EP3317391B1 - Procédé de préparation d'une composition liquide contenant un tensioactif - Google Patents

Procédé de préparation d'une composition liquide contenant un tensioactif Download PDF

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EP3317391B1
EP3317391B1 EP16729927.0A EP16729927A EP3317391B1 EP 3317391 B1 EP3317391 B1 EP 3317391B1 EP 16729927 A EP16729927 A EP 16729927A EP 3317391 B1 EP3317391 B1 EP 3317391B1
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Prior art keywords
mixture
composition
batch process
batch
oder
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German (de)
English (en)
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EP3317391A1 (fr
Inventor
Luca Bellomi
Frank Meier
Sheila Edwards
Matthias Sunder
Gerd Bösemann
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Henkel AG and Co KGaA
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Henkel AG and Co KGaA
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Priority to PL16729927T priority Critical patent/PL3317391T3/pl
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    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C11D11/0094—Process for making liquid detergent compositions, e.g. slurries, pastes or gels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/50—Mixing liquids with solids
    • B01F23/51—Methods thereof
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C11D11/04—Special methods for preparing compositions containing mixtures of detergents by chemical means, e.g. by sulfonating in the presence of other compounding ingredients followed by neutralising
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0008—Detergent materials or soaps characterised by their shape or physical properties aqueous liquid non soap compositions
    • C11D17/0013—Liquid compositions with insoluble particles in suspension

Definitions

  • the present invention relates to a method for producing a liquid composition comprising surfactants and the compositions obtained therefrom.
  • Liquid, surfactant-containing compositions have become an integral part of everyday life.
  • these are personal care products, such as shampoos, shower gels or bubble baths.
  • detergents or cleaning agents such as household cleaners, fabric softeners, laundry detergents, floor care products, all-purpose cleaners, manual dishwashing detergents, machine dishwashing detergents or heavy-duty detergents are also included.
  • the batch process is a discontinuous production process.
  • certain quantities of feed materials are conveyed into a container according to a predetermined recipe and mixed there.
  • a reaction vessel In a typical batch process or batch process, a reaction vessel is first completely filled with the starting materials, i.e. the starting materials. The reaction of the educts with one another to the end product takes place within the reaction vessel. When the reaction that may have taken place is completed, the reaction vessel is completely emptied and the desired formulation is filled into suitable containers for sale or, if appropriate, for storage. The reaction vessel must then be prepared for the next filling. This means thorough cleaning of the reaction vessel and, if necessary, the lines through which the starting products are introduced into the reaction vessel, as well as the implementation of upcoming maintenance work.
  • Such a batch process has the advantage that the formulation of the recipe can still be adapted in the reaction vessel if necessary. Readjustments of individual components are possible here. In terms of quality, it must be taken into account that there is the possibility of batch tracing.
  • reaction vessel is always completely filled; that is, large quantities of a product are always manufactured. Once a batch (or batch) has been manufactured, it must first be processed before another batch can be started. If direct processing or filling is not possible, An already manufactured product must be stored outside the reaction vessel. This again leads to a high space requirement and additional costs.
  • Another disadvantage of the batch process is that it contains different components that are stable at different temperatures. If, for example, enzymes are contained, a temperature of 40 ° C cannot be exceeded, otherwise they will degrade.
  • a batch can only be stirred with a certain shear force. However, different shear forces are required for different components in order to distribute them homogeneously.
  • a closed system would also be advantageous for certain solvents that are volatile.
  • open reaction vessels are usually used in the batch process. If the mixture contained in it is heated, volatile constituents can escape and thus get into the environment, which can result in a hazard.
  • certain balances in the batch can undesirably shift. Depending on the escape of the solvent, certain components may fail or equilibrium between products may shift. Since in the open system the escape depends on the external conditions, an undesirable variation in the batch product qualities arises.
  • continuous processes for producing liquid, surfactant-containing compositions are also known. Continuous processes offer better opportunities for just-in-time production. However, complex control of the individual process steps is necessary here.
  • mixing by means of static or dynamic mixing devices does not take place in a reaction vessel as in the batch process. Rather, the mixing takes place within a line.
  • the individual ingredients of a recipe are dosed into this line in a predefined sequence. Bottling takes place immediately at the end of this line. It is not possible to add or change the concentration of individual components here.
  • a targeted and controlled monitoring of the addition of each individual component is necessary.
  • the addition of solid components may be necessary. However, these can only be added in a batch process. The addition of solid components in a continuous process is not possible. Only liquid components can be dosed in continuous processes.
  • liquid detergents and cleaning agents that work optimally even after storage and transport at the time of use.
  • the ingredients of the liquid laundry detergent and cleaning agent have neither settled or decomposed nor volatilized.
  • One concept for incorporating sensitive, chemically or physically incompatible and volatile components is the use of particles and in particular microcapsules, in which these ingredients are enclosed in a storage and transport-stable manner.
  • German patent application DE 10 2012 221 360 A1 (Henkel) describes in a continuous process for the production of liquid washing or cleaning agents.
  • German patent application DE 10 2005 018 243 A1 (Henkel) discloses a method for producing a liquid preparation with a solid content.
  • the U.S. patent application US 2001/0031718 A1 (Unilever) describes a continuous process of a liquid detergent based on anionic surfactants.
  • a substance such as a composition or mixture, is liquid according to the definition of the invention if it is in the liquid state at 25 ° C. and 1013 mbar.
  • a substance is solid or solid when it is in the solid state at 25 ° C. and 1013 mbar.
  • pairs of surfactant / surfactants, phosphonate / phosphonates, anionic surfactant / anionic surfactants, nonionic surfactant / nonionic surfactants and similar terms are intended to have the same meaning and to cover both the singular and the plural.
  • the mixture produced in the batch process comprises at least one solvent and preferably at least one active substance.
  • An active substance in the sense of the present invention is a substance that has a specific task in the final composition. For example, this can be at least one surfactant and / or at least one salt.
  • the composition thus comprises at least one solvent, at least one active substance and optionally further components. These further components are constituents which are added in a continuous process, in particular for reasons of optics appealing to the consumer.
  • the method according to the invention further enables the mixture produced to be stored first and to be processed further only after storage in a continuous process.
  • the further processing in a continuous process can, however, also take place immediately after the preparation of the mixture in a batch process, which is preferred according to the invention.
