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
  • 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 with nonionic surfactants, a process for their preparation and their use as a detergent additive.
• Nonionic surfactants are increasingly used in powder detergents. The reasons for this initially lie in their good washing properties, even at low temperatures. This goes hand in hand with the trend towards lower washing temperatures in European countries and the long-used low washing temperatures in America and Asia. Furthermore, the washing properties of the nonionic surfactants are not influenced or only slightly influenced by a high water hardness. Nonionic surfactants also have better cleaning properties for greasy dirt and for fabrics made of synthetic fibers than anionic surfactants. However, due to their liquid to waxy consistency, the penetration of nonionic surfactants in large quantities into powder detergents is associated with some difficulties.
• nonionic surfactants in washing powders, which are produced by a spray process, easily leads to a sticking of the nozzles during spray drying and to a swelling of the powder due to the evaporation of volatile impurities in the nonionic surfactants.
• the nonionic surfactants are therefore usually applied to the powders only after spray drying.
• the absorption capacity of the powders obtained from the spray drying process does not allow large amounts of nonionic surfactants to be applied or introduced.
• additives such as sodium silicate as a builder, an organic polyacrylate salt, also as a builder, an optical brightener, an enzyme, a bleaching agent and an extender can be present.
• the ingredients are kneaded and extruded and then crushed. So there is no simple agglomeration.
• JP 0011310791 describes a granular, non-ionic detergent composition which contains 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 which contain sodium sulfate and synthetic layered silicates.
• the granules are produced by spray drying, producing a porous granulate which can be loaded with liquid surfactants.
• the liquid absorption capacity is between 2 and 50% by weight, preferably up to 35% by weight.
• the surfactant content is above 50% and the agglomerates are not produced by spray drying.
• the nonionic surfactant in the mixing stage (a) the nonionic surfactant is mixed with water, which may or may not contain part, but less than 50% by weight of the total amount of water-soluble or water-insoluble solids can be mixed until a gel phase is formed, whereupon in step (b) the remaining main amount of the solids is mixed in and the mixture is mechanically processed until granules are formed.
• the weight ratio of nonionic surfactant and water in the gel phase to total solids is 25:75 to 65:35.
• Surfactant contents (based on anhydrous alcohol ethoxylate) of 10 to 20.5% by weight are calculated from the examples. The surfactant content is therefore well below 50% by weight. Since the surfactant absorption capacity of zeolite A is only 26% by weight, it is not possible to produce granules with surfactant contents of more than 50% on the basis of zeolite as the sole carrier material. This is also not possible with carrier mixtures made from bentonites and zeolites, since bentonite granules can only absorb a maximum of about 40% by weight of surfactants.
• EP-A-0 690 123 describes a process for the production of a powder detergent, (1) a builder (soda, zeolite, STPP, trisodium nitrilotriacetate, citrates or sulfates or mixtures thereof) is agglomerated with a nonionic surfactant, (2) a barrier material (amorphous silicates / precipitated silicas) is added and (3) further processing with the builder takes place to the final granulate.
• the total surfactant content is 5 to 50% by weight, which is below the upper limit according to the invention.
• the products according to the invention are only produced in a maximum of two steps.
• the agglomerates according to the invention must contain layer silicates containing montmorillonite.
• the object of the invention was therefore to provide agglomerates with a high content of nonionic surfactants, which are not sticky, do not "bleed” and enable the nonionic surfactants to be released more rapidly into the wash liquor.
• the gel effect which is frequently observed when the nonionic surfactants are released should be reduced as far as possible.
• the resulting gel phases have a high viscosity that prevents the surfactants from dissolving quickly and can cause the particles to stick together when they dissolve.
• the agglomerates according to the invention contain
• At least one natural or synthetic layer silicate selected from the group of clays containing montmorillonite, in particular bentonite, and attapulgite, hectorite and / or beidellite (component a), in an amount of more than 10% by weight
• the agglomerates according to the invention with the above composition can absorb very high amounts of nonionic surfactants without becoming sticky or "bleeding".
• the agglomerates according to the invention can be admixed particularly advantageously with washing powders, the gel formation effect mentioned above being limited to the agglomerates and not covering the entire detergent composition, and also surprisingly small.
• a content of at least about 12% by weight of precipitated silica preferably of at least about 15 to at least about 20% by weight of precipitated silica, has a synergistic effect with the layer silicates mentioned above and a very high incorporation of nonionic surfactants is made possible without this leading to stickiness or "bleeding" of the agglomerates.
• the rapid dissolution of the agglomerate particles and the rapid release of the nonionic surfactants into the washing liquor are ensured, incrustations on the laundry can also be avoided.
