EP1871669A1

EP1871669A1 - Method for producing liquid preparations having a solid body content

Info

Publication number: EP1871669A1
Application number: EP06707516A
Authority: EP
Inventors: Bernhard Orlich; Bernd Richter; Alexander Lambotte
Original assignee: Henkel AG and Co KGaA
Current assignee: Henkel AG and Co KGaA
Priority date: 2005-04-19
Filing date: 2006-03-10
Publication date: 2008-01-02
Anticipated expiration: 2026-03-10
Also published as: JP2008538788A; US8741830B2; DE102005018243A1; WO2006111223A1; ATE555019T1; US20080262109A1; EP1871669B1; PL1871669T3; ES2383218T3

Abstract

A method for producing a liquid preparation having a solid body content and the resulting liquid preparation. According to the method, the addition of at least a portion of the solid bodies takes place only (a) in the last stage of the method preceding the pouring of the liquid preparation into a packing unit or (b) during the pouring into a packing unit.

Description

"Process for the preparation of liquid preparations with solids content"

The invention relates to a process for producing liquid preparations with a solids content, in which the addition of at least part of the solids takes place only before or during the filling of a liquid preparation.

Many products used in daily life are liquid preparations. So these are e.g. in the field of detergents and cleaners, liquid or fabric softeners, in the field of food preparations, e.g. finished salad dressings or liquid tomato products such as ketchup, in the field of pharmaceutical preparations e.g. Lotions or tinctures, on the cosmetic sector e.g. Hair shampoos or aftershave, in the field of engineering, e.g. liquid adhesives and paints or paints. This list could be continued arbitrarily.

It is often the case that such liquid preparations should contain a certain solids content. The reasons for this are manifold and depend on the intended use of the product. It may even be the simple reason to set visual accents, in order to increase the purely optical attractiveness of the product for the consumer and thereby make the purchase decision easier.

Thus, for example, In liquid detergents, implement small colored particles that float in the liquid detergent and do not sink, so that no sediment forms and the particles also do not float or cream. These particles may also contain certain active ingredients which allow the product to have improved efficacy. In such a case, the particles would carry a message to the consumer, e.g. "New and Improved Formulation." Consumers could directly identify the particles as functionalities and immediately identify the added value involved, as well as introduce sensitive substances into the liquid matrix through the particles, which are then protected and can cause incompatibility Ingredients are avoided.

The same considerations apply to other technical fields, as can be incorporated into hair shampoos microcapsules, which remain in the hair during washing in the hair and deliver their content, eg nourishing oils to the hair only by the temperature increase when the hair is blown. This is how a consumer-friendly hair care can be realized. Likewise, for example, flavor carriers in microencapsulated form can be introduced into liquid food preparations, which are released only during cooking or during the chewing process, etc. Liquid preparations with a solids content thus enable "smarter" products with increased optical attractiveness and open up new formulation possibilities.

However, the additional incorporation of solids in liquid preparations is associated with additional process engineering effort. However, above all, it is important to be able to continue to use already existing large-scale production plants, which were previously geared in particular to the production of exclusively liquid preparations, so that no fundamentally new production plants have to be built, which would be too costly. This is all the more so since production of exclusively liquid products must continue on the existing large-scale production facilities.

However, if one wants to use the existing large-scale production facilities for the production of solids-containing liquid preparations, one sees itself confronted above all with two problems.

First, there is a risk of contamination, i. the danger that the production plant is contaminated with solids and that secondary products in the production plant are contaminated by solids in so-called dead zones. Here even the smallest amounts of solids are sufficient to make very large quantities of secondary products unsalable. An example of this is the following scenario: On one and the same production line, a manual dishwashing medium with the implementation of free-floating particles is first run. Subsequently, a liquid floor cleaning agent is run on the same production line. The remainder of the free-floating particles present in the system enter the containers of the liquid floor cleaning agent as impurities. These contaminated products could not be offered to the trade as the consumer would consider them to be contaminated. As a consequence, after every single production a very thorough cleaning of the entire production plant would be necessary. This is difficult because the solids are easily susceptible to particularly inadequate locations, e.g. can remain stuck in the pipes and can often be removed from there only after repeated flushing processes. Sometimes it may even be necessary to disassemble whole piping systems, manually or mechanically clean, and reassemble. It may also be necessary to use certain components, e.g. Valves, remove and replace if necessary, since they can clog or even leaking.

On the other hand, there is a further danger that the solids to be added will not survive the production line unscathed. This is because the solids are often unusually fragile, as the release of active substances contained in the solids in the later application should be safe and easy, for example by stimuli such as a slight increase in temperature or slight mechanical influences. Of course, the solids are also exposed to such light stimuli in the existing production lines. As a result, even during production, the integrity of a good part of the solids is damaged. This is very regrettable in several ways. On the one hand, the solids are preferably straight given those active ingredients which are incompatible with the remainder of the formulation. Now comes the incompatible drug too early, namely already in the production with the rest of the formulation in contact, then at best only the active ingredient is destroyed, worst case, but the entire formulation impaired, if not rendered useless. Since the active substances to be added via the solids are generally of high quality and therefore very cost-intensive, their destruction is doubly disadvantageous.

In addition, there is the visual impairment, for example, when the solids are damaged in shape and form, as they are shredded during production, so that very irregularly shaped, torn or frayed solids can, for example, increase their optical attractiveness and create a consumer's sense of being confronted with a low-quality product, leading to significant consumer uncertainty.

These problems lead to the benefits which are actually sought with the incorporation of the solids into the liquid preparations being leveled off or even extinguished altogether, or at least reversed to the contrary when e.g. the complete disuse of the product results.

The object of the present invention was therefore to overcome such problems.

This object is achieved by the subject matter of the invention, namely a method for producing a liquid preparation with a solids content, wherein the addition of at least a portion of the solids (a) only in the last, the filling of the liquid preparation in a packing unit preceding step or (b ) takes place during the filling into a packing unit, wherein the liquid preparation is advantageously already considered to be ready for use before the addition of the solids.

In addition to overcoming the above-described problems, a further advantage of the method according to the invention is that it leads to liquid preparations in which the solids are very homogeneously distributed, in particular when the mixing of solids with liquid preparation takes place shortly before bottling , So in the last, the filling of the liquid preparation in a packing unit preceding process step. Namely, in conventional standard processes, the mixing takes place well in advance, in which case segregation phenomena often occur in the piping systems in these cases.

By the term "liquid preparations" is meant liquid preparations in the broadest sense, ie liquids with a very thin consistency up to liquids with pronounced doughy, tough or even mushy consistency, such as honey, ketchup, mustard or mayonnaise, to show only a few illustrative examples. A liquid preparation in the context of this invention is also a slurry, ie a preferably aqueous slurrying of solids.

Liquid preparations within the meaning of this invention are also gels, creams, pastes, sludges and slimes etc. In the broadest sense, such preparations are also liquid preparations in the sense of this invention which per se do not flow at room temperature but are spreadable, such as e.g. Butter, shoe polish, cream cheese, etc.

For the purposes of the present invention, solids are substances which preferably have both a substantially defined volume and preferably a substantially defined shape and which preferably resist the change (deformation, crushing, etc.) of their volume and / or their shape. This resistance may be smaller with respect to softer solids, or greater, which affects harder solids. If a change in shape occurs under external constraint, the solids may try to return to their original state. For the purposes of the present invention, solids are also preferably dispersions or precipitates which may be present in liquids or as a moist material. A typical solid in the sense of this invention is for example a capsule or a so-called speckle. On capsules and Speckies will be discussed in more detail below.

The fact that the addition of at least part of the solids takes place only in the last process step preceding the filling of the liquid preparation into a packing unit means that following the completion of this process step essentially no further process steps follow and the filling of the liquid preparation follows into a packing unit , The fact that "essentially" no further process steps follow, in the sense of a preferred embodiment, that the preparation containing solids can also be added further ingredients, such as perfume, enzymes, combustible substances, highly flammable substances, water, solvents, although this one It is more preferred to add no further constituents to the solid-containing preparation. "Essentially" that no further process steps follow, in the sense of a preferred embodiment, means that the preparation containing the solids can still be diluted and thickened, although this is a less preferred embodiment. It is more preferable not to dilute or thicken the solid-containing preparation. The fact that "essentially" no further process steps follow, means in the narrowest and most preferred sense that in fact no further process steps follow than the filling of the preparation into packing units, which is the most preferred embodiment. Of course, other substances such as especially solvents, water, fragrances, enzymes, combustible substances, easily inflammable substances can be added to the liquid preparation in the addition of solids. This corresponds to a preferred embodiment.

The addition of the solid "when being filled into a packing unit" means that the solids are added to the liquid preparation during the filling process of the packing unit, which in the sense of a preferred embodiment may mean that the solids are (at least partially) introduced into the packing unit and the This can mean, in the sense of a preferred embodiment, that the packing unit is filled with the liquid preparation and finally the solids are added. (A good distribution of the solids in the liquid preparation can then be achieved by shaking, panning, rotating In the sense of a preferred embodiment, this can mean that the packing unit is partially filled with the liquid preparation, then the solids are added and then filled up with further liquid preparation preferred embodiment means that solid and liquid preparation are filled together in the packing unit, for example in 2 streams, i. a stream of liquid preparation and a stream of solids. Solid and liquid preparation can be added in the sense of a preferred embodiment, but for example also in a stream, i. liquid preparation and solids are combined immediately prior to entry into the packing unit and arrive in a stream in the packing unit. The latter can be realized, for example, by injecting the solids into a liquid jet (jet of liquid preparation) via a nozzle, thereby combining solid and liquid preparation. This corresponds to a preferred embodiment.

The term "otherwise ready to use liquid preparation means that in a particular preferred embodiment, the liquid preparation to be incorporated in the solids is preferably ready for use so that it could readily be filled into packages such as bottles or tubes and then possibly from Consumer could be supplied to its intended use, so that it would no longer have to submit to any further mixing or constriction process. For the purposes of a preferred embodiment, the term "otherwise ready-to-use liquid preparation" also covers the scenario that the active-ingredient-active substances are added to this liquid preparation only with the addition of the solids.A simplified example of this would be, for example, a thickened aqueous preparation which itself Also, such a thickened aqueous preparation which is free of active substances per se prior to the addition of the solid constitutes an "otherwise ready-to-use liquid preparation" in the sense of a preferred embodiment of this invention represents. The fact that "at least part of the solids" must be added shortly before or during the filling process means that the entire amount of solids contained in the liquid preparation does not necessarily have to be added before or during the filling process For example, in the context of a preferred embodiment, it is also possible for a single type of solids to be added in portions, in which case at least one portion being compulsory only before the filling process However, it is particularly preferred if the entire proportion of solids is added only before or during the filling process, which corresponds to a preferred embodiment of the invention.

The "filling" of the preparation preferably means the filling of packing units, in particular individual packing units (eg bottles, canisters, pouches, etc.) with the liquid preparation, the latter can be used directly by the consumer Packing units can also containers, containers, kettles, tanks or This is also, albeit less, preferred.The "filling" of the preparation is preferably carried out by weight and / or volume. The optical filling height control can be performed by humans, for example by a technical employee filling a packing unit (eg tank) and interrupting the supply of the liquid preparation into the tank as soon as the tank is nearly empty The optical level control can also be carried out semi-automatically or fully automatically, for example by means of optical sensors, electronic filling height measurement, etc.

According to a further preferred embodiment of the invention, in the method, the addition of at least a portion of the solids takes place only when the other components of the composition have already undergone a mixing process. Especially . they have already undergone all the steps required for mixing or mixing, except for the essentially last step of mixing with the solids.