  • the proportion of all constituents of the mixture produced in the batch process is 1% by volume to 99% by volume, preferably 5% by volume to 95% by volume, in particular 20% by volume to 90% by volume on the total volume of the composition.
  • the proportion of all constituents which are introduced in the continuous process is preferably 1% by volume to 99% by volume, in particular 5% by volume to 95% by volume, preferably 10% by volume to 80% by volume. %.
  • Ingredients are solvents, active ingredients and other components, i.e. all ingredients of the composition.
  • the method according to the invention is preferably a method for producing personal care, washing or cleaning agents, in particular washing or cleaning agents.
  • the feature that the mixture has a temperature in the range of 35 ° C or more at the beginning of the continuous process means that the mixture which is fed from the batch boiler into the continuous system, when entering the continuous system has a temperature of 35 ° C or more.
  • the temperature of the mixture is determined in the batch boiler and in the continuous system on the supply line using a commercially available PT100 resistance thermometer.
  • the thermometer is installed in the boiler next to the outlet, through which the mixture reaches the continuous system.
  • the mixture in the batch boiler has the same temperature during discharge as at the time of introduction into the continuous system. This is checked using a second PT100 resistance thermometer, which is installed in the continuous system at the point at which the mixture is fed.
  • the temperature of the mixture in the batch boiler is set well above 35 ° C in order to introduce the mixture into the continuous system at 35 ° C or more.
  • the mixture is therefore not reheated between the boiler and the continuous system before it reaches the continuous system. Rather, the heat of the batch mixture is used to feed the mixture into the continuous system at a temperature of 35 ° C. or more without further heating. This is a particular advantage of the present invention because it helps to save energy and stabilize the mixture.
  • Mixtures are usually produced in a batch process at an elevated temperature. In most processes this is 35 ° C or higher. At the end of the batch process, the mixture often has temperatures in the range from 40 ° C. to 90 ° C.
  • the batch temperature is often based on the fact that a solvent with a temperature of 40 ° C. or more, in particular 50 ° C. or more, preferably 60 ° C. or more, is used. These temperatures enable the active substances which are to be dissolved in the solvent in a batch process to dissolve well or to be distributed therein.
  • the solvent can be introduced into the batch process at a temperature which is higher than room temperature.
  • Room temperature in the sense of the present invention means 20 ° C.
  • other substances that have one of the temperatures described above can also be added to the batch.
  • the solvent and the entire mixture can be heated in a batch process. This can be done on the one hand by frictional or shear forces that occur during mixing in a batch process. Heating elements can also be used to heat the mixture in the batch boiler. In the batch process, however, exothermic reactions often take place, in which additional heat is released, as a result of which the temperature in the Batch mixing tank rises. Corresponding exothermic reactions are, for example, neutralization reactions which occur when tensides, in particular anionic surfactants, are produced in batch by neutralization of the corresponding acid.
  • Acids of the anionic surfactants disclosed herein are neutralized in the batch kettle with a suitable neutralizing agent.
  • the heat generated by the neutralization reaction in the boiler or by the supply of the warm neutralizate in the boiler increases the temperature of the mixture in the batch. This improves the solubility of the individual components in the mixture.
  • Suitable neutralizing agents in the context of the present invention are all substances which are able to neutralize the anionic surfactant in its acid form, i.e. convert to an anionic surfactant salt.
  • the neutralizing agent can be added in liquid or solid state.
  • Neutralizing agent in the liquid state includes solutions and suspensions of solid neutralizing agents.
  • alkali metal hydroxides such as NaOH or KOH
  • basic oxides such as alkali metal oxides or basic salts such as carbonates
  • Other neutralizing agents are ammonia and amines.
  • Amines are preferably selected, in particular from the group consisting of monoethanolamine, trimethylamine, triethylamine, tripropylamine, triethanolamine, N-methyneorpholine, morpholine, 2,2-dimethylmonoethanolamine, N, N-dimethylmonoethanolamine and mixtures thereof.
  • the amines are very particularly preferred because they are easy to handle and no water is formed during the neutralization. Monoethanolamine is particularly preferred.
  • the neutralizing agents can be combined with the anionic surfactant acids customary for detergents, cleaning agents and care products, in particular with the anionic surfactant acids corresponding to the anionic surfactants disclosed herein.
  • Neutralizing agents are preferably used in a certain molar stoichiometric ratio to the anionic surfactant acid, which allows the reaction to proceed to completion under the chosen reaction conditions.
  • the molar ratio of neutralizing agent to anionic surfactant acid can be 0.5: 1 to 10: 1, preferably 1: 1 to 3: 1.
  • a particularly preferred anionic surfactant acid is C 9 -C 13 alkylbenzenesulfonic acid, in particular linear C 9 to C 13 alkylbenzenesulfonic acid.
  • linear C 9 -C 13 alkylbenzenesulfonic acid (LAS acid or HLAS) and monoethanolamines, which are preferably constituents of the mixture produced in the batch process (masterbatch), react with one another with the development of heat.
  • linear C 9 -C 13 alkylbenzenesulfonic acid is neutralized with monoethanolamine in a batch process.
  • a particular advantage of using monoethanolamine is the avoidance of water formation as a neutralization product. This is particularly important in the production of anhydrous or low-water mixtures and compositions. It is advantageous to prepare the anionic surfactants from the corresponding acids only in a batch, since on the one hand the acid can be obtained more cheaply and the heat of neutralization heats the mixture, so that the dissolution of the components in the mixture is accelerated. In certain embodiments, the further targeted supply of heat can be dispensed with, which allows a more economical process flow. Heat can also be released when one or more active substances are mixed in a solvent. Such a method is preferred in the batch process since most of the constituents are more soluble in the solvent.
  • the mixture can be provided with defoamers in a continuous process, in particular in such a way that the composition has at least 0.1% by weight of defoamers.
  • solvents with a low flash point can escape and thereby form an explosive atmosphere, which can endanger the safety of the production, so that these, too, are preferably added in a continuous process.
  • Enzymes for the purposes of the present invention are all known enzymes suitable in detergent processes, e.g. Amylases, lipases, cellulases, pectinase and proteases.
  • Defoamers in the context of the present invention are silicones.
  • Silicone oils are particularly preferred.
  • Suitable silicones are conventional organopolysiloxanes, which can have a content of finely divided silica, which in turn can also be silanized.
  • organopolysiloxanes are, for example, in the European patent application EP 0496510 A1 described.
  • Polydiorganosiloxanes which are known from the prior art are particularly preferred.
