cards” or scaffolding a porous structure forms for receiving the nonionic surfactant, wherein the Structure stabilized by the highly porous precipitated silica and this with the three-dimensional layer silicate structure interacts.
  • the agglomerates according to the invention therefore, have a particularly high and relatively stable Porosity on. It is also believed that the precipitated silica a (partial) delamination of the layered silicate causes.
  • a compaction or extrusion is likely a more parallel alignment of the layered silicate platelets, which negatively affects the porosity of the agglomerates and their surfactant receptivity affects.
  • the amount of precipitated used Silica not more than 40% by weight, preferably not more than 30 Wt .-%, based on the total agglomerates.
  • the agglomerates according to the invention show surprisingly with the same surfactant content as agglomerates According to the prior art, a significantly lower stickiness.
  • agglomerates according to the invention are advantageously prepared in the usual sizes for detergent additives particle sizes, those skilled in the art are familiar.
  • agglomerates it is possible to use all conventional precipitated silicas known to the person skilled in the art.
  • starting material for the recovery of silicic acids by wet route are alkali silicate solutions, preferably soda water glass, from which amorphous silicic acid is precipitated by the addition of acid.
  • the precipitated product consists of 86 to 88% SiO 2 and 10 to 12% water which is physically bound both in the molecular structure and on the surface, as well as residues of the salt formed during the reaction and small amounts of metal oxide .
  • the most important precipitation parameters such as precipitation temperature, pH, electrolyte concentration and precipitation duration, it is possible to produce silicas with different surface properties.
  • Silicas can be produced in the range of specific surface areas of about 25 to 700 m 2 / g.
  • the silicic acid suspension obtained in the precipitation is dissolved in Filter presses transferred, wherein the solids content of the filter cake between about 15 and 20%.
  • the drying takes place according to different procedures, which is common Connect grinding and visual steps.
  • hydrophilic and hydrophobic silicas can be used be used, with hydrophobic silicic acids simultaneously can serve as a defoamer.
  • the silicas used in the present invention preferably have an average particle diameter from about 1 to 100 microns. In most cases will be Precipitated silicas with a high specific surface area and high adsorptive capacity, by the oil number or Dibutylphthalateahl (DBP number) according to DIN 53601 characterized is preferred.
  • DBP number Dibutylphthalateahl
  • All agglomerates can be prepared by a person skilled in the art use common nonionic surfactants. These include, without being limited to the group of alcohol ethoxylates or fatty alcohol polyethylene glycol ethers, the alkylpolyglycosides, the fatty alcohol polyglycol ether methyl ester, fatty acid methyl ester ethoxylates, the sorbitan ester or mixtures it. Preferred are fatty alcohol polyethylene glycol ethers, Alkyl polyglycosides, fatty acid methyl ester ethoxylates and Fettalkoholpolyglycolethermethylester.
  • fatty alcohol polyethylene glycol ethers Especially preferred are fatty alcohol polyethylene glycol ethers, fatty alcohol polyglycol ether methyl esters or mixtures of both.
  • fatty acid methyl ester ethoxylates Using of fatty acid methyl ester ethoxylates, the inventive Dissolve agglomerates surprisingly quickly.
  • fatty alcohol polyethylene glycol ethers those are preferred which are common in detergent applications, i. the Ethoxylation degrees between 1 and 12 and alkyl chain radicals having 10 to 17 carbon units. Fettalkoholpolyethylenglycolether with a few ethoxylate units preferably in mixtures with higher ethoxylated fatty alcohol polyethylene glycol ethers used.
  • the individual case preferred nonionic surfactants are of the specific ones Requirements for the detergent depending and can each be determined by the skilled person by means of routine experiments.
  • the agglomerates can be added in the The prior art contains known additives.
  • additives known in the art are added, such as e.g. Alcohols such as ethanol or glycerol, polyethylene glycols or hydrotropes such as Na cumene sulphonate.
  • polyethylene glycols In particular those are used which are low molecular weight Have masses, in particular 200 to 6000 g / mol. These are usually made prior to agglomeration with the surfactant mixed and in amounts of 0.1 to 30%, based on the Amount of surfactant used.