The mixing of the otherwise ready-to-use liquid preparation with the solids to be added is advantageously carried out under mild conditions.

Gentle conditions are in particular those which are advantageously not associated with greater temperature loads and / or preferably not with greater mechanical loads. Preferably, the mixing takes place at temperatures below 70 ⁰ C, advantageously less than 60 ° C, more preferably less than 50 ⁰ C, even more advantageously less than 40 ° C, even more advantageously less than 30 ° C, in particular at room temperature. Preferably, the specific see performance be used for the mixing device less than 5 kW / m ^3, preferably less than 4 kW / m ^3, advantageously less than 3 kW / m ^3, more advantageously less than 2 kW / m ^3, more advantageously in further manner less than 1 kW / m ³ , more preferably less than 0.8 kW / m ³ , very advantageously less than 0.6 kW / m ^3, in an extremely advantageous manner 0.4 kW / m ³ , in particular less than 0, 2 kW / m ³ .

The solids to be added can advantageously be added continuously or discontinuously. It is e.g. possible that the solids to be added are added to the liquid preparation by means of a carrier liquid, preferably in suspended form. This corresponds to a preferred embodiment of the invention.

It is also possible that the solids are added directly into the liquid preparation, preferably by trickling or pouring. This also corresponds to a preferred embodiment of the invention. Of course, you can also add a portion of the solid to be added with the help of a carrier liquid and directly add another part of the solids to be added, so for example trickle or fill.

The mixing of the otherwise ready-to-use aqueous preparation with the solids to be added can advantageously take place in a continuous stirred reactor (CST reactor). This corresponds to a preferred embodiment. Such a continuous stirred reactor is advantageously characterized by a continuous mode of operation and good, preferably almost complete, mixing. In the reactor, almost no concentration profiles and temperature profiles should preferably occur, so that its content can preferably be referred to as virtually homogeneously mixed. Thus, if the mixing of the otherwise ready-to-use preparations with the solids to be added is carried out in a continuous stirred reactor, then a preferred embodiment is present.

Of course, however, other possibilities of mixing or mixing can be used, in particular static mixing sections can be used, which corresponds to a preferred embodiment.

A stirrer which is particularly suitable for the mixing is, for example, an InterMig stirrer (Ekato). Particularly suitable stirring speeds for this type of stirrer are, for example, 0.3 to 7 m / sec. Likewise suitable are stirrers of the blade agitator type, anchor stirrer, crossbar stirrer, helical stirrer or MIG stirrer. In order to avoid fluid rotation and to achieve good homogenization in the continuously stirred container, it is possible to install in the containers preferably baffles (reinforcements). According to a preferred embodiment of the invention, the mixing time (time for mixing the solids with the liquid preparation) is less than 60 minutes, advantageously less than 50 minutes, more advantageously less than 40 minutes, even more advantageously less than 30 minutes, more preferably less than 20 minutes, more preferably less than 10 minutes, most preferably less than 5 minutes, preferably less than 4 minutes, especially less than 3 minutes.

To avoid are stirrer types, which are e.g. are particularly suitable for emulsifying or suspending tasks and thus lead locally to a high seer entry in the liquid. Mentioned here are, for example, the propeller stirrer, the impeller stirrer and the disk stirrer at stirring speeds above 1 m / sec in viscous media (> 500 mPa s). These are unfavorable for the purposes of the invention.

In particular, the following pumps are particularly suitable for transporting the solid-containing liquid preparations: 'Maso-sine pump, Rotan gear pump (a gear), peristaltic pump with min. DN30.

In particular, the following pumps are less suitable for transporting the solid-containing liquid preparations, in particular unsuitable, since they disadvantageously result in comminution _. the solid can contribute: gear pump (double gear), centrifugal pump.

The inventive method is, as far as the nature of the liquid preparation is in no way inferior, preferably the liquid preparation is a washing and cleaning agent, a food preparation, a paint, paint or lacquer preparation, an adhesive preparation, a pharmaceutical preparation and / or a cosmetic preparation. With regard to these preparations mentioned are preferred embodiments of the invention. Very particular preference is given to liquid detergents and cleaners as well as liquid cosmetic preparations. For the purposes of this invention, liquid detergents also include, in particular, fabric softeners, as well as textile treatment agents of all types.

Among other things, the solids content of the liquid preparation also depends on what purpose the preparation and in particular the solids contained therein are intended to serve. In this respect, it may be advantageous to incorporate very large amounts of solids in the liquid preparation. It may also be advantageous to incorporate only moderate amounts of solids or just very small amounts of solids. Very small amounts of solids are useful, for example, if the active substance to be incorporated with the solid is, for example, very expensive or very effective. It may be advantageous for the purposes of the invention if a certain maximum amount of solids in the liquid preparation is not exceeded. If such a maximum amount is not exceeded, so is a preferred embodiment.

Advantageously, in a certain preferred embodiment, the agent contains a maximum of 80% by weight of solids, in a considerably advantageous manner at most 70% by weight of solids, more preferably a maximum of 60% by weight of solids, more preferably a maximum of 50% by weight. Solids, in a further advantageous manner a maximum of 40% by weight of solids, very advantageously not more than 30% by weight solids, in a particularly advantageous manner not more than 25% by weight solids, most preferably not more than 20% by weight Solid, in a substantially advantageous manner, a maximum of 15 wt .-% solids, in a very advantageous manner, a maximum of 10 wt .-% solids, in a very advantageous manner, a maximum of 8 wt .-% solids, most preferably a maximum of 5 wt .-% solids , in most advantageously a maximum of 4 wt .-% solids, in exceptionally advantageous manner, a maximum of 3 wt .-% solids, in an exceptionally advantageous manner, a maximum of 2 wt. % Solids, in an extremely advantageous manner at most 1% by weight solids, in particular not more than 0.07% by weight solids, most preferably not more than 0.05% by weight solids.

It may also be advantageous for the purposes of the invention if a certain minimum amount of solids in the liquid preparation is not exceeded. If such a maximum amount is not undershot, so is another preferred embodiment. Advantageously, in one particular preferred embodiment, the agent contains at least 0.005% by weight of solids, in a considerably advantageous manner at least 0.01% by weight of solids, more preferably at least 0.03% by weight of solids, more preferably at least zero , 05 wt .-% solids, more preferably at least 1 wt .-% solids, in a very advantageous manner at least 1, 5 wt .-% solids, in a particularly advantageous manner at least 2 wt .-% solids, in very particular advantageously at least 2.5% by weight of solids, in a significantly advantageous manner at least 3% by weight of solids, in a significantly advantageous manner at least 4% by weight of solids, in an extremely advantageous manner at least 5% by weight of solids most advantageously at least 8 wt .-% solids, in an extremely advantageous manner, at least 10 wt .-% solids, in an exceptionally advantageous manner at least 15 wt .-% solids, in Exceptional I advantageously at least 20 wt .-% solids, in an extremely advantageous manner, at least 25 wt .-% solids, in particular at least 30 wt .-% solids, in an advantageous manner at least 35 wt .-% solids.

However, it can also be advantageous in the context of another, likewise preferred embodiment, when solids are contained in specific amounts in the liquid preparation. If the agent contains solids in amounts of advantageously 0.01-80 wt .-%, in a considerably advantageous manner in amounts of 0.02-70 wt .-%, more preferably in amounts of 0.05-60 wt. -%, in a further advantageous manner in amounts of 0.1-50 wt .-%, even more advantageously in amounts of 0.5-40 wt .-%, very advantageously in amounts of 1-30 wt. -%, in a particularly advantageous manner in amounts of 1, 5-20 wt .-%, in a particularly advantageous manner in amounts of 2-10 wt .-%, in particular in amounts of 3-7 wt .-%, so is a preferred embodiment of the invention.

The benefit associated with incorporating the solids into the liquid preparation also includes visual aspects which can provide the product with improved aesthetics and thus are beneficial to the overall attractiveness of the product.

Particularly positive associations in this case call forth those prepared according to the invention, in which the solids are spatially stable in the liquid preparation with a uniform spatial distribution, especially float in this, i. neither sink nor rise. "Uniform spatial distribution" means that the solids are not present in very large quantities in certain parts by volume of the preparations and in very small amounts in other parts by volume, but that an approximately equal amount of solids is contained in all parts of the volume, which corresponds to a preferred embodiment However, the concomitant advantage is not only of an optical nature, but also benefits the consumer in the application, ie dosing, since the solids advantageously comprise active substances, for example a liquid detergent which contains active substances in solids which are not spatially stable Before use (ie before dosing), shake by the consumer first to achieve a good distribution of the active ingredients in the liquid detergent, otherwise he would run the risk of dosing either too little or too much of the active substances contained in the solids If, on the other hand, the solids are spatially stable with a uniform spatial distribution, for example, in a liquid detergent, the consumer can immediately dose them without having to take any further precautions.

The nature of the solids to be added is essentially not fundamentally limited. It depends essentially on what and in what form should be introduced into the liquid preparation, as well as the way in which the solid body should interact during use.

For example, it is clear that a different condition is attached to a scouring milk, in which the solids contained, for example, abrasive components, than, for example, a salad dressing containing, for example, microencapsulated flavors. In one case, the abrasive components must withstand relatively high mechanical loads, in the other case, the microencapsulated flavors must be released, for example, during the chewing process.

However, according to a preferred embodiment, it is advantageous if the solids contained have a high stability, preferably mechanical stability, and likewise it is preferred according to another advantageous embodiment if they have low stability, preferably mechanical stability, or else that stability , preferably mechanical stability, lies between these extremes.

The stability may relate to all physical and / or chemical and / or biological loads. A physical load is, for example, a mechanical stimulus, such as pressure or friction, or else a temperature change, etc. A chemical load is, for example, a pH change, an ionic strength change, a change in the uphill or hydrophilicity of the surrounding medium, etc. Biological stress results, for example, from exposure to microorganisms, ie microorganisms are allowed to act on the shaped body or the like. The same applies to any other biological factors.

However, particularly advantageous with regard to the present invention are those solids which are sensitive to mechanical stresses, in particular shear-sensitive solids are preferred. Their use in the process according to the invention represents a preferred embodiment of the invention.

Solid bodies, which are sensitive to mechanical stresses, are therefore extremely useful for many liquid preparations, because in this way it is ensured that the solids lose their integrity almost quantitatively during use, thereby releasing preferably active substances contained, and thus fulfilling their purpose.

The present inventive method brings in this respect an extraordinary improvement. So far, it was only possible to incorporate solids which are at least mechanically stable so that they survive the passage through a normal production plant relatively unscathed. However, this has caused great problems in the application. For example, it has been observed in many cases that solids do not "dissolve" in the actual application, as is illustrated by machine textile washing. In some cases it has been observed, for example, that the solids, rather than "dissolving", are intact deposited on the textile. This was disadvantageous in two ways. First, the valuable active substances preferably contained in the solids were not released during the washing process and therefore could not exert their effect, and second, the solids were on the textile rightly perceived as impurities. It can even be contaminated the washing machine.

On the other hand, the present invention makes it possible to use even those solids which are particularly sensitive to stresses, in particular mechanical stresses, and are in particular exceptionally shear-sensitive. Advantageously, these exceptionally sensitive solids can now be incorporated into the liquid preparations without problems and preferably intact with the aid of the novel process. This ensures that the solids in question can in any case be "dissolved" during the actual application or lose their integrity.

Therefore, such methods according to the invention, in which the solids to be added are particularly sensitive to external stimuli, are preferably sensitive to mechanical stresses, are particularly shear-sensitive, a preferred embodiment of the invention.

In order to ensure that the solids to be added can be incorporated intact into the liquid preparation, it is advantageous if the addition of the solids into the preparation and mixing with the latter takes place under conditions of low shear. This corresponds to a preferred embodiment.