  • the polydiorganosiloxanes contain finely divided silica, which can also be silanized.
  • Silica-containing dimethylpolysiloxanes are particularly suitable.
  • the temperature of the mixture is reduced by the cooling according to the invention.
  • the temperature of the mixture at the end of the continuous process is preferably below 35 ° C., in particular 25 ° C., or less.
  • This mixture obtained at the end of the continuous process is finally filled into suitable containers.
  • the container is a canister or container in which the composition is initially stored.
  • the container is an intermediate storage here.
  • the batch-produced mixture can be cooled in a continuous manner in various ways.
  • a continuous system in which a corresponding continuous process can be carried out, comprises a main line in which the different components of the composition are introduced via secondary lines in a predetermined, defined sequence.
  • the highly concentrated mixture which is usually produced in a batch process, is diluted with a suitable solvent, usually water. Cooling can now take place in that the supplied components and the solvent have a lower temperature than that of the mixture.
  • a suitable solvent usually water.
  • Cooling can now take place in that the supplied components and the solvent have a lower temperature than that of the mixture.
  • cooling medium mostly water
  • Suitable apparatuses include plate heat exchangers, shell-and-tube heat exchangers, double-tube heat exchangers with or without a mixing element in the product-side tube.
  • static and / or dynamic mixers can be provided in the main line. If static mixers are provided, they can also act as cooling.
  • the static mixers can either comprise a material that can be cooled, such as a metal or a thermally conductive plastic. It is also conceivable that a suitable coolant flows through the static mixer, as a result of which the mixture is cooled.
  • the continuous process is characterized in that there is an overpressure within the plant in which the continuous process takes place.
  • the mixture is passed through a pipe system.
  • the flow rate of the composition and thus also the pressure in the line system are controlled by means of pumps.
  • Pressure sensors attached to the line system make it possible to control the pressure within the line system via feedback to the pumps.
  • the main line, into which the mixture is introduced, or the material flow flowing in it, is called the main flow.
  • the other active substances or components of the composition are also metered into this main line.
  • the continuous process under positive pressure also allows gas / air to be avoided in the composition.
  • the continuous process is preferably carried out at a pressure of 0.1 to 6 bar, in particular of 0.5 to 4 bar, which is higher than the ambient pressure.
  • Liquid products in the sense of the present invention are liquids or solutions of solids in a suitable solvent as well as stable suspensions, dispersions or emulsions.
  • the method according to the invention now makes it possible to control the temperature across the entire method.
  • one or more components and / or active substances can be added to the composition at a predetermined temperature, which takes into account the properties of the respective active substance / component.
  • a predetermined temperature which takes into account the properties of the respective active substance / component.
  • saline solutions or other additives for adjusting the viscosity can be added.
  • High temperatures are also possible for the addition of brighteners.
  • Enzymes or dyes are added towards the end of the continuous process, since at this point the mixture is already at a lower temperature than at the beginning due to the cooling.
  • the respective feed lines can also be used to introduce other or further constituents into the main stream in this or a different sequence.
  • the temperature prevailing in the main stream, the number and position of the mixers and the sequence in which the constituents are added are to be observed by a person skilled in the art.
  • only one material is introduced into the feed line via each of the feed lines.
  • water can be dosed via feed line 1, the masterbatch via feed line 2 and ethanol via feed line 3.
  • ethanol it is also possible for ethanol to be metered in via feed line 1, 2 water via feed line and 3 the masterbatch via feed line 3. The same applies to the other supply lines.
  • the master batch is preferably fed into the continuous system only via one access.
  • the masterbatch is introduced via one of the supply lines 1, 2, 3 or 4 as shown above.
  • Solvent water or non-aqueous solvent
  • the masterbatch is introduced into the continuous system via feed line 1 or 2. It is advantageous to dose the preservative in one of the feed lines 2 to 6, since then the major part of the system is flushed with preservative.
  • FIG. 1 and Fig. 2 The embodiments shown by way of example show different feed lines for enzymes (14, 15, 16, 17). All are located along the flow direction within the main line in the second half of the system, so they are added towards the end of the process.
  • This has the advantage that here the mixture, for example through the cooler (A) and the two static mixers (B, C) and the supply of preferably cold water (1, 2, 3, 4, 5, 6, 7) for direct Cooling is cooled so that degradation of the enzymes no longer takes place.
  • the same or different enzymes can be metered in via different feed lines. Different enzymes can also be dosed via the same lines.
  • the defoamer is preferably metered into the continuous system only when the temperature of the main stream is less than 30 ° C. in order to avoid phase separations.
  • the defoamer could be introduced via feed line 5, 6, 7, 8, 9, 10, 11 or 12.
  • a cold solvent in particular cold water, is preferably metered into the main stream via at least one of the first feed lines (1, 2, 3, 4, 5, 6, 7).
  • Cold here means a lower temperature than the masterbatch, i.e. the mixture produced in the batch process.
  • the cold solvent preferably has a temperature in the range from 7 ° C to 20 ° C. A lower temperature would mean an excessive temperature difference compared to the masterbatch, which could impair the product properties and make further processing more difficult. Higher temperatures do not lead to cooling.
  • solvents such as water or alcoholic solvents such as ethanol or propanol are preferably added at the beginning of the process. This also results in cooling. Furthermore, a quick dilution of the supplied components is possible. In addition, a flow in the main stream is generated and maintained by the solvents, in particular by the water.
  • the composition which at the end of the main stream, after thorough mixing, is returned to the main stream.
  • this is shown schematically with supply line 13.
  • individual components can be replenished without, for example, another dynamic mixer having to be kept available.
  • the pH value or the viscosity or similar properties can be readjusted before the composition is then filled at the end of the process.
  • a premixing chamber (D1) can be present.
  • Several raw materials for example enzymes or other components or active substances, can be added to the existing mixture at the same time and premixed in this premixing chamber (D1) in a short residence time.
  • the final mixing of all components contained in the composition then takes place in the subsequent mixer.
  • the residence time in the premixing chamber is usually 2 seconds or less.
  • cooling by means of a cooler (A) does not only take place on the main line.
  • the feed lines also include cooling, so that, for example, the mixture produced from the batch process is introduced into the main line via a feed line (1, 2, 3 or 4), the corresponding feed line comprising a cooling device, so that the mixture is already cooled for the first time.
  • the masterbatch is only metered into the main stream via one of the feed lines.