• montmorillonite-containing silicates such as bentonite, as well as attapulgite, hectorite and / or beidellite, as natural or synthetic layered silicates, provide particularly advantageous results.
• natural or synthetic bentonites preferably Na bentonite
• At- tapulgite preferably Na bentonite
• At- tapulgite preferably Na bentonite
• At- tapulgite preferably Na bentonite
• At- tapulgite preferably Na bentonite
• At- tapulgite preferably Na bentonite
• At- tapulgite preferably Na bentonite
• At- tapulgite preferably At- tapulgite
• Bentonite and hectorite in particular also have a positive effect on washing performance and a fabric softening effect.
• synthetic layered silicates can also be used according to the invention, for example synthetic hectorite.
• activated bentonite in particular bentonite activated with soda, is used, for example.
• a content of precipitated silicas of at least about 12% by weight, based on the total amount of the support materials (components a, b and, if appropriate, d according to claims 1 and 7, respectively) is shown in combination with the natural or synthetic Layered silicates surprisingly have a synergistic effect.
• the amount of precipitated silica in the agglomerates according to the invention is therefore adjusted so that on the one hand it is at least about 12% by weight, preferably at least about 14% by weight, and in particular at least about 16% by weight, based on the total amount of support materials.
• the layered silicate used in the manner of a "house of cards" or framework, forms a porous structure for taking up the nonionic surfactant, the structure being formed by the highly porous precipitated silica stabilized is siert and this interacts with the three-dimensional layered silicate structure.
• the agglomerates according to the invention therefore have a particularly high and relatively stable porosity.
• the precipitated silica causes (partial) delamination of the layered silicate.
• the agglomerates according to the invention are therefore neither compacted nor extruded.
• the person skilled in the art is familiar with what is to be understood by compacting and extrusion, whereby according to the invention such energy inputs are to be avoided which would cause a considerable change in the porosity and density of the agglomerates.
• the energy input is too high or the action of high shear or compression forces, such as in particular in the case of (roller) compaction or extrusion, the above-described stabilized card house structure composed of bentonite flakes and silica particles is adversely affected.
• Compacting here also means (compacting) kneading.
• the amount of precipitated silica used does not exceed 40% by weight. , preferably not more than 30 % By weight, based on the total agglomerates.
• the agglomerates according to the invention being rapidly soluble.
• the agglomerates according to the invention surprisingly show a significantly lower tack with the same surfactant content as agglomerates according to the prior art.
• agglomerates according to the invention are advantageously produced in the particle sizes customary for detergent additives, which are familiar to the person skilled in the art in this field.
• premixing when the particles are compacted or extruded, premixing must first be carried out, for example by kneading in cylindrical rollers or by kneading in an extruder, coarse material then being obtained as a cake or extrudate pressed through a nozzle.
• This material must be comminuted in a subsequent step, which is problematic and energy and cost-intensive, in particular given the high surfactant contents desired according to the invention and the increased stickiness of the compacted or extruded material.
• silicas can be used in the agglomerates according to the invention.
• starting materials for the extraction of silicas by wet are alkali silicate solutions, preferably sodium silicate, from which amorphous silicic acid is precipitated by the addition of acid.
• the precipitated product consists of 86 to 88% Si0 2 and 10 to 12% water, which is physically bound both in the molecular structure and on the surface, lu as well as from residues of the salt formed during the reaction and small additions of metal oxides.
• precipitation temperature precipitation temperature
• pH value pH value
• electrolyte concentration and precipitation time silicas with different surface properties can be produced.
• Silicas can be produced in the range of specific surfaces from about 25 to 700 m 2 / g.
• the silica suspension obtained during the precipitation is transferred to filter presses, the solids content of the filter cake being between about 15 and 20%. Drying takes place according to different processes, which are often followed by grinding and classifying steps.
• hydrophilic and hydrophobic silicas can be used, whereby hydrophobic silicas can simultaneously serve as defoamers.
• the silicas used in the present invention preferably have an average particle diameter of approximately 1 to 100 ⁇ m.
• precipitated silicas with a high specific surface area and a high adsorption capacity which is characterized by the oil number or the dibutyl phthalate number (DBP number) according to DIN 53601, are preferred.