  • the inventive Agglomerates at least 52 wt .-%, in particular at least 55% by weight, more preferably at least 58% % By weight of nonionic surfactants, based on the total agglomerate.
  • the ratio of layered silicate to precipitated Silica, based on wt .-% in the inventive Agglomerates between 2: 1 and 1: 2.
  • the layered silicate and the precipitated silica in about the same amounts, based on wt .-%, before.
  • the agglomerates contain 10 to 15% by weight Bentonite, 5 to 15 wt .-% zeolite and 10 to 30 % By weight of precipitated silica, based on the total agglomerate.
  • the agglomerates according to the invention additionally contain additives known in the art may consist of a preferred embodiment the agglomerates consist essentially of nonionic surfactant, Phyllosilicate and precipitated silica, leaving one intimate contact between these components ensured is.
  • the above components make at least 85 wt .-%, in particular at least 90 wt .-%, and especially preferably 95 wt .-% of the agglomerates.
  • the additional Inclusion of at least one zeolite in the agglomerates leads to particularly positive results. It is known, that it is not readily possible agglomerates by agglomeration of zeolite with nonionic surfactant too obtained because of the fineness of the zeolites only heavy agglomerates with usual particle size in more satisfactory Make yield.
  • a preferred embodiment becomes intensive Mixing generates a mechanical fluidized bed.
  • the known in the art intensive mixer in batch or continuous processes be used.
  • Agglomeration becomes batchwise Batch mixers from Eirich, Hartheim, Loedige mixer (e.g., Loedige FKM mixer, Paderborn) or Drais (Drais Turbomix, Mannheim) in question.
  • at continuous process control can typically be mixer von Loedige, Paderborn (e.g., Loedige CB mixer), Drais, Mannheim (e.g., Drais CoriMix), of Ballestra, Milan, Italy (e.g., Ballestra Cetemix) or from Schugi-Leylistad, The Netherlands (e.g., Schugi Flexomix).
  • the production of the agglomerates is preferably carried out in one Intensive mixer by mixing the above-mentioned support materials with the surfactant.
  • the support materials component a, b, and optionally d
  • the surfactant or the Surfactant mixture which is optionally provided with other additives is, can be added in the pure state or mixed with water become. Preference is given to water contents between 0 and set about 50%. Particular preference is given to water contents between 0 and about 20%.
  • the use of pure surfactants agglomeration has the advantage that the resulting Agglomerates do not need to be dried. This also applies to surfactant-water mixtures which have water contents, those of the finished washing powder or Waschpulverformlinge correspond.
  • a particularly preferred embodiment takes place in a coating of the agglomerate particles to a second mixer, whereby the structure of the particles is obtained remains.
  • the coating of the agglomerate particles Zeolite, bentonite, talc or titanium dioxide powder If the agglomerates according to the invention already contain zeolite are, the coating can also be omitted, if one given sufficient degree of whiteness of Agglomeratteilchen and a further reduction of stickiness is not required.
  • no according to the present invention Crushing of the agglomerate particles.
  • Another aspect of the present invention is concerned layered mineral agglomerates with nonionic surfactants, which are obtainable by the above method.
  • the agglomerates are used as additives to detergents used. It is particularly advantageous that due to the very high content of nonionic surfactants only added quite small amounts of the detergent composition Need to become. This is also the aforementioned gel effect limited to the added agglomerates and due the composition of the agglomerates according to the invention quite low.
  • the added agglomerates meet both the function of providing a sufficient salary on nonionic surfactants as well as the increase of Soft grip of the wash.
  • Another aspect of the present invention relates to Detergent or a detergent additive, the or the Contains agglomerates according to the invention.
  • the agglomerates are used in detergents which are in Tablet form present.
  • agglomeration parameters were, if not stated otherwise, in the following each chosen so that more than 50% of the agglomerates in a particle size range from 0.2 to 1.2 mm.
  • the mean particle size can be like known in the art by routine choice the manufacturing parameters are modified.
  • the agglomerates were indicated, with inorganic powders such. Coated or zeolite coated.
  • a first variant was the material is transferred into a plastic bag, the inorganic one Powder was added and shaken for about 2 minutes.