  • the continuous system according to the invention can furthermore have a decoupling container as an atmospheric buffer. This enables a constant pressure at the end of the continuous system, so that easy filling is possible.
  • the mixture produced in the batch process preferably has a high concentration of the at least one active substance contained.
  • the active substance is preferably at least one surfactant.
  • the mixture preferably has anionic surfactant in a proportion from 8% by weight to 36% by weight, particularly preferably from 10% by weight to 30% by weight, more preferably from 20% by weight to 28% % By weight.
  • the mixture more preferably has nonionic surfactant in a proportion of 1% by weight to 27% by weight, in particular 10% by weight to 26% by weight, particularly preferably 15% by weight to 25% by weight on.
  • Anionic surfactants anionic surfactants
  • nonionic surfactants nonionic surfactants
  • mixtures which have at least one surfactant are usually only stable at elevated temperature, so that the mixture which is prepared in a batch process preferably has a temperature of over 40 ° C. and as long as it has this temperature the continuous process is introduced. It is desirable that the surfactant mixture be diluted rapidly in the continuous process, since otherwise the surfactants may flocculate. In addition to the surfactants, flocculation of soaps or phosphonates can also occur. With certain surfactants, a slow dilution would result in a mixture of very high viscosity, which could then no longer be processed further.
  • a rapid dilution can easily be made possible in the continuous process, since the metering of the mixture in relation to the metering of water into the main line can be controlled well. It is particularly preferred to use a high-shear mixer for thorough mixing, for example a so-called Pentax mixer, in the continuous system.
  • a high-shear mixer for thorough mixing, for example a so-called Pentax mixer, in the continuous system.
  • Pentax mixer for thorough mixing
  • This enables a more flexible preparation of a starting mixture in batch, since there are now fewer limitations with regard to the batch mixture.
  • This enables more concentrated mixtures to be made, which can be flexibly differentiated by dilution in a continuous system.
  • the proportion of solvent in the batch mixture can be reduced, which is why a smaller batch boiler can be used. This saves investment, cleaning and maintenance costs.
  • the present invention thus makes it possible to produce the agents more cheaply and more efficiently.
  • phosphonate is understood here to mean those phosphonates which act as complexing agents in the compositions produced according to the invention.
  • the mixture produced in the batch process still has a total phosphonate content of from 0.5% by weight to 8.0% by weight, preferably from 1.0% by weight to 5% by weight more preferably from 1.5% to 3.0% by weight.
  • the complex-forming phosphonates comprise a number of different compounds such as, for example, diethylenetriaminepenta (methylenephosphonic acid) (DTPMP). Hydroxyalkane or aminoalkane phosphonates are particularly preferred in this application.
  • HEDP 1-hydroxyethane-1,1-diphosphonate
  • HEDP 1-hydroxyethane-1,1-diphosphonate
  • It is preferably used as the sodium salt, the disodium salt reacting neutrally and the tetrasodium salt in an alkaline manner (pH 9).
  • Aminoalkane phosphonates are preferably ethylenediamine tetramethylene phosphonate (EDTMP), diethylene triamine pentamethylene phosphonate (DTPMP) and their higher homologs. They are preferably in the form of the neutral sodium salts, e.g. B. as the hexasodium salt of EDTMP or as the hepta and octa sodium salt of DTPMP. HEDP is preferably used as the builder from the class of the phosphonates.
  • the aminoalkanephosphonates also have a pronounced ability to bind heavy metals. Accordingly, it may be preferred, particularly if the agents also contain bleach, to use aminoalkanephosphonates, in particular DTPMP, or to use mixtures of the phosphonates mentioned.
  • HEDP 1-hydroxyethane-1,1-diphosphonic acid
  • DTPMP diethylenetriaminepenta
  • the mixtures can of course contain two or more different phosphonates.
  • Preferred mixtures are characterized in that the washing or cleaning agent contains at least one complexing agent from the group of the phosphonates, preferably 1-hydroxyethane-1,1-diphosphonate, the proportion by weight of the phosphonate in the total weight of the mixture preferably being from 0.1 to 8 , 0 wt .-%, preferably from 0.2 to 5.0 wt .-% and in particular from 0.5 to 3.0 wt .-%.
  • the mixture produced in the batch process has a total fatty acid content of 3.0% by weight to 20% by weight, preferably from 5.0% by weight to 15% by weight, still more preferably of 7.0% to 10% by weight.
  • Stable in the sense of the present invention means that creaming, phase separation, sedimentation, flocculation or specks, clouds, cloudiness, a milky appearance, solidification or color changes are not to be observed.
  • the mixture (masterbatch) prepared in the batch process is preferred over a period of 1 day or more, in particular 5 days or more or of 1 week or more, preferably of 2 weeks or more and in particular of 3 weeks or more, preferably of 4 weeks or more stable, if it is stored at a temperature of 40 ° C or above, especially from 40 ° C to 90 ° C.
  • the masterbatch, when stored at 40 ° C. is preferably stable for 2 weeks or longer, in particular 4 weeks.
  • the composition produced according to the invention is preferably stable over a period of 4 weeks or more, in particular 8 weeks or more, preferably 12 weeks or more.
  • the composition can be stored at room temperature or above, especially at 20 ° C to 40 ° C.
  • the composition is particularly preferably stable when stored at 40 ° C. for at least 12 weeks.
  • the composition and in particular the mixture can have one or more surfactants.
  • These surfactants are selected from the group consisting of anionic, cationic, zwitterionic, nonionic surfactants and mixtures thereof. If the composition or the mixture comprises several surfactants, these can be, for example, several different nonionic surfactants. However, it is also possible for the composition or the mixture to comprise, for example, both nonionic and anionic surfactants. This applies analogously to the other surfactants.
  • the composition and / or the mixture preferably comprise at least one anionic surfactant and at least one nonionic surfactant. If the mixture does not include any surfactants, these are added to the mixture in a continuous process. If the mixture comprises one or more surfactants, further surfactants can be added in a continuous process if required.
  • Anionic surfactants are preferably selected from the group consisting of C 9-13 alkyl benzene sulfonates, olefin sulfonates, C 12-18 alkane sulfonates, ester sulfonates, alk (en) yl sulfates, fatty alcohol ether sulfates and mixtures thereof. It has been shown that these sulfonate and sulfate surfactants are particularly suitable for producing stable liquid compositions, in particular those with a flow limit. Liquid compositions which comprise C 9-13 alkyl benzene sulfonates and fatty alcohol ether sulfates as the anionic surfactant have particularly good dispersing properties.