• non-ionic surfactants known to the person skilled in the art can be used to produce the agglomerates. These include, but are not limited to, the group of alcohol ethoxylates or fatty alcohol polyethylene glycol ethers, alkyl polyglycosides, fatty alcohol polyglycol ether methyl esters, fatty acid methyl ester ethoxylates, sorbitan esters or mixtures thereof. Fatty alcohol polyethylene glycol ethers, alkyl polyglycosides, fatty acid methyl ester ethoxylates and Fatty alcohol polyglycol ether methyl ester. Fatty alcohol polyethylene glycol ethers, fatty alcohol polyglycol ether methyl esters or mixtures of the two are particularly preferred. When using fatty acid methyl ester ethoxylates, the agglomerates according to the invention can be dissolved surprisingly quickly.
• Preferred fatty alcohol polyethylene glycol ethers are those which are common in detergent applications, i.e. which have degrees of ethoxylation between 1 and 12 and alkyl chain residues with 10 to 17 carbon units. Fatty alcohol polyethylene glycol ethers with a few ethoxylate units are preferably used in mixtures with higher ethoxylated fatty alcohol polyethylene glycol ethers.
• the preferred non-ionic surfactants in individual cases depend on the specific requirements for the detergent and can be determined by the person skilled in the art on the basis of routine tests.
• the agglomerates can contain additional additives known in the art.
• additives known in the prior art can be added to the agglomerates according to the invention, such as e.g. Alcohols such as ethanol or glycerin, polyethylene glycols or hydrotropes such as Na cumene sulfonate.
• the polyethylene glycols used are in particular those which have low molecular weights, in particular 200 to 6000 g / mol. These are generally mixed with the surfactant before agglomeration and used in amounts of 0.1 to 30%, based on the amount of surfactant.
• the agglomerates according to the invention contain at least 52% by weight, in particular at least 55% by weight, particularly preferably at least 58% by weight, of nonionic surfactants, based on the total agglomerate.
• the ratio of layered silicate to precipitated silica, based on% by weight in the agglomerates according to the invention is preferably between 2: 1 and 1: 2. According to a particularly preferred embodiment, the layered silicate and the precipitated silica are present in approximately the same amounts, based on% by weight.
• the agglomerates contain about 10 to 15% by weight of bentonite, about 5 to 15% by weight of zeolite and about 10 to 30% by weight of precipitated silica, based on the total agglomerate.
• the agglomerates according to the invention can additionally contain additives known in the prior art, in a preferred embodiment the agglomerates consist essentially of nonionic surfactant, layered silicate and precipitated silica, so that intimate contact between these components is ensured.
• the above components preferably make up at least 85% by weight, in particular at least 90% by weight, and particularly preferably about 95% by weight of the agglomerates.
• the additional uptake of at least one zeolite into the agglomerates leads to particularly positive results. It is known that it is not readily possible to obtain agglomerates by agglomeration of zeolite with nonionic surfactant, since the fine particle size of the zeolites makes it difficult to produce agglomerates with the usual particle size in a satisfactory yield.
• zeolites can be used for the agglomerates, for example Wessalith P “ , Wessalith 200 ⁇ “ from Degussa, Doucil A24 “ and Doucil A4 " from Crosfield, Eijsden, the Netherlands.
• the layered silicate-containing agglomerates can be produced according to the invention by a process in which
• component a at least one natural or synthetic layered silicate, selected from the group of clays containing montmorillonite, in particular bentonite, and attapulgite, hectorite and / or beidellite, in an amount of more than 10% by weight (component a);
• component c) at least one nonionic surfactant in an amount of greater than 50% by weight (component c), based on the total agglomerate;
• zeolite optionally in an amount of 0.5% by weight to 30% by weight, based on the total amount of support materials
• a mechanical fluidized bed is generated for intensive mixing.
• the intensive mixers known in the prior art can generally be used in batch-wise or continuous processes. If the agglomeration is carried out in batches, batch mixers from Eichrich, Hartheim, Loedige-Mixer (eg Loedige FKM-Mixer, Paderborn) or Drais (Drais Turbomix, Mannheim) can be used. With continuous process control, mixers from Loedige, Paderborn (e.g. Loedige-CB mixer), from Drais, Mannheim (e.g. Drais CoriMix), from Ballestra, Milan, Italy (e.g.
• Ballestra Cetemix or from Schugi-Leylistad, Netherlands (e.g. Schugi.) Flexomix
• two mixers can also be combined with one another, such as a Loedige CB mixer and a Loedige KM mixer, whereby coating with an inorganic powder can also take place in the second mixer.
• the agglomerates are preferably produced in an intensive mixer by mixing the above-mentioned carrier materials with the surfactant. In many cases, it is preferred to intensively mix the carrier materials (components a, b, and optionally d) beforehand.