  • the coating performed in Eirichmischer. This was after the agglomeration added the inorganic powder for coating and then the agglomerate / powder mixture again for 2 minutes mixed. The other results were comparable.
  • the time was the measurement of the surface tension of the solution the agglomerates used.
  • the measurement of the surface tension as a function of time the bubble pressure method was used with an online tensiometer, SITA-Online F10. to Recording of the measured curves was performed with a bubble frequency of 1 Hz worked.
  • the measurements were standardized samples used of particle sizes between 0.2 and 1.2 mm. It samples of 1 g were used, distilled in 200 ml Add water and stir with a length of 1.5 cm was stirred at a frequency of 150 revolutions.
  • the Surface tension can be used as a measure of this measurement Surfactant release serve. As a comparison, this was the following most widely used surfactant Genapol OA 070 in one concentration of 0.5 g / l used. Such a solution showed under the same measuring conditions a surface tension of 30-32 mN / m.
  • the bulk density was in the following Examples determined by adding 100 g of the agglomerates in a 1,000 ml can filled and shaken for about 30 seconds.
  • the measuring cylinder is weighed empty to 10 mg. On it is the Powder funnels with tripod and clamp over the opening of the cylinder attached. After starting the stopwatch of the Measuring cylinder within 15 seconds with the agglomerates filled. With the spatula is continuously poured filling, so that the measuring cylinder is always filled slightly overhanging is. After 2 minutes, the supernatant is removed by spatula, being careful that no pressing forces compact the material in the cylinder. The filled measuring cylinder is brushed and weighed.
  • Bulk density is expressed in g / l.
  • General allow the bulk densities obtained of more than 600 g / l, in particular of more than 650 g / l, also a use of the invention Agglomerates in common compact detergents.
  • Example 1 Agglomerates of nonionic surfactants and mixtures of the precipitated silica Sipernat 50 and the bentonite EX0255
  • the corresponding powders were placed in the Eirich mixer and agglomerated by slow addition of the surfactant.
  • component a) was an alkaline activated bentonite from Süd-Chemie (EX0255), as component b) the precipitated silica Sipernat 50, available from Degussa, Frankfurt, and as component c) the nonionic surfactant Imbentin-C / 135/070 the company Kolb used.
  • the pure bentonite and the pure precipitated silica were agglomerated with the nonionic surfactant. In all cases, so much surfactant was added that free-flowing agglomerates were obtained.
  • the surfactant content of the agglomerates produced is listed in the following table. To increase the whiteness these can be coated with 10% Wessalith P.
  • Agglomerates of nonionic surfactants and mixtures of sipernate 50 and bentonite as solid carriers Share of EX 0255 in% Amount used EX 0255 [g] Amount used Sipernat 50 [g] Addition to imbentin C135 / 070 [g]
  • Surfactant content of agglomerates [%] 100 800 - 676 45, 8 98 784 16 719 47 95 760 40 746 48 90 720 80 806 50.2 88 704 96 910 53.2 85 680 120 945 54.2 75 300 100 588 59.5 66.66 300 150 697 60.8 50 200 200 761 65.5 0 (Comparison, pure Sipernat 50) - 400 1090 74
  • the speed became the surfactant release by measuring the interfacial tension as a function of the stirring time on the basis of the above-described Method determined.
  • Example 2 Agglomerates of nonionic surfactants and mixtures of sipernate 22 and EX 0255 as solid carriers
  • Example 2 As in Example 1, when using more than about 12 wt .-% precipitated silica a disproportionate increase the Tensidability elevate. Exactly the investigation showed the surfactant release from those given in Table 2 Agglomerates comparable results as in Example 1 specified.
  • Example 3 Agglomerates of mixtures of Laundrosil DGA with different precipitated silicas
  • Analogous agglomerates could also be made with blends of Laundrosil DGA, a soda-activated bentonite available from Süd-Chemie AG, and other precipitated silicas. Also in these cases the agglomerates were coated with 10% Wessalith P.