  • the surfactants of the sulfonate type are preferably C 9-13- alkylbenzenesulfonates, olefin sulfonates, that is to say mixtures of alkene and hydroxyalkanesulfonates and disulfonates such as are obtained, for example, from C 12-18 monoolefins having a terminal or internal double bond by sulfonating with gaseous Sulfur trioxide and subsequent alkaline or acidic hydrolysis of the sulfonation products is considered.
  • esters of ⁇ -sulfofatty acids for example the ⁇ -sulfonated methyl esters of hydrogenated coconut, palm kernel or tallow fatty acids.
  • alk (en) yl sulfates are the alkali and especially the sodium salts of the sulfuric acid half esters of C 12 -C 18 fatty alcohols, for example from coconut fatty alcohol, tallow fatty alcohol, lauryl, myristyl, cetyl or stearyl alcohol or the C 10 -C 20 oxo alcohols and those half-esters of secondary alcohols of this chain length are preferred.
  • the C 12 -C 16 alkyl sulfates and C 12 -C 15 alkyl sulfates as well as C 14 -C 15 alkyl sulfates are preferred from the point of view of washing technology. 2,3-Alkyl sulfates are also suitable anionic surfactants.
  • fatty alcohol ether sulfates such as the sulfuric acid monoesters of the straight-chain or branched C 7-21 alcohols ethoxylated with 1 to 6 moles of ethylene oxide, such as 2-methyl-branched C 9-11 alcohols with an average of 3.5 moles of ethylene oxide (EO) or C 12 -18 -Fatty alcohols with 1 to 4 EO are suitable.
  • the liquid composition and / or the mixture produced in the batch process contain a mixture of sulfonate and sulfate surfactants.
  • the liquid composition and / or the mixture prepared in a batch process contains C 9-13 -alkylbenzenesulfonates and fatty alcohol ether sulfates as anionic surfactant.
  • the liquid composition and / or the mixture produced in a batch process can also contain soaps.
  • Saturated and unsaturated fatty acid soaps are suitable, 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 and the soaps can be in the form of their sodium, potassium or magnesium or ammonium salts.
  • the anionic surfactants are preferably in the form of their sodium salts.
  • Other preferred counterions for the anionic surfactants are the protonated forms of choline, triethylamine, monoethanolamine or methylethylamine.
  • the composition and / or the mixture produced in the batch process can also have at least one nonionic surfactant.
  • the nonionic surfactant includes alkoxylated fatty alcohols, alkoxylated fatty acid alkyl esters, fatty acid amides, alkoxylated fatty acid amides, polyhydroxy fatty acid amides, alkylphenol polyglycol ethers, amine oxides, alkyl polyglucosides and mixtures thereof.
  • the nonionic surfactant used is preferably alkoxylated, advantageously ethoxylated, in particular primary alcohols having preferably 8 to 18 carbon atoms and an average of 4 to 12 moles of ethylene oxide (EO) per mole of alcohol, in which the alcohol radical is linear or preferably in 2-position can be methyl-branched or can contain linear and methyl-branched radicals in the mixture, as are usually present in oxo alcohol radicals.
  • EO ethylene oxide
  • alcohol ethoxylates with linear residues of alcohols of native origin with 12 to 18 carbon atoms, for example from coconut, palm, tallow fat or oleyl alcohol, and an average of 5 to 8 EO per mole of alcohol are particularly preferred.
  • the preferred ethoxylated alcohols include, for example, C 12-14 alcohols with 4 EO or 7 EO, C 9-11 alcohol with 7 EO, C 13-15 alcohols with 5 EO, 7 EO or 8 EO, C 12-18 -Alcohols with 5 EO or 7 EO and mixtures of these.
  • the degrees of ethoxylation given represent statistical averages, which can be an integer or a fraction for a specific product.
  • Preferred alcohol ethoxylates have a narrow homolog distribution (narrow range ethoxylates, NRE).
  • fatty alcohols with more than 12 EO can also be used. Examples include 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.
  • a mixture of a (more) branched ethoxylated fatty alcohol and an unbranched ethoxylated fatty alcohol such as a mixture of a C 16-18 fatty alcohol with 7 EO and 2-propylheptanol with 7 EO.
  • the washing, cleaning, post-treatment or auxiliary washing agent particularly preferably contains a C 12-18 fatty alcohol with 7 EO or a C 13-15 oxo alcohol with 7 EO as the nonionic surfactant.
  • the composition produced according to the invention further comprises one or more solvents in the mixture.
  • This can be water and / or non-aqueous solvents.
  • the mixture preferably contains water as the main solvent.
  • the batch-made mixture may further comprise non-aqueous solvents. Suitable non-aqueous solvents include monohydric or polyhydric alcohols, alkanolamines or glycol ethers.
  • the solvents are preferably selected from ethanol, n-propanol, i-propanol, butanols, glycol, propanediol, butanediol, methylpropanediol, glycerol, diglycol, propyldiglycol, butyldiglycol, hexylene glycol, ethylene glycol methyl ether, ethylene glycol ethyl ether, ethylene glycol propyl ether, ethylene glycol mono-ether, ethylene glycol, n-butyl butyl Diethylene glycol ethyl ether, propylene glycol methyl ether, propylene glycol ethyl ether, propylene glycol propyl ether, dipropylene glycol monomethyl ether, dipropylene glycol monoethyl ether, methoxytriglycol, ethoxytriglycol, butoxytriglycol, 1-butoxyethoxy-2-propanol, 3-
  • the composition has one or more non-aqueous solvents, in particular those with low vapor pressure, such as ethanol or 2-propanol, these are preferably added to the mixture in a continuous process.
  • the continuous process is carried out in a closed system so that the corresponding solvent cannot evaporate. This reduces the risk to the environment and almost impossible. It is also possible according to the invention that water or other suitable solvents, regardless of their vapor pressure, are introduced in a continuous process.
  • the present method has the advantage that a composition can be obtained in which the individual components can be metered in such a way that they are only exposed to the temperature at which they are stable. Effective cooling and dilution can also take place. Cooling of a boiler from a batch process depends on the difference in the temperature in the boiler and the ambient temperature. Accordingly, cooling a mixture which has a temperature of 40 ° C. and in particular 35 ° C. is lengthy and time-consuming. The cooling from, for example, 90 ° C to 40 ° C takes place relatively quickly. However, the further cooling to approximate room temperature, at which filling preferably takes place, takes a very long time. Filling at room temperature is therefore desirable since the containers usually comprise a plastic, so that the containers can be deformed at higher temperatures. Cooling in the batch process is usually only possible at the edge of the container, whereby, however, the entire mixture is not cooled, but only the part of the mixture which is in contact with the edge of the container.