• the surfactant or the surfactant mixture which is optionally provided with further additives, can be added in the pure state or mixed with water. Water contents are preferably set between 0 and about 50%. Water contents between 0 and about 20% are particularly preferred.
• the use of the pure surfactants for agglomeration has the advantage that the resulting agglomerates do not have to be dried. This also applies to surfactant-water mixtures that have water contents that correspond to those of the finished washing powder or washing powder tablets.
• the agglomerate particles are coated (coating) in a second mixer, the structure of the particles being retained.
• zeolite, bentonite, talc or titanium dioxide powder are used to coat the agglomerate particles. If the agglomerates according to the invention already contain zeolite, the coating can also be omitted if the whiteness of the agglomerate particles is sufficient and a further reduction in the tackiness is not necessary. According to the present invention, there is preferably no comminution of the agglomerate particles.
• Another aspect of the present invention relates to agglomerates containing layered minerals and containing nonionic surfactants which can be obtained by the above process.
• the agglomerates are used as additives to detergents. It is particularly advantageous here that the very high content of nonionic surfactants means that only very small amounts of the detergent composition have to be added. As a result, the gel effect mentioned above is also limited to the added agglomerates and is quite low due to the composition of the agglomerates according to the invention.
• the added agglomerates fulfill both the function of providing a sufficient content of nonionic surfactants and increasing the softness of the laundry.
• Another aspect of the present invention relates to a detergent or detergent additive which contains the agglomerates according to the invention.
• the agglomerates can be used in detergents which are in tablet form.
• an Eirich R02E intensive mixer was used to produce the agglomerates discussed in the following examples.
• the low setting (level 1) for the rotation speed of the plate and the maximum rotation speed for the vertebrate were chosen.
• the agglomeration parameters were chosen below so that more than 50% of the agglomerates were in a particle size range of 0.2-1.2 mm.
• the average particle size can be modified by routine selection of the production parameters.
• the agglomerates were, if indicated, with inorganic powders such as e.g. Talc or zeolite coated (coated).
• the material was transferred to a plastic bag, the inorganic powder was added and shaken for about 2 minutes.
• the coating was carried out in the Eirich mixer. For this purpose, after the agglomeration, the inorganic powder was added for coating and the agglomerate / powder mixture was then mixed again for 2 minutes. The other results were comparable.
• the measurement of the surface tension of the solution of the agglomerates was used.
• the surface tension was measured as a function of time after the bladder pressure method with an online tensiometer, SITA-Online F10.
• a bubble frequency of 1 Hz was used to record the measurement curves.
• Standardized samples with particle sizes between 0.2 and 1.2 mm were used for the measurements.
• 1 g samples were used, placed in 200 ml of distilled water and stirred with a 1.5 cm long stirring fish at a frequency of 150 revolutions.
• the surface tension can serve as a measure of the surfactant release.
• the most commonly used surfactant Genapol OA 070 in a concentration of 0.5 g / l was used as a comparison.
• Such a solution had a surface tension of 30-32 mN / m under the same measurement conditions.
• the bulk density was determined in the examples below by pouring 100 g of the agglomerates into a 1,000 ml can and shaking for about 30 seconds.
• the measuring cylinder is weighed empty to 10 mg.
• the powder funnel is then attached to the opening of the cylinder using a stand and clamp.
• the measuring cylinder is filled with the agglomerates within 15 seconds. With the spatula, filling material is continuously refilled, so that the measuring cylinder is always slightly protruding. After 2 minutes, the excess is wiped off with a spatula, taking care that no pressing forces compress the material in the cylinder.
• the filled measuring cylinder is brushed off and weighed.
• the bulk density is given in g / 1.
• the bulk densities obtained allow more than 600 g / 1, in particular more than 650 g / 1, also a use of the agglomerates according to the invention 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 an Eirich mixer and agglomerated by slowly adding the surfactant.
• component a) 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 used by the Kolb company.
• 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 still 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.
• Table 1 Agglomerates of non-ionic surfactants and mixtures of Sipernat 50 and bentonite as solid carriers
• the straight line drawn in Figure 1 shows the course that one would expect with an ideal mixing behavior of the carrier materials with regard to the binding capacity for nonionic surfactants.
• the content of non-ionic surfactants in the agglomerates at levels above about 12% precipitated silica, based on the total amount of carrier materials increases significantly disproportionately when a part of the bentonite is replaced by the precipitated silica.
• the rate of surfactant release was determined by measuring the interfacial tension as a function of the stirring time using the method described above.