  • Table 3 lists the composition and bulk density of the agglomerates screened to sizes of 0.2-1.2 mm: Agglomerates of mixtures of Laundrosil DGA and various precipitated silicas and the nonionic surfactant Genapol OA 070 bentonite silica relationship surfactant Bulk weight after coating with 10% Wessalith P Laundrosil DGA Sipernat 22 1: 1 59% 650 g / l Laundrosil DGA Sipernat 22 S (Degussa) 1: 1 59% 720 g / l Laundrosil DGA Neosyl GP (Crosfield) 1: 1 58% 670 g / l
  • the agglomeration was carried out with the Eirich R02E mixer discussed above carried out. 200 g of Sipernat 22 were used for this purpose with 200 g Laundrosil DGA presented in the Eirich mixer and after intense Mixing, the powder was agglomerated with Genapol OA 070. This agglomerates containing 59% Genapol OA 070 received. These can be optional with 10% Wessalith P (zeolite) are coated by the appropriate Amount of zeolite is added to the agglomerates and the Mixture is mixed again.
  • the process can be optimized in this way be that maximum 20% of agglomerates greater than 2 mm and a maximum of 20% of the agglomerates are less than 0.5 mm.
  • the comminution required before addition to a washing powder could not after pressing on the extruder be carried out because the knives stuck and the plant had to be cleaned in very short intervals.
  • the few obtained granules also showed a slower surfactant release as the agglomerates produced according to the invention on.
  • the method according to the invention is thus much more efficient, cheaper and comes with much less machine use than when extruding or compacting the case is, especially in the latter manufacturing processes in general, a subsequent comminution the extruded or compacted products required is.
  • Example 5 Investigation of the storage stability at 40 ° C over 3 days
  • Example 2 A sample of Example 2 with a carrier material based on Sipernat 22 and EX0255 in the ratio 1: 1, which to increase Whiteness grade has been coated with 10% Wessalith P. was a 3-day storage test at 40 ° C in a drying oven subjected to the Heraeus brand. After the camp test a sieve analysis was performed in 0.2 mm increments. To the The comparison became part of the corresponding agglomerates of Sieben analysis subjected without storing at 40 ° C. Like in shown below, the agglomerates are under such storage conditions stable. A clumping could not be proved since the sieve analyzes are stored at room temperature and the samples stored at 40 ° C within the Measuring error and small deviations caused by the sampling is identical.
  • Example 6 Agglomerates with a fatty acid methyl ester ethoxylate
  • Example 7 Agglomerates with other bentonites or other layer minerals / Influence of the degree of activation of the bentonite
  • Example 8 Agglomerates using hectorite instead of bentonite
  • Agglomerates were prepared as described in Example 1, instead of bentonite EX0255 the hectorite Optigel SH, available from Süd-Chemie AG has been. Again, it was found that from a content of about 12 wt .-% precipitated silica a disproportionate increase the surfactant uptake was observed. It could at a ratio of hectorite: precipitated silica logo CNRS logo INIST 1: 1, a surfactant content of 58% can be achieved.
  • Example 9 Agglomerates of nonionic surfactants and mixtures of zeolite, bentonite and precipitated silica
  • Example 7 by replacing a portion of the precipitated silica by zeolite the maximum content of nonionic Surfactant is reduced only slightly (by 2%), although the pure zeolite (Wessalith P) only a Tensidabilitysort has about 30%.
  • the zeolite can be used here Precipitated silicic acid functional in the stabilized "house of cards structure" replace the agglomerates according to the invention.

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Claims (20)

  1. Agglomérés contenant des phyllosilicates avec des tensio-actifs non ioniques en tant qu'additif pour détergent, contenant
    a) au moins un phyllosilicate naturel ou synthétique choisi dans le groupe des argiles contenant de la montmorillonite, en particulier la bentonite, ainsi que l'attapulgite, l'hectorite et/ou la beidellite, en une quantité de plus de 10% en poids (composant a),
    b) au moins un acide silicique précipité en une quantité d'au moins 12% en poids (composant b), à chaque fois par rapport à la quantité totale de matières support,
    c) au moins un tensio-actif non ionique en une quantité de plus de 50% en poids (composant c) par rapport à l'aggloméré entier, aucun compactage ni aucune extrusion n'étant réalisés lors de la préparation de l'aggloméré.
  2. Agglomérés selon la revendication 1, caractérisés en ce qu'ils contiennent au moins 52% en poids, en particulier au moins 55% en poids de tensio-actif non ionique.