  • the Konti system now enables effective cooling, rapid dilution, and mixing that is adapted to the components introduced.
  • a particularly effective mixing of all active substances and components can be achieved by permutation of static and dynamic mixers within the main line which is preferred according to the invention.
  • the active ingredients or components can now be metered in either directly before the static or dynamic mixer (s), so that the shear force required for mixing can be ensured.
  • Components or active substances that are sensitive to shear forces can be introduced after the dynamic mixer (s).
  • the method according to the invention thus not only enables temperature-adapted production, but also takes into account the shear forces acting on the components, so that the mechanical load can also be controlled.
  • solids which are to be stably suspended in the liquid surfactant-containing composition can be introduced into the main line after the last dynamic mixer and preferably before the last static mixer.
  • the composition obtained is preferably a composition with a yield point. It is particularly preferred if the composition has a yield point of 0.01 to 50 Pa. In rheology, the yield point is understood to be the shear stress (in Pa) below which a sample deforms exclusively or at least largely elastically and above which an irreversible, plastic deformation, i.e. a flow, takes place.
  • the yield point of the liquid, surfactant-containing composition is measured with an absolute measuring rotary rheometer from TA-Instruments, type AR G2 (shear stress controlled rheometer, cone-plate measuring system with 40 mm diameter, 2 ° cone angle, 20 ° C).
  • This is a so-called shear stress controlled rheometer.
  • the samples in the rheometer are subjected to a shear stress ⁇ (t) that increases with time.
  • the shear stress can be increased from the smallest possible value (for example 0.01 Pa) to for example 100 Pa in the course of 30 minutes.
  • the deformation ⁇ of the sample is measured as a function of this shear stress ⁇ .
  • the composition preferably has a yield point in the range from 0.01 Pa to 50 Pa, preferably from 0.1 Pa to 10 Pa, particularly preferably from 0.5 Pa to 5 Pa.
  • Compositions which have a yield point of at most 10 Pa are particularly preferred. These are particularly easy to fill and easy to dose by the consumer.
  • composition can further comprise builders and / or alkaline substances. These are particularly preferably added to the mixture in a batch process. However, it is also possible for these to be added in solution in a suitable solvent in a continuous process.
  • Polymeric polycarboxylates are suitable as builders. These are, for example, the alkali metal salts of polyacrylic acid or polymethacrylic acid, for example those with a relative molecular weight of 600 to 750,000 g / mol.
  • Suitable polymers are, in particular, polyacrylates, which preferably have a molecular weight of 1,000 to 15,000 g / mol. Because of their superior solubility, the short-chain polyacrylates with molecular weights of 1,000 to 10,000 g / mol, and particularly preferably 1,000 to 5,000 g / mol, can in turn be preferred from this group.
  • copolymeric polycarboxylates in particular those of acrylic acid with methacrylic acid and of acrylic acid or methacrylic acid with maleic acid.
  • the polymers can also contain allylsulfonic acids, such as allyloxybenzenesulfonic acid and methallylsulfonic acid, as monomers.
  • silicates As builders, which can be contained in the composition, silicates, aluminum silicates (in particular zeolites), carbonates, salts of organic di- and polycarboxylic acids and mixtures of these substances are to be mentioned in particular.
  • Organic builders which may also be present in the composition are, for example, the polycarboxylic acids which can be used in the form of their sodium salts, polycarboxylic acids being understood to mean those carboxylic acids which carry more than one acid function.
  • these are citric acid, adipic acid, succinic acid, glutaric acid, malic acid, tartaric acid, maleic acid, fumaric acid, sugar acids, aminocarboxylic acids, nitrilotriacetic acid (NTA), methylglycinediacetic acid (MGDA) and their derivatives, and mixtures of these.
  • Preferred salts are the salts of polycarboxylic acids such as citric acid, adipic acid, succinic acid, glutaric acid, tartaric acid, sugar acids and mixtures of these.
  • soluble builders such as citric acid, or acrylic polymers with a molecular weight of 1,000 to 5,000 g / mol are preferably used in the basic formulation.
  • alkaline substances or washing alkalis are chemicals for raising and stabilizing the pH of the composition.
  • the process according to the invention therefore makes it possible to produce a mixture which can then be differentiated into different products in a continuous process. This results in an effective production of different products, since only one mixture has to be produced for several products.
  • the storage time of the finished products is shorter because the quantity of the product manufactured can be controlled and adjusted more easily in continuous processes.
  • a large quantity of a product is manufactured in a batch process, which must then be stored either before or after filling. This results in a large space requirement, which can be reduced in the method according to the invention.
  • dyes in particular, dyes, perfume compositions, enzymes, perfume capsules, microbeads, opacifiers, color transfer inhibitors, brighteners, salt solutions, co-surfactants and water or other solvents, in particular for dilution in a continuous process, are added.
  • the mixture is further processed along the main stream through which the mixture flows from the batch process.
  • the active substances or components to be metered can also be premixed and metered together into the main stream or individually or in various combinations of, for example 2-3 components or active substances can be metered into the main stream via separate feed lines. It is preferred that there is a mixer, in particular a static mixer, at the point at which the metering into the main stream takes place, which ensures the rapid and homogeneous distribution of the metered agents (components and / or active substances) in the main stream.
  • a mixer in particular a static mixer, at the point at which the metering into the main stream takes place, which ensures the rapid and homogeneous distribution of the metered agents (components and / or active substances) in the main stream.
  • dyes, microcapsules and perfume can be metered separately into the stream. From the introduction of the basic recipe, the perfume can be dosed first, followed by the dye in a subsequent step.
  • the order of dosing can also be done in reverse order, i.e. first dye and then perfume.
  • a dye is first dosed into the basic recipe and the perfume or another substance is only added in a later step, the path taken by the dye through the system is long, so that when changing the recipe, much more cleaning effort is required to also to remove the last traces of dye.
  • the location of the perfume dosage must also be determined in this regard.
  • the visual perception is stronger for the consumer than the odor-specific one, so that in case of doubt the dye must be dosed after the perfume in order to avoid that the consumer perceives unintentional product discoloration due to a change in formulation.