It is likewise advantageous if, after the solids have been added, the preparation is supplied to the bottling under conditions of low shear. This corresponds to a preferred embodiment.

It is advantageous for the method according to the invention if the flow behavior of the liquid preparation after addition of the solids in the piping systems to be flown thereafter is essentially associated with Reynolds numbers up to 10000, but preferably less than 2300, advantageously less than 2000, in particular less than 1500. This corresponds to a preferred embodiment.

The Reynolds number (Re) is the characteristic quantity for the course of flow processes in preferably fully filled cavities (pipelines) by defining the ratio of inertial to frictional forces in flowing liquids:

Re _ ^2R ' ^{V "} P _ ^ L-! _ ²⁰⁰ Q η v π- R -k - t ^2'

In the equations, R = radius of the flow-through pipe or I = diameter or characteristic length, V = mean flow velocity, or w = characteristic velocity, p = density of the liquid to be measured, η = dynamic viscosity, v = kinema- table viscosity, Q = volume flowed through, k = device constant for viscometer without extraneous pressure and t = flow time.

It is also advantageous if the flow behavior of the liquid preparation after addition of the solids in the then to be flowed through piping systems with friction numbers to 0.03, preferably lying in the range 0.03 to 0.1, accompanied.

The friction coefficient obeys Darcy's pressure loss equation as follows: λ = (ΔP-d'2) / (hp'U ² )

In the equation, λ = friction coefficient, ΔP = pressure loss in the pipe, d = diameter of the pipe, I = length of the pipe, p = density of the liquid, U = velocity. For example, there are also various empirical approaches to determining \. In the laminar flow region, preferably λ = 64 / Re. For Reynolds numbers in the range of 2320 to 10000, λ = 0.3164 / (Re ⁰ ^'25 ). For Reynolds numbers <100000, Blasius holds λ = 0.0054 + 0.396 / Re ⁰ ' ³ . In principle, λ is inversely proportional to Re in laminar flow, whereas in the turbulent range, there is little dependence.

Pressure losses in the piping system, however, not only occur in the pipe, but also in other components such as elbows, knees, flange, valves, taps, valves, orifices, etc. These additional pressure losses are not distributed over the entire length in contrast to the pipe. One speaks therefore of local pressure losses. The local pressure loss is taken into account by a coefficient ζ for detecting the pressure loss: Δp = ζ-0,5-pu ² .

In the equation, ζ = coefficient of individual resistance ΔP = pressure loss in the component, u = velocity, p = density of the liquid.

Coefficients of the individual resistances for various components can be taken from the literature, e.g. from: K.F. Pavlov, P.C. Romankow, A.A: Noskow: Examples and Exercises in Chemical Engineering, VEB Deutscher Verlag für Grundstoffindustrie, 1979. Coefficients of individual resistances are generally between 0 (e.g., tube expansions) and 20 (e.g., valves), depending on the component.

For the present invention it is advantageous if the coefficients of the individual resistances of the components for the pipeline system after addition of the solids are in each case per individual resistance in the range 0 to 20, preferably a total value of 10, advantageously of 7, more advantageously of 5, in a further advantageous manner of 4, in still further advantageous manner of 3, in particular of 2 is not exceeded. The liquid preparation which can be prepared according to the method according to the invention is subject to the nature of the liquid contained substantially no restriction. It can therefore be composed of most arbitrary liquids or solvents, etc.

A particularly preferred liquid in this context is the water. Water has the advantages that it is clear, odorless and tasteless, colorless, available inexpensively in large quantities, easy to handle and enjoyable and ecologically harmless.

Preferred liquid preparations are therefore aqueous agents. This corresponds to a preferred embodiment. In the context of this invention, an aqueous agent is preferably present if it contains at least 0.01% by weight of water.

Advantageously, in a certain preferred embodiment, the composition contains at least 1% by weight of water, in a considerably advantageous manner at least 5% by weight of water, more preferably at least 10% by weight of water, more preferably at least 15% by weight. Water, more preferably at least 20 wt .-% water, in a very advantageous manner at least 25 wt .-% water, in a particularly advantageous manner at least 30 wt .-% water, in a particularly advantageous manner at least 35 wt .-% Water, in a substantially advantageous manner, at least 40 wt .-% water, in a very advantageous manner, at least 45 wt .-% water, in an extremely advantageous manner at least 50 wt .-% water, most preferably at least 55 wt .-% water in an exceedingly advantageous manner at least 60% by weight of water, in an exceptionally advantageous manner at least 65% by weight of water, in an exceptionally advantageous manner at least 70% by weight of water, in extremely advantageous proportions at least 75% by weight of water, in particular at least 80% by weight of water, most preferably at least 85% by weight of water.

However, it can also be advantageous in the sense of another, likewise preferred embodiment that a certain upper limit of water is not exceeded. If the agent at most 95 wt .-% water, in a considerably advantageous manner at most 90 wt .-% water, more preferably at most 85 wt .-% water, more preferably at most 80 wt .-% water, in even more advantageous A maximum of 75 wt .-% water, in a very advantageous manner, a maximum of 70 wt .-% water, in a particularly advantageous manner, a maximum of 65 wt .-% water, in a particularly advantageous manner, a maximum of 60 wt .-% water, in a considerably advantageous manner a maximum of 55 wt .-% water, in a very advantageous manner, a maximum of 50 wt .-% water, in an extremely advantageous manner, a maximum of 45 wt .-% water, most preferably a maximum of 40 wt .-% water, in a very advantageous maximum 35 wt .-% water, in exceptionally advantageous manner, a maximum of 30 wt .-% water, in an exceptionally advantageous manner, a maximum of 25 wt .-% water, in an extremely advantageous manner, a maximum of 20 wt .-% water, in particular a maximum of 15 wt .-% Water, in most advantageous W not more than 10% by weight of water. According to a further preferred embodiment, the agent is anhydrous, that is less than 10 wt .-%, preferably less than 5 wt .-%, more preferably less than 3 wt%, more preferably less than 1 wt .-% water in particular, it is entirely anhydrous.

However, it can also be advantageous in the sense of another, likewise preferred embodiment, if water is contained in certain quantitative ranges. When the composition advantageously contains water in amounts of 5-95% by weight, in significantly advantageous amounts of 10-90% by weight, more preferably in amounts of 15-85% by weight, more advantageously In amounts of from 20 to 80% by weight, more preferably in amounts of from 25 to 75% by weight, very advantageously in amounts of from 30 to 70% by weight, most preferably in amounts of 35-65 wt .-%, in a particularly advantageous manner in amounts of 40-60 wt .-%, in particular in amounts of 45-55 wt .-%, so is a preferred embodiment of the invention.

As far as the size of the solids to be added to the liquid preparation is concerned, essentially all conceivable sizes are possible here, which make sense in the sense of the respective intended application. Accordingly, the solids may have a diameter along their largest dimension of preferably 0.01 to 20,000 μm, which corresponds to a preferred embodiment.

According to another preferred embodiment, however, the solids are smaller than 20,000 μm.

If the solid has a diameter along its maximum extent of a maximum of 10,000 microns, in a considerably advantageous manner, a maximum of 9000 microns, more preferably a maximum of 8000 microns, in a further advantageous maximum 7000 microns, in a further advantageous manner, a maximum of 6000 microns, in very advantageous Way maximum 5000 microns, in a particularly advantageous manner, a maximum of 4000 microns, in a particularly advantageous manner, a maximum of 3000 microns, in a considerably advantageous manner, a maximum of 2000 microns, in a very advantageous manner, a maximum of 1000 microns, in a very advantageous manner, a maximum of 500 microns, in highly advantageous Way maximally 400 .mu.m, in a very advantageous manner a maximum of 300 .mu.m, in an exceptionally advantageous manner at most 200 .mu.m, in an exceptionally advantageous manner at most 100 .mu.m, in an exceptionally advantageous manner at most 50 .mu.m, in particular at most 10 .mu.m, in the most advantageous manner at most 1 .mu.m is a preferred embodiment.

However, it may also be desirable for certain applications advantageously if the solids have a certain minimum size. Therefore, if the solid has a diameter along its largest dimension of at least 0.1 μm, in considerably advantageous Advantageously, at least 1 μm, more preferably at least 10 μm, more preferably at least 100 μm, even more advantageously at least 200 μm, very advantageously at least 400 μm, in a particularly advantageous manner at least 600 μm, in a particularly advantageous manner Way at least 800 microns, in a considerably advantageous manner at least 1000 microns, in a very advantageous manner at least 2000 microns, in an extremely advantageous manner at least 3000 microns, most advantageously at least 4000 microns, in an extremely advantageous manner at least 5000 microns, in exceptionally advantageous manner at least 6000 microns, in an exceptionally advantageous manner at least 7000 microns, in an extremely advantageous manner at least 8000 microns, in particular at least 9000 microns, in an advantageous manner at least 10,000 microns, so again is a preferred embodiment.

However, it can also be advantageous in the context of another, likewise preferred embodiment if the solid body has a diameter along its greatest extent, which is contained in certain length ranges. If the agent advantageously contains solid particles with a diameter along its largest dimension of 1-10000 μm, in a considerably advantageous manner in quantities of 10-9000 μm, more advantageously in quantities of 100-9000 μm, and in an advantageous manner in quantities of 200-7000 microns, in a further advantageous manner in amounts of 300-6000 microns, in a very advantageous manner in amounts of 400-5000 microns, in a particularly advantageous manner in amounts of 500-4000 microns, in a particularly advantageous manner in amounts of 600-3000 microns, especially in amounts of 700-2000 microns, so is a preferred embodiment of the invention.

It is within the scope of a further preferred embodiment advantageous if the solids contained in the liquid preparation have a substantially spherical or spherical shape.

For a stable preparation of the solids in the liquid preparation is preferably a precise density adjustment of solids advantageous, for example via hollow microspheres, see below), to prevent later floating and / or lowering of the capsules in the detergent even safer.

It is also advantageous in a further preferred embodiment, when the solids contained in the liquid composition have a narrow particle size range, which is particularly the case when the grain size distribution of the solid body is such that the ratio of d _{so as} to d ₉₀ of the solid substantially at least 0.5, preferably at least 0.6, advantageously at least 0.75, more preferably at least 0.8 and in particular at least 0.9, wherein d _{50 represents} the median value. The median value is defined as the particle size below and above which 50% of the particle quantity is located. correspond Accordingly, 90% of the particulate matter is below the value at d ₉₀ , ie 10% higher. The ratio d ₅₀ / dgo approximates the value of 1 for very narrow particle size distributions, or is well below 0.5 for broad distributions.

According to a further preferred embodiment, the solids essentially have an average form factor of at least 0.77, preferably of at least 0.79, advantageously of at least 0.83, in particular of at least 0.87. Substantially here means, in particular, that at least 80%, preferably at least 90% and, even more advantageously, at least 95% of the solids have the aforementioned form factor.

The shape factor in the sense of the present invention can be precisely determined by modern particle-measuring techniques with digital image processing. In a typical particle shape analysis, as it is feasible, for example, with the Camsizer® system from Retsch Technology or with the KeSizer® Kemira, based on the fact that the particles or the solid state with ^'a light source to be irradiated and the particle detected as projection , digitized and processed by computer technology. The surface curvature is determined by an optical measurement method, which determines the "shadow cast" of the parts to be examined and converts them into a corresponding form factor.The underlying principle for determining the shape factor was described by Gordon Rittenhouse in "A Visual Method of estimating two-dimensional sphericity "in Journal of Sedimentary Petrology, Vol. 13, No. 2, pp. 79-81., The numerical values for d ₅₀ and d ₉₀ are also available via the aforementioned measuring method.