  3. Agglomérés selon la revendication 1 ou 2, caractérisés en ce qu'ils contiennent jusqu'à 75% en poids, et en particulier jusqu'à 80% en poids de tensio-actif non ionique.
  4. Agglomérés selon l'une quelconque des revendications précédentes, caractérisés en ce qu'ils présentent une teneur en acide silicique précipité d'au moins 15% en poids, en particulier d'au moins 20% en poids par rapport à la quantité totale de matières support.
  5. Agglomérés selon l'une quelconque des revendications précédentes, caractérisés en ce que le rapport du phyllosilicate à l'acide silicique précipité, par rapport aux pourcentages en poids, est compris entre 1:20 et 20:1, de préférence entre 2:1 et 1:2, en particulier est d'environ 1:1.
  6. Agglomérés selon l'une quelconque des revendications précédentes, caractérisés en ce que les composants a) à c) constituent au moins 85% en poids, de préférence au moins 90% en poids, et de manière plus particulièrement préférée au moins 95% en poids des agglomérés.
  7. Agglomérés selon l'une quelconque des revendications 1 à 5, caractérisés en ce qu'ils contiennent en plus au moins une zéolithe (composant d), de préférence dans une quantité comprise entre 0,5% et 60% en poids, en particulier entre 5% et 30% en poids par rapport aux matières support.
  8. Agglomérés selon l'une quelconque des revendications précédentes, caractérisés en ce qu'ils contiennent 10% à 15% en poids de bentonite, 5% à 15% en poids de zéolithe et 10% à 30% en poids d'acide silicique précipité par rapport à l'aggloméré entier.
  9. Agglomérés selon la revendication 6 ou 7, caractérisés en ce que les composants a) à d) constituent au moins 85% en poids, de préférence au moins 90% en poids, et de manière plus particulièrement préférée au moins 95% en poids des agglomérés.
  10. Procédé de fabrication d'agglomérés contenant des phyllosilicates avec un tensio-actif non ionique, dans lequel
    a) au moins un phyllosilicate naturel ou synthétique choisi dans le groupe des argiles contenant de la montmorillonite, en particulier la bentonite, ainsi que l'attapulgite, l'hectorite et/ou la beidellite, en une quantité de plus de 10% en poids (composant a) ;
    b) au moins un acide silicique précipité en une quantité d'au moins 12% en poids (composant b), à chaque fois par rapport à la quantité totale de matières support ;
    c) au moins un tensio-actif non ionique en une quantité de plus de 50% en poids (composant c) par rapport à l'aggloméré entier ;
    d) éventuellement au moins une zéolithe, de préférence en une quantité de 0,5% en poids à 60% en poids par rapport à la quantité totale de matières support, sont mélangés intimement et agglomérés sans compactage ni extrusion.
  11. Procédé selon la revendication 10, caractérisé en ce que plus de 60%, en particulier plus de 80% des particules présentent un diamètre de particules compris entre 0,1 et 3 mm, en particulier entre 0,2 et 2 mm, de manière plus particulièrement préférée entre 0,4 et 1,4 mm.
  12. Procédé selon la revendication 10 ou 11, caractérisé en ce que l'on réalise le mélange intime et l'aggloméréion dans un lit fluidisé par voie mécanique.
  13. Procédé selon l'une quelconque des revendications 10 à 12, caractérisé en ce que le dispositif pour le mélange intime est un mélangeur intensif fonctionnant en continu ou en discontinu.
  14. Procédé selon l'une quelconque des revendications 10 à 13, caractérisé en ce que dans un deuxième mélangeur, on réalise un revêtement (coating) des particules d'aggloméré, lors de quoi les particules restent en l'état.
  15. Procédé selon l'une quelconque des revendications 10 à 14, caractérisé en ce que l'on utilise, pour le revêtement, une zéolithe, une bentonite, du talc ou de la poudre de dioxyde de titane.
  16. Agglomérés contenant des minéraux en feuillets avec des tensio-actifs non ioniques pouvant être obtenus à l'aide du procédé selon l'une quelconque des revendications 10 à 15.