  • further processing takes place in a continuous process, in particular by adding one or more co-surfactants and / or one or more electrolytes.
  • the micellar structure of the surfactants in the mixture is changed by the co-surfactant or the co-surfactants. This effect can be enhanced by one or more electrolytes. This creates a lamellar structure of the surfactants.
  • Corresponding structured detergents or cleaning agents with a flow limit are, for example, in the prior art in WO 2013/064357 A1 described. Full reference is made to the content of this application.
  • Co-surfactants in the sense of the present invention are amphiphilic molecules with a small, hydrophilic head group. In a binary system with water, these co-surfactants are often only slightly or not soluble at all. Accordingly, they do not form micelles there either. In the presence of the surfactants of the basic formulation, the co-surfactants are incorporated into their associates and thereby change the morphology of these associates. The ball micelles become rod and / or disc micelles. If the total surfactant content is sufficiently high, lamellar phases or structures are formed.
  • the co-surfactant is preferably selected from the group consisting of alkoxylated C 8 -C 18 fatty alcohols with a degree of alkoxylation 3 3, aliphatic C 6 -C 14 alcohols, aromatic C 6 -C 14 alcohols, aliphatic C 6 -C 12 -Dial alcohols, monoglycerides of C 12 -C 18 fatty acids, monoglycerin ethers of C 8 -C 18 fatty alcohols and mixtures thereof.
  • Other suitable co-surfactants are 1-hexanol, 1-heptanol, 1-octanol, 1,2-octanediol, stearin monoglycerin and mixtures thereof.
  • fragrance alcohols such as geraniol, nerol, citronellol, linalool, rhodinol and other terpene alcohols or fragrance aldehydes such as lilial or decanal are suitable as co-surfactants.
  • Preferred co-surfactants are C 12 -C 18 fatty alcohols with a degree of alkoxylation 3. 3. These co-surfactants are particularly well incorporated into the preferred associations of anionic and nonionic surfactant.
  • Suitable alkoxylated C 12 -C 18 fatty alcohols with a degree of alkoxylation 3 3 include, for example, iC 13 H 27 O (CH 2 CH 2 O) 2 H, iC 13 H 27 O (CH 2 CH 2 O) 3 H, C 12-14 -Alcohol with 2 EO, C 12-14 -alcohol with 3 EO, C 13-15 -alcohol with 3 EO, C 12-18 -alcohols with 2 EO and C 12-18 -alcohols with 3 EO.
  • An electrolyte in the sense of the present invention is an inorganic salt.
  • Preferred inorganic salts include sodium chloride, potassium chloride, sodium sulfate, sodium carbonate, potassium sulfate, potassium carbonate, sodium hydrogen carbonate, potassium hydrogen carbonate, calcium chloride, magnesium chloride and mixtures thereof. Particularly stable compositions are obtained when sodium chloride or mixtures of sodium chloride and potassium sulfate are used.
  • the addition of the inorganic salt supports the formation of lamellar structures.
  • the inorganic salt has an influence on the viscosity, so that the viscosity of the liquid composition can be adjusted with the aid of the inorganic salt.
  • the flow limit is preferably generated by metering the co-surfactants and / or one or more electrolytes in the continuous process. This has the advantage that the constituents metered in the continuous process are immediately available in the desired lamellar structure.
  • the proportion of co-surfactants and / or electrolytes in the final liquid, surfactant-containing composition with a yield point is up to 15% by weight, preferably up to 10% by weight, even more preferably up to 5% by weight.
  • Dispersed particles are preferably added to the mixture in a continuous process.
  • Dispersed particles for the purposes of the present invention are not soluble in the solvent of the mixture from the batch process. However, they can be dispersed in them.
  • the inventive method enables a homogeneous distribution and stable dispersion of these particles.
  • these dispersed particles can be functional and / or have an aesthetic function. Functional materials affect the effect of the composition, whereas aesthetic materials only affect the appearance or the smell.
  • the dispersed particles are preferably visible particles. This means that the particles can be clearly recognized by the consumer in the composition (in the end product) and can be distinguished from the other constituents. This preferably means colored particles. Such particles give the composition a special impression that is appreciated by consumers.
  • the composition can particularly preferably contain a dissolved dye and additionally colored particles which have a color which is a contrasting color to the dissolved dye.
  • Functional dispersed particles can be capsules, abrasives, granules or compounds in the context of the present invention.
  • capsule means on the one hand aggregates with a core-shell structure and on the other hand aggregates with a matrix.
  • Core-shell capsules (microcapsules, microbeads) contain at least one solid or liquid core which is enclosed by at least one continuous shell, in particular a shell made of polymer (s).
  • the capsules can contain, for example, optical brighteners, surfactants, complexing agents, bleaching agents, bleach activators, bleaching catalysts, dyes and fragrances, antioxidants, builders, enzymes, enzyme stabilizers, antimicrobial agents, graying inhibitors, anti-redeposition agents, pH regulators, electrolytes, detergent boosters, vitamins , Proteins, foam inhibitors and / or UV absorbers.
  • the capsule fillings can be solids or liquids in the form of solutions or emulsions or suspensions.
  • the dispersed particles can have a density which corresponds to that of the liquid composition. According to the invention, this means that the density of the dispersed particles corresponds to 90% to 110% of the composition. However, it is also possible for the dispersed particles to have a different density. Nevertheless, because of the method according to the invention, it is also possible here to obtain a uniform dispersion of the particles in the composition. They can consist of different materials such as alginates, gelatin, cellulose, agar, waxes or polyethylenes. Particles that have no core-shell structure can also have an active ingredient in a matrix made of a matrix-forming material. Such particles are called "speckles". In these materials, matrix formation takes place, for example, via gelation, polyanion-polycation interaction or polyelectrolyte-metal ion interaction and is well known in the art as is the production of particles using these matrix-forming materials.
  • composition is in particular a personal care, washing or cleaning agent.
  • Personal care, washing or cleaning agents for the purposes of the present invention include cosmetics, household cleaners, fabric softeners, laundry detergents, floor care products, all-purpose cleaners, dishwashing detergents for manual and machine cleaning, heavy-duty detergents, shampoos, shower gels and foam baths, preferably a washing or cleaning agent .
  • the method according to the invention enables effective cooling during production and thus improved product stability.
  • a "one pass" production enables targeted uniform homogenization.