When the solids are capsules, microcapsules or speckles, a preferred embodiment is present. The solids may also be agglomerates or granules. The solids may also be granules, e.g. like the grains of sand or rice grains. The solids could also be shreds or have film structure.

Capsules are in the broadest sense all those structures in which solid, semi-solid or liquid substances are surrounded by cladding layers. The cladding layers can be composed of all possible substances, for example containing gelatin, wax, (co) polymers or wafer material. The production of capsules is known to the person skilled in the art or it can be found in the relevant specialist literature. A capsule may have multiple cladding layers.

Advantageously, microencapsulation is the term for the encapsulation preferably finely dispersed liquid or solid phases by coating with film-forming (co) polymers, which are reflected, for example, after emulsification and coacervation or interfacial polymerization on the material to be enveloped. The microscopically small capsules (synonym: nano capsules) can be dried like powder. In this way, for example, gasoline, water, alcohol, pharmaceuticals, solvents, vitamins, enzymes, liquid crystals, food flavorings, perfumes and many other substances can be converted into a dry matter that can not dry out and. If necessary, their contents become free (liquid) again by thermal, mechanical, chemical or enzymatic action.

The term "microcapsule" is therefore preferably understood to mean aggregates which contain at least one solid, semi-solid or liquid core which is enclosed by at least one preferably continuous shell, in particular a shell of polymer (s). These are usually finely dispersed liquid or solid phases coated with film-forming polymers, during the production of which the polymers precipitate on the material to be enveloped after emulsification and coacervation or interfacial polymerization. The microscopic capsules can be dried like powder. Besides mononuclear microcapsules, multinuclear aggregates, also called microspheres, are known, which contain two or more cores distributed in the continuous shell material. Mono- or polynuclear microcapsules can also be enclosed by an additional second, third, etc., sheath. Preferred are mononuclear microcapsules with a continuous shell. The shell may be made of natural, semi-synthetic or synthetic materials. Naturally, shell materials are, for example, gum arabic, agar agar, agarose, maltodextrins, alginic acid or its salts, e.g. Sodium or calcium alginate, fats and fatty acids, cetyl alcohol, collagen, chitosan, lecithins, gelatin, albumin, shellac, polysaccharides such as starch or dextran, sucrose and waxes. Semisynthetic shell materials include chemically modified celluloses, especially cellulose esters and ethers, e.g. Cellulose acetate, ethylcellulose, hydroxypropylcellulose, hydroxypropylmethylcellulose and carboxymethylcellulose, and also starch derivatives, in particular starch ethers and esters. Synthetic shell materials are, for example, polymers such as polyacrylates, polyamides, polyvinyl alcohol or polyvinylpyrrolidone.

In the interior of the solids, in particular capsules, microcapsules or speckles, it is possible to enclose preferably stable, chemically or physically incompatible as well as volatile components (= active ingredients) in a stable and transport-stable manner. In the solids, for example, optical brighteners, surfactants, complexing agents, bleaching agents, bleach activators, dyes and fragrances, antioxidants, builders, enzymes, enzyme stabilizers, antimicrobial agents, cationic surfactants, vitamins, proteins, preservatives, detergency booster or pearlescers, grayness inhibitors, Anti redeposition agents, pH adjusters, electrolytes, foam inhibitors and UV absorbers are to be used to illustrate individual illustrative examples, which are particularly relevant in the context of detergents and cleaners. The fillings of the solids may preferably be solids or liquids in the form of solutions or emulsions or suspensions. The microcapsules are accessible by methods known in the art, with coacervation and interfacial polymerization being the most important. As microcapsules all surfactant-stable microcapsules available on the market can be used, for example the commercial products (in parentheses is the shell material) Hallcrest Microcapsules (gelatin, gum arabic), co / ef / ca Thalaspheres (marine collagen), Lipotec millicapsules (alginic acid, Agar-agar), induchem unispheres (lactose, microcrystalline cellulose, hydroxypropylmethylcellulose); Unicerin C30 (lactose, microcrystalline cellulose, hydroxypropylmethylcellulose), Kobo Glycospheres (modified starch, fatty acid esters, phospholipids), soft spheres (modified agar agar) and Kuhs Probiol Nanospheres (phospholipids).

Alternatively, it is also possible to use particles which have no core-shell structure but in which the active substance is distributed in a matrix of a matrix-forming material. Such particles are also referred to as "speckies".

A preferred matrix-forming material is alginate. To produce alginate-based speckles, an aqueous alginate solution, which preferably also contains the active substance to be enclosed or the active substances to be enclosed, is dripped off and then cured in a precipitation bath containing Ca ²⁺ ions or Al ³⁺ ions. In a particular embodiment of the present invention, the precipitation bath contains a Ca ²⁺ concentration of at least 0.15 mol / l.

It may be advantageous that the alginate-based speckles are subsequently washed with water and then washed in an aqueous solution with a complexing agent to free Ca ²⁺ ions or free Al ³⁺ ions, which undesirable interactions with ingredients of the liquid preparation can go out, wash out. Subsequently, the alginate-based speckles are washed again with water to remove excess complexing agent.

Alternatively, other, matrix-forming materials can be used instead of alginate. Examples of matrix-forming materials include polyethylene glycol, polyvinylpyrrolidone, polymethacrylate, polylysine, poloxamer, polyvinyl alcohol, polyacrylic acid, polyethylene oxide, polyethoxyoxazoline, albumin, gelatin, acacia, chitosan, cellulose, dextran, Ficoll®, starch, hydroxyethylcellulose, hydroxypropylcellulose, Hydroxypropylmethylcellulose, hyaluronic acid, carboxymethylcellulose, carboxymethylcellulose, deacetylated chitosan, dextran sulfate and derivatives of these materials. The matrix formation in these materials takes place for example via gelation, polyanion-polycation interactions or polyelectrolyte-metal ion interactions and is well known in the art as well as the production of particles with these matrix-forming materials. The solids may preferably be stably dispersed in the liquid preparations. Stable means that the compositions are stable at room temperature and at 40 ^° C. for a period of at least 4 weeks, and preferably for at least 6 weeks, without the medium creaming or sedimenting. An important advantage of the present invention in this combination is that extraordinarily stable preparations can be provided by the process according to the invention. The preparations are in particular so stable because the solids can be incorporated in the preparation according to the invention substantially intact in the preparation. Such essentially intact solids are, of course, much more stable than those which suffered damage to shape and integrity even during production of the preparation. It follows that the entire preparation is even more stable, especially in terms of storage and transport.

The release of the active substances from the solids is usually carried out during the application of the agents containing them by destruction of the shell or the matrix, preferably due to mechanical, thermal, chemical or enzymatic action.

In a preferred embodiment, the solids additionally contain at least one hollow microspheres.

Hollow microspheres have a diameter of preferably 2 to 500 μm, in particular of 5 to 20 μm, and a specific gravity of less than preferably 1 g-cm ^'3 . By incorporating one or more hollow microspheres into the respective solids, the density of the solids can be adjusted to the density of the surrounding preparation, thereby preventing undesirable settling or floating (creaming) of the capsules.

Preferably, the hollow microspheres are round and smooth. The hollow microspheres may be made of inorganic material such as water glass, aluminum silicate, borosilicate glass soda lime glass or a ceramic or of organic polymers such as homo- or copolymers of styrene, acrylonitrile and vinylidene chloride. Suitable hollow microspheres are commercially available, for example, under the names Fillite® (ex Trelleborg Filled), Expancel® (ex Akzo Nobel), Scotchlite® (ex 3M), Dualite® (es Sove Reign Specialty Chemicals), Sphericel® (ex Potters Industries). , Zeeospheres® (ex 3M), Q-Cel® (ex PQ Corporation) or Extendospheres® (ex PQ Corporation). Further suitable hollow microspheres are available under the product name E-Spheres from OMEGA MINERALS. E-spheres are white, hollow ceramic microspheres, which are available in different grain sizes, particle size distributions, bulk densities and bulk volumes. Many of the hollow microspheres mentioned are chemically inert and are dispersed in the wash liquor after destruction of the capsule and then removed with it. In particular, with regard to the intended use, it may be advantageous if the viscosity of the preparation falls below certain values. The viscosity of the liquid preparation can be measured by conventional standard methods (for example, Brookfield LVT-II viscosimeter at 20 rpm and 20 ^° C., spindle 3).

If the viscosity of the preparation has a maximum value of 20,000 mPas, in a considerably advantageous manner at most 15,000 mPas, more preferably not more than 10,000 mPas, more preferably not more than 9,000 mPas, even more preferably not more than 8,000 mPas, most preferably not more than 7,000 mPas, in a particularly advantageous manner, a maximum of 6000 mPas, in a particularly advantageous manner, a maximum of 5000 mPas, in a significantly advantageous manner, a maximum of 4000 mPas, in a very advantageous manner, a maximum of 3000 mPas, in an extremely advantageous manner a maximum of 2000 mPas, in particular a maximum of 1000 mPas , so is a preferred embodiment.

On the other hand, with regard to the subsequent application, it may also be advantageous if the viscosity of the preparation exceeds certain values. If the viscosity therefore has a value of at least 0.1 mPas, in a considerably advantageous manner at least 1 mPas, more preferably at least 10 mPas, more preferably at least 100 mPas, even more advantageously at least 200 mPas, very advantageously at least 300 mPas, in a particularly advantageous manner at least 400 mPas, in a particularly advantageous manner at least 500 mPas, in a considerably advantageous manner at least 600 mPas, in a remarkably advantageous manner at least 700 mPas, in an extremely advantageous manner at least 800 mPas, most advantageously at least 900 mPas, in an extremely advantageous manner at least 1000 mPas, in an exceptionally advantageous manner at least 1200 mPas, in an exceptionally advantageous manner at least 1400 mPas, in an extremely advantageous manner at least 1500 mPas, in particular at least 1700 mPas, in an advantageous manner at least 2000 mPas, then again another , also preferred embodiment.

However, it can also be advantageous in the context of another, likewise preferred embodiment if the preparation has a viscosity which lies in certain ranges. If the preparation has a viscosity of advantageously 10-10000 mPas, in a considerably advantageous manner in quantities of 200-9000 mPas, more advantageously in quantities of 300-8000 mPas, moreover in amounts of 400-7000 mPas, in even more advantageously in amounts of 500-6000 mPas, very advantageously in amounts of 1000-5000 mPas, more preferably in amounts of 1500-4500 mPas, in a particularly advantageous manner in amounts of 1800-4200 mPas, in particular in amounts of 2000-4000 mPas, so is a preferred embodiment of the invention. Advantageously, the preparation according to the invention also contains thickening agents. Thickening agents are preferably organic, high molecular weight substances which preferably absorb liquids (usually water), thereby advantageously swelling (swelling) and finally (except for the inorganic thickening agents.) Preferably pass into viscous true or colloidal solutions. Thickeners are preferably used to increase the viscosity of liquids and to improve the thixotropic properties of gels. Thickeners therefore play a role in the manufacture of many technical, cosmetic, pharmaceutical or dietary products and foods (all of which are within the scope of the invention), for example creams, cleansers, finishes, printing inks, paint dispersions, adhesives, puddings, slimming products (The organic thickening agents are preferably edible, but often have no nutritional value).