• Example 2 Agglomerates of nonionic surfactants and mixtures of Sipernat 22 and EX 0255 as solid carriers
• Table 2 Agglomerates from mixtures of EX 0255 and Sipernat 22 with the non-ionic surfactant Genapol OA 070
• Example 2 As in Example 1, the use of more than about 12% by weight of precipitated silica showed a disproportionate increase in the surfactant absorption capacity. Likewise, the investigation of the surfactant release from the agglomerates shown in Table 2 showed results comparable to those given in Example 1.
• agglomerates were obtained after coating with zeolite, of which over 80% were in a size range between 0.2 and 1.2 mm.
• the fine fraction (agglomerates with sizes smaller than 0.2 mm) was less than 5% in this system after optimization of the manufacturing parameters.
• the bulk density of these agglomerates was 650 g / i.
• Example 3 Agglomerates from mixtures of Laundrosil DGA with different precipitated silicas
• Analogous agglomerates could also be produced with mixtures of Laundrosil DGA, a sodon-activated bentonite, available from Süd-Chemie AG, and other precipitated silicas. In these cases too, the agglomerates were coated with 10% Wessalith P.
• Table 3 lists the composition and bulk density of the agglomerates that were sieved to sizes of 0.2-1.2 mm:
• Table 3 Agglomerates from mixtures of Laundrosil DGA and various precipitated silicas as well as the non-ionic surfactant Genapol OA 070
• Example 4 Comparison of the agglomeration according to the invention in the intensive mixer with an extrusion or compacting
• the agglomeration was carried out with the E ⁇ ch-R02E mixer explained above. 200 g of Sipernat 22 were initially charged with 200 g of Laundrosil DGA in an egg mixer and after intensive mixing the powder was agglomerated with Genapol OA 070. Agglomerates with a content of 59% were received napol OA 070. These can optionally be coated with 10% Wessalith P (zeolite) by adding the appropriate amount of zeolite to the agglomerates and mixing the mixture again. The process can be optimized so that a maximum of 20% of the agglomerates are larger than 2 mm and a maximum of 20% of the agglomerates are smaller than 0.5 mm.
• Wessalith P zeolite
• the agglomerates produced according to the invention had advantageous properties in relation to extruded or compacted materials in terms of surfactant absorption, low stickiness and rapid surfactant release.
• particle sizes of about 0.4 to 2 mm particle diameter, as are common in the detergent industry, could be obtained with high yields.
• the process used to produce the agglomerates according to the invention is less time and cost intensive.
• the process according to the invention is thus considerably more efficient, less expensive and requires far less machine than is the case with extrusion or compacting, especially since the latter production processes generally require subsequent comminution of the extruded or compacted products.
• Example 5 Investigation of the storage stability at 40 ° C over 3 days
• Example 2 A sample from Example 2 with a carrier material based on Sipernat 22 and EX0255 in a ratio of 1: 1, which had been coated with 10% Wessalith P to increase the whiteness, was subjected to a 3-day storage test at 40 ° C. in a Heraeus brand drying cabinet subjected. After the storage test, a sieve analysis was carried out in 0.2 mm steps. For comparison, some of the corresponding agglomerates were subjected to a sieve analysis without storing them at 40 ° C. As shown below, the agglomerates are stable under such storage conditions.
• Example 6 Agglomerates with a fatty acid methyl ester ethoxylate
• agglomerates also show a rapid release of the nonionic surfactant in the test shown above (measurement of the surface tension as a function of the stirring time with 1 g of granules). Surface tension values of 30 - 35 mN / m are achieved after just 70 seconds of stirring.
• Example 7 Agglomerates with other bentonites or other layer minerals / influence of the degree of activation of the bentonite
• the corresponding non-activated bentonite EX0276 was used instead of the bentonite EX0255 used in Examples 1 and 2 above.
• the agglomerates were prepared as described in Example 1, the respective bentonite being used in a ratio of 1: 1, based on% by weight, with the precipitated silica Sipernat 22. It was shown that when using the non-activated bentonite EX0276 a surfactant content of 54% was achieved, whereas when using the corresponding activated bentonite EX0255 a significantly higher surfactant content of 61% was achieved. This proves the positive influence of an activation of the layered silicate used.
• Example 8 Agglomerates using hectorite instead of bentonite
• Example 9 Agglomerates of nonionic surfactants and mixtures of zeolite, bentonite and precipitated silica
• Example 7 by replacing part of the precipitated silica with zeolite, the maximum nonionic surfactant content is reduced only slightly (by 2%), although the pure zeolite (Wessalith P) only has a surfactant absorption capacity of about 30%.
• the zeolite can functionally replace the precipitated silica in the stabilized "house of cards" structure of the agglomerates according to the invention.

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