  • Investment costs can be reduced because the product formulation is based on a basic recipe, the batch-produced mixture, which can be produced in a simple process. This mixture can then be used for different products. This saves the storage of batches of end products that are not immediately sold. This reduces energy and production costs and at the same time increases the capacities of existing systems.
  • the components mentioned were produced in a batch reactor.
  • the cooling took place by means of recirculation in a plate heat exchanger.
  • the temperature was measured using a commercially available PT100 resistance thermometer, which was installed in the lower area of the batch boiler at the outlet of the batch.
  • the constituents mentioned were mixed with one another in a stirred kettle at a maximum temperature of 80 ° C. over a period of about 4 hours. It was then cooled to 30 ° C. The mass obtained showed flocculation after a short time and even phase separation was observed. Filling or further processing was not possible.
  • the constituents mentioned were mixed with one another in a stirred kettle at a maximum temperature of 80 ° C. over a period of about 4 hours.
  • the mixture produced was finally cooled to a temperature of 40 ° C.
  • the resulting mixture was kept at 40 ° C and remained clear and transparent for 4 weeks.
  • the decisive factor was the temperature measured by the thermometer at the batch outlet.
  • the 40 ° C warm mixture from the batch boiler was fed directly into the continuous system via the outlet next to which the resistance thermometer was installed. It was checked via a PT100 thermometer on the supply line to the continuous system that the mixture also had a temperature of 40 ° C when it was introduced.
  • the 40 ° C warm mixture was cooled in a continuous system at the same time and processed with different raw materials, such as dye, enzyme and perfume.
  • the cooling in the continuous system takes place up to a temperature of 20 ° C to 25 ° C, especially room temperature.
  • compositions were stable.

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Claims (11)

  1. Procédé de préparation d'une composition liquide contenant un tensioactif, dans lequel un mélange est préparé dans une première étape dans un procédé discontinu, lequel mélange est ensuite traité ultérieurement dans un procédé continu dans une seconde étape, caractérisé en ce que
    - le mélange préparé dans le procédé discontinu contient un tensioactif anionique dans une proportion de 5 à 40 % en poids ;
    - le tensioactif anionique est neutralisé dans le procédé discontinu ;
    - le mélange présente une température se trouvant dans la plage de 35 °C ou plus au début du procédé continu, et un refroidissement est effectué dans la seconde étape.
  2. Procédé selon la revendication 1, caractérisé en ce que le mélange préparé dans le procédé discontinu présente un solvant à une température de 40 °C ou plus, notamment de 60 °C ou plus.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce que l'acide alkylbenzènesulfonique en C9 à C13 est neutralisé par la monoéthanolamine dans le procédé discontinu.
  4. Procédé selon l'une des revendications 1 à 3, caractérisé en ce que le mélange préparé dans le procédé discontinu présente un tensioactif anionique dans une proportion de 8 à 36 % en poids, en particulier de 10 à 30 % en poids, de manière encore plus préférée de 20 à 28 % en poids, et/ou
    en ce que le mélange préparé dans le procédé discontinu présente un tensioactif non ionique dans une proportion de 1 à 27 % en poids, notamment de 10 à 26 % en poids, en particulier de 15 à 25 % en poids.
  5. Procédé selon l'une des revendications 1 à 4, caractérisé en ce que le mélange préparé dans le procédé discontinu présente une teneur totale en phosphonate de 0,5 à 8,0 % en poids, de préférence de 1,0 à 5 % en poids, de manière encore plus préférée de 1,5 à 3,0 % en poids, et/ou
    en ce que le mélange préparé dans le procédé discontinu présente une teneur totale en acides gras de 3,0 à 20 % en poids, de préférence de 5,0 à 15 % en poids, de manière encore plus préférée de 7,0 à 10 % en poids.
  6. Procédé selon l'une des revendications 1 à 5, caractérisé en ce que la composition présente une limite d'écoulement de 0,01 à 50 Pa.
  7. Procédé selon l'une des revendications 1 à 6, caractérisé en ce que la proportion de tous les constituants de la composition qui sont préparés dans le procédé discontinu est de 1 à 99 % en volume, de 5 à 95 % en volume, de manière encore plus préférée notamment de 20 à 90 % en volume, par rapport au volume total de la composition, et/ou en ce que la proportion de tous les constituants de la composition qui sont préparés dans le procédé continu est de 1 à 99 % en volume, notamment de 5 à 95 % en volume, de manière encore plus préférée de 10 à 80 % en volume, par rapport au volume total de la composition.
  8. Procédé selon l'une des revendications 1 à 7, caractérisé en ce que le mélange préparé dans le procédé discontinu est exempt d'agents d'anti-moussage, et/ou en ce que le mélange est pourvu d'agents d'anti-moussage dans le procédé continu, notamment de façon à ce que la composition présente au moins 0,1 % en poids d'agents d'anti-moussage.
  9. Procédé selon l'une des revendications 1 à 8, caractérisé en ce que la température du mélange au début du procédé continu est comprise entre 40 et 90 °C.
  10. Procédé selon l'une des revendications 1 à 9, caractérisé en ce que la température de la composition à la fin du procédé continu est de 35 °C ou moins, notamment de 25 °C.
  11. Procédé selon l'une des revendications 1 à 10, caractérisé en ce que, à la fin du procédé continu, la composition est transvasée dans des récipients, notamment dans des bouteilles et/ou dans des stockages intermédiaires.
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DE102018222190A1 (de) * 2018-12-18 2020-06-18 Henkel Ag & Co. Kgaa Verfahren zur Herstellung einer Partikel- und Tensid-haltigen Flüssigkeit
DE102019126124A1 (de) * 2019-09-27 2021-04-01 Henkel Ag & Co. Kgaa Verfahren zur Herstellung Tensid enthaltender Zusammensetzungen in einem sequenziellen Verfahren
US11680225B2 (en) * 2020-07-23 2023-06-20 Henkel Ag & Co. Kgaa Method for producing a washing agent with improved optical and rheological properties

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PL3317391T3 (pl) 2020-11-16
DE102015212131A9 (de) 2017-03-02
DE102015212131A1 (de) 2017-01-05
EP3317391A1 (fr) 2018-05-09
US20180112157A1 (en) 2018-04-26
WO2017001218A1 (fr) 2017-01-05
ES2804173T3 (es) 2021-02-04
AU2016288363A1 (en) 2018-02-22

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