According to a preferred embodiment, the preparation to be prepared according to the invention therefore contains thickening agents, in particular selected from at least one of the following groups: a) Organic, natural thickening agents (here in particular substances such as agar-agar, carrageenan, tragacanth, gum arabic, alginates, pectins, polyoses, guar Flour, locust bean gum, starch, dextrins, gelatin, casein, etc.) b) Organic, modified natural products (here in particular substances such as carboxymethylcellulose and other cellulose ethers, ethylhydroxyethylcellulose, hydroxyethylcellulose, hydroxypropylmethylcellulose and hydroxypropylcellulose, etc., core flour ethers). c) organic, fully synthetic thickening agents (here preferably polyacrylic and polymethacrylic compounds, polyvinyl alcohols, polyacrylamides, polyvinylpyrrolidone, polyethylene glycols, vinyl polymers, polycarboxylic acids, styrene-maleic anhydride copolymers and their salts, polyethers, polyimines, polyamides, etc., but in particular the copolymers and terpolymers of acrylic and methacrylic acid) d) inorganic thickeners (here in particular polysilicic acids, clay minerals such as montmorillonite hectorite, zeolites, silicas, etc.). e) Low molecular weight, organic products (here in particular: metal soaps, hydrogenated castor oil, modified fatty derivatives, polyamides, etc.). f) Associative thickeners.

Associative thickeners differ, for example, from the abovementioned modified natural substances and the organic, fully synthetic thickeners in that, in addition to water-solubilizing hydrophilic groups, they preferably also contain hydrophobic terminal or side groups in the molecule. As a result, associative thickeners advantageously have a surfactant character and are preferably capable of forming micelles. Particularly preferred associative thickeners are a) hydrophobically modified Polyacrylates which preferably contain in a anionic acrylate thickener molecule by copolymerization built nonionic hydrophilic and hydrophobic groups; b) hydrophobically modified cellulose ethers, preferably prepared by reaction of hydroxyethylcellulose during the etherification or subsequently with long-chain alkyl epoxides or -halides; c) hydrophobically modified polyacrylamides, preferably prepared by copolymerization of acrylamide with alkyl-modified acrylamide and optionally acrylic acid; d) hydrophobically modified polyethers, e) associative polyurethane thickeners, preferably consisting of urethane group-linked hydrophilic, relatively high molecular weight polyether segments, advantageously capped with at least two terminal, hydrophobic molecule groups.

The thickener may thus, for example, a polyacrylate thickener, xanthan gum, gellan gum, guar gum, alginate, carrageenan, carboxymethylcellulose, bentonites, Wellan gum, locust bean gum, agar-agar, tragacanth, gum arabic, pectins, polyoses, starch, dextrins, gelatin and Casein include.

The polyacrylic and polymethacrylic thickeners include, for example, the high molecular weight homopolymers of acrylic acid crosslinked with a polyalkenyl polyether, in particular an allyl ether of sucrose, pentaerythritol or propylene (INCI name according to "International Dictionary of Cosmetic Ingredients" of "The Cosmetic, Toiletry and Fragrance Association (CTFA) ": Carbomer), also referred to as carboxyvinyl polymers. Such polyacrylic acids are available, inter alia, from the company 3V Sigma under the 'trade name Polygel®, eg Polygel DA, and from the company BF Goodrich under the trade name Carbopol®, eg Carbopol 940 (molecular weight about 4,000,000), Carbopol 941 ( Molecular weight about 1. 250,000) or Carbopol 934 (molecular weight about 3,000,000). Furthermore include the following acrylic acid copolymers: (i) copolymers of two or more monomers from the group of acrylic acid, methacrylic acid and their simple, preferably with CI_ -Alka _4-nolen formed, esters (INCI Acrylates Copolymer), to which about the copolymers of methacrylic acid, butyl acrylate and methyl methacrylate (CAS designation according to Chemical Abstracts Service: 25035-69-2) or butyl acrylate and methyl methacrylate (CAS 25852-37-3) and the example of the company. Rohm & Haas under the trade names Aculyn® and Acusol®, as well as from the company Degussa (Goldschmidt) under the trade name Tego® polymer, for example the anionic non-associative polymers Aculyn 22, Aculyn 28, Aculyn 33 (crosslinked), Acusol 810, Acusol 820, Acusol 823 and Acusol 830 (CAS 25852-37-3); (ii) crosslinked high molecular weight acrylic acid copolymers, such as those crosslinked with an allyl ether of sucrose or pentaerythritol copolymers of C ₁₀ - ₃₀ alkyl acrylates with one or more monomers from the group of acrylic acid, methacrylic acid and their simple, preferably with Ci _-4 - Alkanols formed, esters (INCI AcryIates / Ci _O .3o alkyl acrylate crosspolymer) include and which are available, for example, from the company. BF Goodrich under the trade name Carbopol®, for example, the hydrophobized Carbopol ETD 2623 and Carbopol 1382th (INCI Acrylates / C, _0. ₃₀ Alkyl Acrylate Crosspolymer) and Carbopol Aqua 30 (formerly Carbopol EX 473).

Another preferred polymeric thickening agent is xanthan gum, a microbial anionic heteropolysaccharide produced by Xanthomonas campestris and some other species under aerobic conditions and having a molecular weight of from 2 to 15 million daltons. Xanthan is formed from a chain of β-1,4-linked glucose (cellulose) with side chains. The structure of the subgroups consists of glucose, mannose, glucuronic acid, acetate and pyruvate, the number of pyruvate units determining the viscosity of the xanthan gum.

The preparations to be prepared according to the invention contain, depending on the purpose they are intended to serve, correspondingly suitable ingredients which are familiar to the respective person skilled in the art or are accessible from the relevant technical literature. For example, liquid foods contain consumable ingredients, etc.

Particularly preferred preparations for the purposes of this invention are those from the field of detergents and cleaners, including fabric softeners and textile treatment agents in the broadest sense.

In addition to the solids, the liquid detergents and cleaners to be produced according to the invention contain surfactant (s), wherein anionic, nonionic, cationic and / or amphoteric surfactants can be used. From an application point of view, preference is given to mixtures of anionic and nonionic surfactants. The total surfactant content of a preferred liquid detergent and cleaning agent is preferably below 40 wt .-% and particularly preferably below 35 wt .-%, based on the total liquid detergent and cleaning agent.

The nonionic surfactants used are preferably alkoxylated, advantageously ethoxylated, in particular primary, alcohols having preferably 8 to 18 carbon atoms and an average of 1 to 12 moles of ethylene oxide (EO) per mole of alcohol, in which the alcohol residue can be linear or preferably methyl-branched in the 2-position or linear and methyl-branched radicals in the mixture can contain, as they are usually present in Oxoalkoholresten. In particular, however, alcohol ethoxylates with linear radicals of alcohols of native origin having 12 to 18 C atoms, for example coconut, palm, tallow or oleyl alcohol, and on average 2 to 8 EO per mole of alcohol are preferred. The preferred ethoxylated alcohols include, for example, C _12-14 -alcohols with 3 EO, 4 EO or 7 EO, C _9-11 -alkoxy with 7 EO, C ₁₃ . _15- alcohols with 3 EO, 5 EO, 7 EO or 8 EO, C ₁₂ . ₁₈ alcohols with 3 EO, 5 EO or 7 EO and mixtures of these, such as mixtures of C _12-14 -alcohol with 3 EO and C _12-18 -alcohol with 7 EO. The stated ethoxylation de represent statistical averages, which can be a whole or a fractional number for a particular product. Preferred alcohol ethoxylates have a narrow homolog distribution (narrow rank ethoxylates, NRE). In addition to these nonionic surfactants, fatty alcohols with more than 12 EO can also be used. Examples of these are tallow fatty alcohol with 14 EO, 25 EO, 30 EO or 40 EO. Nonionic surfactants which contain EO and PO groups together in the molecule can also be used according to the invention. Here, block copolymers with EO-PO block units or PO-EO block units can be used, but also EO-PO-EO copolymers or PO-EO-PO copolymers. Of course, mixed alkoxylated niotic side can be used in which EO and PO units are not distributed blockwise, but statistically distributed. Such products are available by the simultaneous action of ethylene and propylene oxide on fatty alcohols.

In addition, as further nonionic surfactants and alkyl glycosides of the general formula RO (G) _x can be used in which R is a primary straight-chain or methyl-branched, especially in the 2-position methyl-branched aliphatic radical having 8 to 22, preferably 12 to 18 carbon atoms and G is the symbol which represents a glycose unit having 5 or 6 C atoms, preferably glucose. The degree of oligomerization x, which indicates the distribution of monoglycosides and oligoglycosides, is any number between 1 and 10; preferably x is 1, 2 to 1, 4.

Another class of preferred nonionic surfactants which are used either as the sole nonionic surfactant or in combination with other nonionic surfactants are alkoxylated, preferably ethoxylated or ethoxylated and propoxylated fatty acid alkyl esters, preferably having 1 to 4 carbon atoms in the alkyl chain, in particular fatty acid methyl ester, as described for example in Japanese Patent Application JP 58/217598 or which are preferably prepared according to the method described in International Patent Application WO-A-90/13533.

Nonionic surfactants of the amine oxide type, for example N-cocoalkyl-N, N-dimethylamine oxide and N-tallowalkyl-N, N-dihydroxyethylamine oxide, and the fatty acid alkanolamides may also be suitable. The amount of these nonionic surfactants is preferably not more than that of the ethoxylated fatty alcohols, especially not more than half thereof.

Further suitable surfactants are polyhydroxy fatty acid amides of the formula (1), R ¹

I

R-CO-N- [Z] (1) in the RCO for an aliphatic acyl radical having 6 to 22 carbon atoms, R ^ for hydrogen, an alkyl or hydroxyalkyl radical having 1 to 4 carbon atoms and [Z] for a linear or branched polyhydroxyalkyl having 3 to 10 carbon atoms and 3 to 10 hydroxyl groups. The polyhydroxy fatty acid amides are known substances which can usually be obtained by reductive amination of a reducing sugar with ammonia, an alkylamine or an alkanolamine and subsequent acylation with a fatty acid, a fatty acid alkyl ester or a fatty acid chloride.

The group of polyhydroxy fatty acid amides also includes compounds of the formula (2)

R ¹ -OR ²

I

R-CO-N- [Z] (2) in the R is a linear or branched alkyl or alkenyl radical having 7 to 12 carbon atoms, R ^{1 is} a linear, branched or cyclic alkyl radical or an aryl radical having 2 to 8 carbon atoms and R ^{2 is} a linear, branched or cyclic alkyl radical or an aryl radical or an oxyalkyl radical having 1 to 8 carbon atoms, with C _1-4 -alkyl or phenyl radicals being preferred and [Z] being a linear polyhydroxyalkyl radical whose alkyl chain is at least substituted two hydroxyl groups, or alkoxylated, preferably ethoxylated or propoxylated derivatives of this radical.

[Z] is preferably obtained by reductive amination of a sugar, for example glucose, fructose, maltose, lactose, galactose, mannose or xylose. The N-alkoxy- or N-aryloxy-substituted compounds can then be converted into the desired polyhydroxy fatty acid amides, for example according to the teaching of the international application WO-A-95/07331, by reaction with fatty acid methyl esters in the presence of an alkoxide as catalyst.

The content of nonionic surfactants of a preferred liquid detergents and cleaners is preferably 5 to 30 wt .-%, preferably 7 to 20 wt .-% and in particular 9 to 15 wt .-%, each based on the total agent.