  17. Utilisation des agglomérés contenant des minéraux en feuillets avec des tensio-actifs non ioniques selon l'une quelconque des revendications 1 à 9 dans un détergent.
  18. Utilisation selon la revendication 17, où les agglomérés contenant des minéraux en feuillets sont utilisés dans le détergent en une quantité de 0,5% à 60% en poids, en particulier de 1% à 40% en poids, et de manière plus particulièrement préférée de 5% à 25% en poids.
  19. Utilisation selon l'une quelconque des revendications 17 et 18, caractérisée en ce que le détergent se présente sous forme de tablettes.
  20. Détergent ou additif pour détergent contenant les agglomérés selon l'une quelconque des revendications 1 à 9.
EP01919340A 2000-02-25 2001-02-23 Agglomeres contenant du mineral en feuillets et des tensioactifs non ioniques Expired - Lifetime EP1257628B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DK01919340T DK1257628T3 (da) 2000-02-25 2001-02-23 Lagmineralholdige agglomerater med ikke-ioniske tensider

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10008815 2000-02-25
DE10008815A DE10008815A1 (de) 2000-02-25 2000-02-25 Schichtmineralhaltige Agglomerate mit nichtionischen Tensiden
PCT/EP2001/002116 WO2001062883A1 (fr) 2000-02-25 2001-02-23 Agglomeres contenant du mineral en feuillets et des tensioactifs non ioniques

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EP1257628A1 EP1257628A1 (fr) 2002-11-20
EP1257628B1 true EP1257628B1 (fr) 2005-01-26

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EP (1) EP1257628B1 (fr)
AT (1) ATE287942T1 (fr)
AU (1) AU2001246473A1 (fr)
DE (2) DE10008815A1 (fr)
ES (1) ES2232608T3 (fr)
WO (1) WO2001062883A1 (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10344938A1 (de) 2003-09-27 2005-04-21 Clariant Gmbh Tensid-Compounds enthaltend Fettalkoholalkoxylate
BRPI0506638A (pt) * 2004-02-06 2007-05-08 Unilever Nv composição detergente
RU2756808C2 (ru) * 2018-09-24 2021-10-05 Валерий Алексеевич Арабинский Применение отходов добычи и/или обогащения неметаллических полезных ископаемых, содержащих слоистые силикаты, в качестве компонентов моющего средства

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3702111A1 (de) * 1987-01-24 1988-08-04 Henkel Kgaa Poroeses schichtsilikat/natriumsulfat-agglomerat
DE3835918A1 (de) * 1988-10-21 1990-04-26 Henkel Kgaa Verfahren zur herstellung von tensidhaltigen granulaten
EP0627484A1 (fr) * 1993-06-02 1994-12-07 The Procter & Gamble Company Agglomérats d'argiles revêtus des matériaux particulaires finement divisés
JPH07286197A (ja) * 1994-04-15 1995-10-31 Lion Corp 粒状非イオン洗剤組成物の製造方法
US5496486A (en) * 1994-06-30 1996-03-05 Amway Corporation Process for increasing liquid surfactant loading in free flowing powder detergents
AUPN535095A0 (en) * 1995-09-12 1995-10-05 Procter & Gamble Company, The Compositions comprising hydrophilic silica particulates
JPH0987696A (ja) * 1995-09-27 1997-03-31 Lion Corp 錠剤型ノニオン洗剤組成物
DE19718664A1 (de) * 1997-05-02 1998-11-05 Clariant Gmbh Verfahren zur Herstellung von lagerstabilen schmutzablösevermögende Polymere (Soil Release Polymere, SRP) enthaltende Granulate und ihre Verwendung zur Herstellung fester Wasch- und Reinigungsmittel
JPH11302686A (ja) * 1998-04-17 1999-11-02 Lion Corp 粒状ノニオン洗剤組成物及びその製造方法

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Publication number Publication date
DE50105195D1 (de) 2005-03-03
DE10008815A1 (de) 2001-08-30
EP1257628A1 (fr) 2002-11-20
ATE287942T1 (de) 2005-02-15
ES2232608T3 (es) 2005-06-01
AU2001246473A1 (en) 2001-09-03
WO2001062883A1 (fr) 2001-08-30

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