As anionic surfactants, for example, those of the sulfonate type and sulfates are used. As surfactants of the sulfonate type preferably come C ₉ .i ₃ -alkylbenzenesulfonates, olefinsulfonate, ie mixtures of alkene and hydroxyalkanesulfonates and disulfonates, as they are, for example, from Ci ₂ -is monoolefins with terminal or internal double bond obtained by sulfonation with gaseous sulfur trioxide and subsequent alkaline or acidic hydrolysis of the sulfonation, into consideration. Also suitable are alkanesulfonates, which are obtained from C ₂ .is alkali-nen for example by sulfochlorination or sulfoxidation and subsequent hydrolysis or neutralization. Likewise suitable are the esters of .alpha.-sulfo fatty acids (ester sulfonates), for example the .alpha.-sulfonated methyl esters of hydrogenated coconut, palm kernel or tallow fatty acids. Further suitable anionic surfactants are sulfated fatty acid glycerol esters. Fatty acid glycerines are to be understood as meaning the mono-, di- and triesters and mixtures thereof, as in the preparation by esterification of a monoglycerol with 1 to 3 mol fatty acid or in the transesterification of triglycerides with 0.3 to 2 mol Glycehn can be obtained. Preferred sulfated fatty acid glycerol esters are the sulfonation products of saturated fatty acids having 6 to 22 carbon atoms, for example caproic acid, caprylic acid, capric acid, myristic acid, lauric acid, palmitic acid, stearic acid or behenic acid.

Alk (en) yl sulfates are the alkali metal and especially sodium, salts of the C ₁₂ -C Schwefelsäurehalbester _B fatty alcohols, for example coconut fatty alcohol, tallow fatty alcohol, lauryl, styl- myristic, cetyl or stearyl alcohol, or C ₁₀ -C ₂ o-oxo alcohols and those half-esters of secondary alcohols of these chain lengths are preferred. Also preferred are alk (en) ylsulfates of said chain length, which contain a synthetic, produced on a petrochemical basis straight-chain alkyl radical, which have an analogous degradation behavior as the adequate compounds based on oleochemical raw materials. From a washing-technical point of view, preference is given to the C ₁₂ -C ₁₆ -alkyl sulfates and C ₁₂ -C ₁ -salkyl sulfates and also C ₄ -C ₁₅ -alkyl sulfates. In addition, 2,3-alkyl sulfates, which are produced for example in accordance with US Patent No. 3,234,258 or 5,075,041 and which are commercially obtainable as products of the Shell Oil Company under the name DAN ^®, are suitable anionic surfactants.

Also, the sulfuric acid monoesters of straight-chain or branched C ₇ ethoxylated with 1 to 6 moles of ethylene oxide. ₂₁ -alcohols, such as 2-methyl-branched Cg-n-alcohols having on average 3.5 moles of ethylene oxide (EO) or C _12-18 -fatty alcohols having 1 to 4 EO, are suitable. Due to their high foaming behavior, they are preferably used in detergents only in relatively small amounts, for example in amounts of from 1 to 5% by weight.

Further suitable anionic surfactants are also the salts of alkylsulfosuccinic acid, which are also referred to as sulfosuccinates or as sulfosuccinic esters and which are monoesters and / or diesters of sulfosuccinic acid with alcohols, preferably fatty alcohols and in particular ethoxylated fatty alcohols. Preferred sulfosuccinates contain C ₈ -i ₈ -fatty alcohol residues or mixtures of these. Particularly preferred sulfosuccinates contain a fatty alcohol residue derived from ethoxylated fatty alcohols, which in themselves constitute nonionic surfactants (see description below). Sulfosuccinates, whose fatty alcohol residues are derived from ethoxylated fatty alcohols with a narrow homolog distribution, are again particularly preferred. Likewise, it is also possible to use alk (en) yl-succinic acid having preferably 8 to 18 carbon atoms in the alk (en) yl chain or salts thereof. Particularly preferred anionic surfactants are soaps. Suitable are saturated and unsaturated fatty acid soaps, such as the salts of lauric acid, myristic acid, palmitic acid, stearic acid, (hydrogenated) erucic acid and behenic acid and, in particular, soap mixtures derived from natural fatty acids, for example coconut, palm kernel, olive oil or tallow fatty acids.

The anionic surfactants, including the soaps, may be 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, in particular in the form of the sodium salts.

The content of preferred liquid detergents and cleaners to anionic surfactants is 2 to 30 wt .-%, preferably 4 to 25 wt .-% and in particular 5 to 22 wt .-%, each based on the total agent.

In addition to the solids, preferred liquid detergents and cleaners may contain further ingredients which further improve the performance and / or aesthetic properties of the liquid detergent and cleaning agent. In the context of the present invention, preferred agents furthermore comprise one or more substances from the group of builders, bleaches, bleach activators, enzymes, electrolytes, nonaqueous solvents, pH adjusters, fragrances, perfume carriers, fluorescers, dyes, hydrotopes, foam inhibitors, silicone oils, antiredeposition agents , optical brighteners, grayness inhibitors, anti-shrinkage agents, anti-crease agents, color transfer inhibitors, antimicrobial agents, germicides, fungicides, antioxidants, corrosion inhibitors, antistatic agents, ironing aids, repellents and impregnating agents, swelling and anti-slip agents and UV absorbers.

Suitable builders which may be present in the liquid detergents and cleaners are, in particular, silicates, aluminum silicates (in particular zeolites), carbonates, salts of organic di- and polycarboxylic acids and mixtures of these substances.

Suitable crystalline, layered sodium silicates have the general formula NaMSi _x O _{2x + I} H ₂ O, where M is sodium or hydrogen, x is a number from 1, 9 to 4 and y is a number from 0 to 20 and preferred values for x 2 , 3 or 4 are. Such crystalline sheet silicates are described, for example, in European Patent Application EP-AO 164 514. Preferred crystalline layered silicates of the formula given are those in which M is sodium and x assumes the values 2 or 3. In particular, both β- and δ-sodium disilicates

Na ₂ Si ₂ O ₅ -yH ₂ θ is preferred, wherein β-sodium disilicate can be obtained, for example, by the method described in International Patent Application WO-A-91/08171. It is also possible to use amorphous sodium silicates with a Na ₂ O: SiO ₂ modulus of from 1: 2 to 1: 3.3, preferably from 1: 2 to 1: 2.8 and in particular from 1: 2 to 1: 2.6, which Delayed and have secondary washing properties. The dissolution delay compared with conventional amorphous sodium silicates may have been caused in various ways, for example by surface treatment, compounding, compaction / densification or by overdrying. In the context of this invention, the term "amorphous" is also understood to mean "X-ray amorphous". This means that the silicates do not yield sharp X-ray reflections typical of crystalline substances in X-ray diffraction experiments, but at most one or more maxima of the scattered X-rays which have a width of several degrees of diffraction angle. However, it may even lead to particularly good buil- ding properties if the silicate particles produce fuzzy or even sharp diffraction maxima in electron diffraction experiments. This is to be interpreted as meaning that the products have microcrystalline regions of size 10 to a few hundred nm, with values of up to a maximum of 50 nm and in particular up to a maximum of 20 nm being preferred. Such so-called X-ray-amorphous silicates, which likewise have a dissolution delay compared to the conventional water glasses, are described, for example, in German patent application DE-A-44 00 024. Particularly preferred are compacted / compacted amorphous silicates, compounded amorphous silicates and overdried X-ray amorphous silicates.

The finely crystalline, synthetic and bound water-containing zeolite used is preferably zeolite A and / or P. As zeolite P, zeolite MAP® (commercial product from Crosfield) is particularly preferred. Also suitable, however, are zeolite X and mixtures of A, X and / or P. Commercially available and preferably usable in the context of the present invention is, for example, a cocrystal of zeolite X and zeolite A (about 80% by weight of zeolite X) which is sold by SASOL under the brand name VEGOBOND AX ^® and by the formula Na ₂ O. '(1-n) K ₂ ^O' AI ₂ O ₃ '(2 to 2.5) SiO _^2), (3, 5 - 5.5) H ₂ O n = 0.90 - 1, 0 can be described. The zeolite can be used as a spray-dried powder or else as an undried, stabilized suspension which is still moist from its production. In the event that the zeolite is used as a suspension, it may contain minor additions of nonionic surfactants as stabilizers, for example 1 to 3 wt .-%, based on zeolite, of ethoxylated C ₁₂ -C ₁₈ fatty alcohols having 2 to 5 ethylene oxide groups , C ₁₂ -C ₁₄ fatty alcohols having 4 to 5 ethylene oxide groups or ethoxylated isotridecanols. Suitable zeolites have an average particle size of less than 10 μm (volume distribution, measuring method: Coulter Counter) and preferably contain 18 to 22% by weight, in particular 20 to 22% by weight, of bound water. Of course, a use of the well-known phosphates as builders is possible, unless such use should not be avoided for environmental reasons. Particularly suitable are the sodium salts of orthophosphates, pyrophosphates and in particular tripolyphosphates.

Among the compounds which serve as bleaches and deliver H ₂ O ₂ in water, the sodium perborate tetrahydrate and the sodium perborate monohydrate are of particular importance. Further usable bleaching agents are, for example, sodium percarbonate, peroxypyrophosphates, citrate perhydrates and H ₂ O ₂ -producing peracidic salts or peracids, such as perbenzoates, peroxophthalates, diperazelaic acid, phthaloiminoperacid or diperdodecanedioic acid.

In order to achieve an improved bleaching effect during washing at temperatures of 60 ° C. and below, bleach activators can be incorporated into the detergents and cleaners to be produced according to the invention. As bleach activators, it is possible to use compounds which, under perhydrolysis conditions, give aliphatic peroxycarboxylic acids having preferably 1 to 10 C atoms, in particular 2 to 4 C atoms, and / or optionally substituted perbenzoic acid. Suitable substances are those which carry O- and / or N-acyl groups of the stated C atom number and / or optionally substituted benzoyl groups. Preference is given to polyallylated alkylenediamines, in particular tetraacetylethylenediamine (TAED), acylated triazine derivatives, in particular i-.delta.-diacetylM-dioxohexahydro-1'δ-triazine (DADHT), acylated glycolurils, in particular tetraacetylglycoluril (TAGU), N-acylimides, especially N-acylimides. Nonanoylsuccinimide (NOSI), acylated phenolsulfonates, in particular n-nonanoyl or lsononanoyloxybenzolsulfonat (n- or iso-NOBS), carboxylic anhydrides, especially phthalic anhydride, acylated polyhydric alcohols, especially triacetin, ethylene glycol diacetate and 2,5-diacetoxy-2,5-dihydrofuran ,

In addition to or in place of the conventional bleach activators, so-called bleach catalysts can also be incorporated into the liquid detergents and cleaners. These substances are bleach-enhancing transition metal salts or transition metal complexes such as Mn, Fe, Co, Ru or Mo-salen complexes or carbonyl complexes. Mn, Fe, Co, Ru, Mo, Ti, V and Cu complexes with nitrogen-containing tripod ligands and Co, Fe, Cu and Ru ammine complexes can also be used as bleach catalysts.

The liquid washing and cleaning agent to be produced according to the invention preferably contains at least one thickener.

Preferred liquid detergents and cleaners may contain enzymes in encapsulated form and / or directly in the detergent composition. Suitable enzymes are, in particular, those from the classes of the hydrolases, such as the proteases, esterases, lipases or polymetallic enzymes, amylases, cellulases or other glycosyl hydrolases and mixtures the enzymes mentioned in question. All of these hydrolases in the wash contribute to the removal of stains such as proteinaceous, greasy or starchy stains and graying. In addition, cellulases and other glycosyl hydrolases can contribute to color retention and to increasing the softness of the textile by removing pilling and microfibrils. Oxireductases can also be used for bleaching or inhibiting color transfer. Particularly suitable are enzymatic agents obtained from bacterial strains or fungi such as Bacillus subtilis, Bacillus lichenifor- mis, Streptomyceus griseus and Humicola insolens. Preferably, subtilisin-type proteases and in particular proteases derived from Bacillus lentus are used. Enzyme mixtures are, for example, from protease and amylase or protease and lipase or lipolytic enzymes or protease and cellulase or from cellulase and lipase or lipolytic enzymes or from protease, amylase and lipase or lipolytic enzymes or protease, lipase or lipolytic enzymes and cellulase, but in particular protease and / or lipase-containing mixtures or mixtures with lipolytic enzymes of particular interest. Examples of such lipolytic enzymes are the known cutinases. Peroxidases or oxidases have also proved to be suitable in some cases. Suitable amylases include in particular α-amylases, iso-amylases, pullulanases and pectinases. As cellulases are preferably cellobiohydrolases, endoglucanases and ß-glucosidases, which are also called cellobiases, or mixtures thereof used. Since different cellulase types differ by their CMCase and avicelase activities, the desired activities can be set by targeted mixtures of the cellulases.

The enzymes may be adsorbed to carriers to protect against premature degradation. The proportion of enzymes, enzyme mixtures or enzyme granules directly in the detergent composition can be, for example, about 0.1 to 5% by weight, preferably 0.12 to about 2.5% by weight.

As electrolyte ^ from the group of inorganic salts, a wide number of different salts can be used. Preferred cations are the alkali and alkaline earth metals, preferred anions are the halides and sulfates. From a production point of view, the use of NaCl or MgCl ₂ in the compositions is preferred. The proportion of electrolytes in the agents is preferably 0.5 to 5 wt .-%.

Non-aqueous solvents which can be used in the liquid preparations to be prepared according to the invention and in particular in detergents and cleaners are derived, for example, from the group of monohydric or polyhydric alcohols, alkanolamines or glycol ethers, provided they are miscible with water in the stated concentration range. The solvents are preferably selected from ethanol, n- or i-propanol, butanols, glycol, propane or butanediol, glycerol, diglycol, propyl or butyl diglycol, hexylene glycol, ethylene glycol methyl ether, ethylene glycol ethyl ether, ethylene glycol propyl ether, ethylene glycol mono-n-butyl ether, diethylene glycol methyl ether, diethylene glycol ethyl ether, propylene glycol methyl, -ethyl or -propyl ether, dipropylene glycol monomethyl ether. or -ethyl ether, di-isopropylene glycol monomethyl or ethyl ether, methoxy, ethoxy or Butoxytriglykol, 1-butoxyethoxy-2-propanol, 3-methyl-3-methoxybutanol, propylene glycol t-butyl ether and mixtures of these solvents. Non-aqueous solvents may be used in the liquid preparations, for example in amounts of between 0.5 and 15 wt .-%, but preferably below 12 wt .-% and in particular below 9 wt .-%. However, according to another preferred embodiment more than 15 wt .-%, preferably more than 20 wt .-%, in particular more than 25 wt .-% of non-aqueous solvent.

In order to bring the pH of the liquid preparations and in particular the liquid detergents and cleaning agents in the desired range, the use of pH adjusting agents may be indicated. Can be used here are all known acids or alkalis, unless their use is not for technical application or environmental reasons or for reasons of consumer protection prohibited. Usually, the amount of these adjusting agents does not exceed 7% by weight of the total formulation.

In order to improve the aesthetic impression of the liquid preparations and in particular the liquid detergents and cleaners, they can be colored with suitable dyes. Preferred dyes, the selection of which presents no difficulty to the skilled person, have a high storage stability and insensitivity to the other ingredients of the agents and to light and no pronounced substantivity to textile fibers so as not to stain them.

Suitable foam inhibitors which can be used in the liquid preparations and in particular in the liquid detergents and cleaners are, for example, soaps, paraffins or silicone oils, which may optionally be applied to support materials. Suitable antiredeposition agents, which are also referred to as "soil repellents", are, for example, nonionic cellulose ethers such as methylcellulose and methylhydroxypropylcellulose with a proportion of methoxy groups of 15 to 30% by weight and of hydroxypropyl groups of 1 to 15% by weight, based in each case on nonionic cellulose ethers and the polymers of phthalic acid and / or terephthalic acid known from the prior art or of derivatives thereof, in particular polymers of ethylene terephthalates and / or polyethylene glycol terephthalates or anionically and / or nonionically modified derivatives thereof, particularly preferred of these are the sulphonated derivatives the phthalic and terephthalic acid polymers. Optical brighteners (so-called "whiteners") may be added to the liquid detergents and cleaners to remove graying and yellowing of the treated textile fabrics which will attract the fiber and cause lightening and fake bleaching by exposing invisible ultraviolet radiation to visible The ultraviolet light absorbed from the sunlight is emitted as a faint bluish fluorescence and gives pure white with the yellow color of the grayed or yellowed wash 'stilbene disulphonic acids (flavonic acids), 4,4'-distyrylbiphenyls, methyl umbeliferones, coumarins, dihydroquinolinones, 1,3-diarylpyrazolines, naphthalsimides, benzoxazole, benzisoxazole and benzimidazole systems, and the heterocyclic substituted pyrene derivatives. The optical brighteners are preferred in amounts between 0.03 and 0.3 wt .-%, based on the finished composition used.

Grayness inhibitors have the task of keeping the dirt detached from the fiber suspended in the liquor and thus preventing the dirt from being rebuilt. Water-soluble colloids of mostly organic nature are suitable for this purpose, for example glue, gelatine, salts of ether sulfonic acids or cellulose or salts of acidic sulfuric acid esters of cellulose or starch. Also, water-soluble polyamides containing acidic groups are suitable for this purpose. It is also possible to use soluble starch preparations and starch products other than those mentioned above, for example degraded starch, aldehyde starches, etc. Polyvinylpyrrolidone is also useful. However, preference is given to cellulose ethers such as carboxymethylcellulose (Na salt), methylcellulose, hydroxyalkylcellulose and mixed ethers such as methylhydroxyethylcellulose, methylhydroxypropylcellulose, methylcarboxymethylcellulose and mixtures thereof in amounts of preferably 0.1 to 5% by weight, based on the compositions used.

Since fabrics, particularly rayon, rayon, cotton and blends thereof, can tend to wrinkle because the individual fibers are susceptible to flexing, buckling, squeezing and squeezing across the grain, the compositions may contain synthetic crease inhibitors. These include, for example, synthetic products based on fatty acids, fatty acid esters, fatty acid amides, alkylol esters, -alkylolamides or fatty alcohols, which are usually reacted with ethylene oxide, or products based on lecithin or modified phosphoric acid ester.

To combat microorganisms, the liquid detergents and cleaning agents may contain antimicrobial agents. Depending on the antimicrobial spectrum and mechanism of action, a distinction is made between bacteriostatic agents and bactericides, fungistatics and fungicides, etc. Important substances from these groups are, for example, benzalkonium chlorides, alkylarylsulfur fonates, halophenols and Phenolmercuriacetat, which can be completely dispensed with the compounds according to the invention in these compounds.

To prevent undesirable changes to the liquid detergents and cleaners and / or the treated fabrics caused by oxygen and other oxidative processes, the agents may contain antioxidants. This class of compounds includes, for example, substituted phenols, hydroquinones, catechols and aromatic amines, as well as organic sulfides, polysulfides, dithiocarbamates, phosphites and phosphonates.

Increased comfort may result from the additional use of antistatic agents added to the compositions. Antistatic agents increase the surface conductivity and thus allow an improved drainage of formed charges. External antistatic agents are generally substances with at least one hydrophilic molecule ligand and give a more or less hygroscopic film on the surfaces. These mostly surface-active antistatic agents can be subdivided into nitrogen-containing (amines, amides, quaternary ammonium compounds), phosphorus-containing (phosphoric acid esters) and sulfur-containing (alkyl sulfonates, alkyl sulfates) antistatic agents. External antistatics are described, for example, in patent applications FR 1, 156,513, GB 873,214 and GB 839,407. The lauryl (or stearyl) -dimethylbenzylammonium chlorides disclosed herein are useful as antistatics for textile fabrics or as an additive to laundry detergents, with a softening effect being additionally achieved.

To improve the water absorption capacity, the rewettability of the treated fabrics and to facilitate the Bügeins the treated fabrics can be used in the liquid detergents and cleaners, for example, silicone derivatives. These additionally improve the rinsing behavior of the agents by their foam-inhibiting properties. Preferred silicone derivatives are, for example, polydialkyl or alkylaryl siloxanes in which the alkyl groups have one to five carbon atoms and are completely or partially fluorinated. Preferred silicones are polydimethylsiloxanes, which may optionally be derivatized and are then amino-functional or quaternized or have Si-OH, Si-H and / or Si-Cl bonds. The viscosities of the preferred silicones are in the range between 100 and 100,000 mPas at 25 ° C, wherein the silicones in amounts between 0.2 and 5 wt .-%, based on the total agent can be used.

Finally, the liquid detergents and cleaners may also contain UV absorbers that wick onto the treated fabrics and improve the lightfastness of the fibers. Compounds having these desired properties include, for example, the non-radiative deactivating compounds and derivatives of benzophenone having substituents in the 2- and / or 4-position. Furthermore, substituted benzotriazoles, in 3- Position phenyl-substituted acrylates (cinnamic acid derivatives), optionally with cyano groups in the 2-position, salicylates, organic Ni complexes and natural products such as umbelliferone and the body's urocanic acid suitable.

In order to avoid the catalyzed by heavy metals decomposition of certain detergent ingredients, substances that complex heavy metals can be used. Suitable heavy metal complexing agents are, for example, the alkali metal salts of ethylenediaminetetraacetic acid (EDTA) or nitrilotriacetic acid (NTA) and alkali metal salts of anionic polyelectrolytes such as polymaleates and polysulfonates.

A preferred class of complexing agents are the phosphonates, which in preferred liquid detergents and cleaners in amounts of 0.01 to 2.5 wt .-%, preferably 0.02 to 2% by weight and in particular from 0.03 to 1 , 5 wt .-% are included. These preferred compounds include in particular organophosphonates such as 1-hydroxyethane-1, 1-diphosphonic acid (HEDP), amihotri (methylenephosphonic acid) (ATMP), diethylenetriamine penta (methylene phosphonic acid) (DTPMP or DETPMP) and 2-phosphonobutane -1, 2,4-tricarboxylic acid (PBS-AM), which are mostly used in the form of their ammonium or alkali metal salts.

The resulting aqueous liquid preparations, in particular washing and cleaning agents, are preferably clear, ie they have no sediment and are particularly preferably transparent or at least translucent.

The detergents and cleaning agents according to the invention can be used in particular for cleaning textile surface fabrics.

According to a preferred embodiment, the liquid agent to be produced according to the invention is a textile treatment agent, an ironing aid, a detergent, a cleaning agent, in particular for hard and / or soft surfaces, a household cleaner, a care agent, a laundry care product, a laundry care product, a room fragrancing agent, an air freshener, a conditioning agent, a coloring agent, a fabric softener, a pharmaceutical, a pesticide, a cleaning agent, a food, a cosmetic, a fertilizer, a building material, an adhesive, a bleach, a descaling agent, a car care product, floor care products, stoves, Leather care products, furniture care products, a scrubbing agent, a disinfectant, a fragrancing agent, a mold remover and / or a precursor of the aforementioned agents. Such agents to be prepared according to the invention represent a preferred embodiment of the invention, in particular as a gel. In the following, certain agents are listed, which are very preferred in the context of the present invention.

Among the preferred, according to the invention to be produced liquid cleaning agents include u.a. the toilet cleaner or toilet cleaner, ie products for cleaning toilet bowls and urinals, which liquids, preferably gels, offered. Among other common ingredients such as surfactants, they preferably contain organic acids (e.g., citric acid and / or lactic acid) or sodium hydrogen sulfate, amidosulfuric acid, or phosphoric acid to remove limescale or so-called primal stones. Such agents to be prepared according to the invention represent a preferred embodiment of the invention, in particular as a gel.

The preferred liquid detergents to be produced according to the invention include, inter alia, the pipe cleaners or drain cleaners. These are preferably strong alkaline preparations, which are usually the elimination of pipe blockages of organic materials - such as hair, fat, food residues, soap deposits, etc.- serve. To form H ₂ -GaS with a bubble effect, additives of Al or Zn powder may preferably be used. Possible ingredients are preferably alkalis, alkaline salts, oxidizing agents and neutral salts. In particular, hypochlorite may be included. In addition, there are also drain cleaner on Enzymbasis. Acid preparations are also preferred. Such agents to be prepared according to the invention represent a preferred embodiment of the invention, in particular as a gel.

Among the preferred, according to the invention to be produced liquid detergents include u. a. also the universal or all-purpose cleaner or all-purpose cleaner. These are universally applicable cleaners for all hard surfaces in household and commercial, which are wet or damp wipeable. As a rule, these are neutral or weakly alkaline or weakly acidic products. All-purpose cleaners or all-purpose cleaners preferably comprise surfactants, builders, solvents and hydrotropes, dyes, preservatives, etc. Such agents to be prepared according to the invention represent a preferred embodiment of the invention, in particular as a gel.

There are also special disinfecting all-purpose cleaners. These preferably additionally contain antimicrobial agents (for example aldehydes, alcohols, quaternary ammonium compounds, amphosurfactants, triclosan). Such agents to be prepared according to the invention represent a preferred embodiment of the invention, in particular as a gel.

The preferred liquid detergents to be produced according to the invention include, among others, sanitary cleaners. These are liquid products for cleaning in the bathroom and toilet. The alkaline sanitary cleaners are preferably used to remove grease, while the acidic sanitary cleaners are used primarily for the removal of limescale. Sanitary cleaners advantageously also have a significant disinfectant Effect, in particular the strongly alkaline, chlorine-containing sanitary cleaner. Such agents to be prepared according to the invention represent a preferred embodiment of the invention, in particular as a gel.

Among the preferred, according to the invention to be produced liquid cleaning agents include u.a. also the oven cleaner or grill cleaner, which are advantageously offered in the form of gels. These are usually used to remove burnt or charred food particles. Preferably, oven cleaners are e.g. strongly alkaline with sodium hydroxide, sodium metasilicate, 2-aminoethanol. Preferably, they also contain anionic and / or nonionic surfactants, water-soluble solvents and in part thickeners such as polycarboxylates, carboxymethylcellulose. Such agents to be prepared according to the invention represent a preferred embodiment of the invention, in particular as a gel.

Among the preferred, according to the invention to be produced liquid cleaning agents include u.a. also the metal cleaner. These are liquid cleaners for certain types of metals such as stainless steel or silver. Stainless steel cleaners preferably contain not only acids (preferably up to 3% by weight, eg citric acid, lactic acid), surfactants (in particular up to 5% by weight, preferably nonionic and / or anionic surfactants), water also solvents (preferably up to 15% by weight). %) to eliminate greasy soiling and other substances such as Thickener and preservative. Very fine polishing bodies are also contained in products for preferably glossy stainless steel surfaces. Silver cleaning agents, in turn, are preferably acidified. In particular, they preferably contain complexing agents (e.g., thiourea, sodium thiosulfate) to remove black deposits of silver sulfide. Typical offer forms are cleaning cloths, dip baths, pastes, liquids. To remove dark discolorations (oxide layers), copper and non-ferrous metal cleaners (for example for brass and bronze) are used. These are usually adjusted to weakly alkaline (preferably with ammonia) and usually contain polishing agents and preferably also ammonium soaps and / or complexing agents. Such agents to be prepared according to the invention represent a preferred embodiment of the invention, in particular as a gel.

The preferred liquid detergents to be produced according to the invention include, among others, the glass cleaners or window cleaners. These liquid preparations are preferably used to eliminate especially greasy soil from glass surfaces. They preferably contain substances such as anionic and / or nonionic surfactants (in particular up to 5% by weight), ammonia and / or ethanolamine (in particular up to 1% by weight), ethanol and / or 2-propanol, glycol ethers (in particular 10 -30% by weight), water, preferably preservatives, dyes, anti-fogging agents, etc. Such agents to be prepared according to the invention represent a preferred embodiment of the invention, in particular as a gel. The preferred liquid detergents to be produced according to the invention include, inter alia, also all special cleaners, for example those for cooktops made of glass ceramic, as well as carpet cleaners and stain removers. Such agents to be prepared according to the invention represent a preferred embodiment of the invention, in particular as a gel.

Among the preferred, according to the invention to be produced liquid car care products include u.a. Paint preservatives, paint polishes, paint cleaners, Waschkonservierer, shampoos for car wash, car wash and wax products, polishes for decorative metals, protective films for decorative metals, plastic cleaner, tar remover, window cleaner, engine cleaner, etc. Such means according to the invention constitute a preferred embodiment of the invention, in particular Gel.

Preferred liquid cosmetic products to be prepared according to the invention are preferably (a) cosmetic liquid skin care preparations, in particular bath preparations, skin cleansing and cleansing preparations, skin care products, ocular cosmetics, lip care products, nail care products, intimate care products, foot care products, (b) cosmetic liquid agents having a specific action , in particular light stabilizers, skin tanning agents, depigmenting agents, deodorants, antihidrotic agents, depilatories, shaving agents, fragrances, (c) cosmetic liquid agents for dental care, in particular dental and. Oral care products, dentifrices, denture cleansing preparations, dentifrice adhesives, (d) cosmetic liquid hair care preparations, in particular shampoos, hair care preparations, hair hardening preparations, hair shaping preparations, hair dyes. Such agents to be prepared according to the invention represent a preferred embodiment of the invention, in particular as a gel or as other customary cosmetic dosage forms such as lotions, creams, milk, emulsions, etc.

Also particularly preferred are the liquid air improvers and room fragrancing agents. Such products preferably contain volatile and usually pleasant-smelling substances, which can advantageously cover even in very small amounts of bad odors. Air fresheners for living spaces contain, in particular, natural and / or synthetic essential oils, such as, for example, royal needle oil, citrus oil, eucalyptus oil, lavender oil, for example in amounts of up to 50% by weight. As aerosols they contain rather lower amounts of such essential oils, for example less than 5 wt .-% or less than 2 wt .-%, but preferably also substances such as acetaldehyde (in particular <0.5 wt .-%), preferably isopropyl alcohol (in particular <5 wt .-%), mineral oil (in particular <5 wt .-%) and propellant gases. Preferably, gel concentrates of essential oils can be used. Examples

Example 1 :

(Preparation of a liquid detergent)

By mixing water with surfactants (anionic surfactant, nonionic surfactant, soap), small particles (defoamers, perfume) and thickening agents (for example polyacrylates), a liquid detergent with defined viscosity and flow limit (viscosity 4200 mPas, flow limit 1, 2 Pa) was produced. The preparation was carried out batchwise at a mixing time of 1, 5 h / batch.

Speckles were already added during the preparation of the liquid detergent. It could be observed that the speckles were torn after a short time. Even if the speckles were added only at the very end of the production, still a good part (about 25 wt .-% of the speckles) was already during the mixing and a large part (about 60 wt .-% of the speckies) during the emptying and during transport through various parts of the plant (pipes, valves, pumps, intermediate container) up to the filling torn.

The resulting product made a visually inferior and unprofessional impression.

Example 2:

(Batch incorporation of a Speckies dispersion)

A 20 l stirred glass container (container diameter: 300 mm / container height: 400 mm with Intermig

Stirrer Stirrer diameter (3 AFS): 210 mm and 4 baffles) was filled to 50% by volume with a conventional liquid detergent (viscosity 4300 mPas with a flow limit of 1.3 Pa), which had been previously prepared. Subsequently, at a stirrer speed of 55 rpm

250g of a Speckies dispersion added (200g of Speckies in 800g of water). Already after 3 min, all the speckles were homogeneously incorporated in the liquid detergent and could be bottled directly. A destruction of the speckies could not be observed.

Example 3:

(Continuous incorporation of a Speckies dispersion)

The mixture aμs example 2 was used as a template. Into this original were continuously metered 117 kg / h of ordinary liquid detergent and 3 kg / h of the speckies dispersion while continuously removing 200 kg / h of the mixture from the bottom outlet valve. Even after 25 minutes of continuous driving, all the speckles were still homogeneously incorporated in the liquid detergent and could be bottled directly. There were no fluctuations in the product. A destruction of the speckies could not be observed.

Claims

claims

1. A process for the preparation of a liquid preparation with a solids content, characterized in that the addition of at least a portion of the solids only

(a) in the last process step preceding the filling of the liquid preparation into a packing unit, or

(b) when filling into a packing unit.

2. The method according to claim 1, characterized in that it is the liquid preparation is a liquid detergent and cleaning agent, a food preparation, a coating, dye or lacquer preparation, an adhesive preparation, a pharmaceutical preparation and / or a cosmetic preparation ,

3. A method according to any one of claims 1 or 2, characterized in that the solids content in the range of 0.01 to 80 wt .-%, with the percentages by .-% based on the entire ^'te preparation refers:

4. The method according to any one of claims 1 to 3, characterized in that the solids are added by means of a carrier liquid, preferably in suspended form to the liquid preparation.

5. The method according to any one of claims 1 to 3, characterized in that the solids are added directly into the liquid preparation, preferably by trickling or pouring.

6. The method according to any one of claims 1 to 5, characterized in that the solids are spatially stable in the liquid preparation with uniform spatial distribution, in particular floating in this.

7. The method according to any one of claims 1 to 6, characterized in that the solids to be added are shear sensitive.

8. The method according to any one of claims 1 to 7, characterized in that the addition of the solid in the preparation and the mixing with this takes place under conditions of low shear.

9. The method according to any one of claims 1 to 8, characterized in that the preparation, after the solids have been added, is supplied to the filling under conditions of low shear.

10. The method according to any one of claims 1 to 9, characterized in that the flow behavior of the liquid preparation after addition of the solid in the then to be flown through piping systems with Reynolds numbers up to 10,000.

11. The method according to any one of claims 1 to 10, characterized in that the flow behavior of the liquid preparation after addition of the solid in the then to be flown through piping systems with friction numbers up to 0.03.

12. The method according to any one of claims 1 to 11, characterized in that the coefficients of the individual resistances of all components for the piping system after addition of the solids each per individual resistance in the range 0 to 20 are.

13. The method according to any one of claims 1 to 12, wherein the preparation is an aqueous medium.

14. The method according to any one of claims 1 to 13, characterized in that the solids have a diameter along their largest dimension of 0.01 to 20,000 microns.

15. The method according to any one of claims 1 to 14, characterized in that it is the solids to capsules, microcapsules or speckles. ■

16. The method according to any one of claims 1 to 15, characterized in that the solids contain hollow microspheres (s).

17. The method according to any one of claims 1 to 16, characterized in that the addition of at least a portion of the solids takes place only when the other components of the composition have already undergone a mixing process.

18. The method according to any one of claims 1 to 17, characterized in that the combination of the otherwise ready-to-use preparations is carried out with the solids to be added in a CST reactor.

19. The method according to any one of claims 1 to 18, characterized in that the preparation has a viscosity in the range of 1 to 10,000 mPa s.

20. The method according to any one of claims 1 to 19, characterized in that the solids have substantially an average form factor of at least 0.77.

21. Liquid preparation which is obtainable by one of the preceding processes, characterized in that it contains at least one surfactant.