Process for manufacturing a detergent portion unit
Patent Information
- Application Number
- EP2023701091
- Authority / Receiving Office
- EP · EP
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2022-04-13
- Filing Date
- 2023-01-18
- Publication Date
- 2025-02-19
AI Technical Summary
Existing detergent packaging materials are hygroscopic, leading to adhesion issues and reduced mechanical stability, which complicates handling and dissolution in cold washing processes, while also being non-washing active and contributing to packaging waste.
A method for producing detergent portion units with a dimensionally stable gel body formed by mixing surfactant and gelling agent compositions, which are then solidified to create a gel body with specific geometric shapes and compositions that enhance mechanical stability and dissolution rates, reducing packaging material usage and improving handling and performance.
The method results in detergent portion units with high product and storage stability, efficient dissolution, reduced packaging waste, and improved consumer appeal, while maintaining mechanical stability and washing performance.
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Abstract
Description
[0001] .Method for producing a detergent portion unit'
[0002] The present invention relates to a process for producing a detergent portion unit comprising a gel body.
[0003] The packaging and distribution of detergents and cleaning agents are constantly evolving. For some time now, a key focus has been on convenient dosing of detergents and cleaning agents for consumers and simplifying the steps required to carry out a washing or cleaning process. One technical solution is pre-portioned detergents or cleaning agents, for example, water-soluble containers with one or more compartments for powdered or liquid detergents or cleaning agents. Another technical solution is detergent tablets, which can be designed as single- or multi-phase products.
[0004] To produce the water-soluble containers, water-soluble polymers are typically formed into receiving chambers, which are then filled with a detergent or cleaning agent and finally sealed. The receiving chambers can be produced, for example, from water-soluble polymer films using a deep-drawing process. In an alternative process, a water-soluble polymer is formed into a receiving container using injection molding.
[0005] The water-soluble packaging material used to package the filled detergent portion units is generally hygroscopic. The water absorption capacity and tendency of the packaging material during production, packaging, storage, and subsequent use by the consumer can lead to portion units adhering to the surfaces of machines or packaging materials and preventing optimal conveyance, or to adjacent portion units sticking together, for example, in shared outer packaging. To prevent this tendency of the water-soluble portion units to adhere, it is possible to modify their surface properties by applying a powder. Powdering the water-soluble detergent portion units, in turn, requires an additional process step.
[0006] The water-soluble packaging materials used generally do not have any washing or cleaning properties, and therefore do not contribute to the product's effectiveness. Reducing the proportion of packaging in the total weight of the detergent portion units would therefore not result in any loss of performance and would be welcome for reasons of sustainability and cost-effectiveness.
[0007] Finally, the washing performance achieved by the detergent dosage unit is directly related to its dissolution properties. Especially in view of the increasing use of cold-wash processes, it is preferable to keep the thickness of the water-soluble film material contained in the detergent dosage unit as low as possible in order to accelerate the dissolution process. However, reducing the thickness of the surrounding film material simultaneously results in reduced mechanical stability of the dosage units. Overcoming this apparent dichotomy between mechanical stability and dissolution rate using water-soluble film-packaged detergent dosage units remains a relevant consideration in the development of water-soluble detergent dosage units.
[0008] An alternative to the previously described sachets is offered by detergent tablets, although sufficient mechanical stability and a high dissolution rate are incompatible in a similar way to the case of sachets.
[0009] An alternative to fully compressed detergent tablets is offered by multiphase detergent portion units, for example in the form of core tablets, which, in addition to a tableted body, also contain wax or gel phases. For example, European patent EP 1 032 642 B1 describes detergent tablets comprising a compressed phase and a non-compressed gel phase, and processes for their production.
[0010] Against the background of the previously described prior art, the application was based on the objective of providing efficient processes for the production of rapidly dissolving detergent portion units that exhibit high product and storage stability, are easy to package using minimal packaging materials, and appeal to the consumer through an appealing olfactory, visual, and / or tactile quality. The detergent portion units should exhibit high product performance and be easy and safe to handle for the consumer.
[0011] A first subject of the application is a method for producing a detergent portion unit, comprising a) a dimensionally stable gel body, comprising the steps: i) providing a first flowable surfactant-containing composition; ii) providing a second flowable gel-forming agent-containing composition different from the first flowable composition; iii) continuously feeding the first and second flowable compositions to a dynamic mixer; iv) mixing the first and second flowable compositions by means of the dynamic mixer to form a surfactant-containing and gel-forming agent-containing mixture; v) introducing the surfactant-containing and gel-forming agent-containing mixture into a
[0012] Forming device; vi) allowing the surfactant-containing and gelling agent-containing mixture to solidify to form a dimensionally stable gel body.
[0013] The term "detergent portion unit" describes a packaging containing a measured portion of a detergent or cleaning agent. Detergent portion units therefore refer to packaging for both textile washing and packaging for cleaning hard surfaces such as ceramics, glass, metal, or tiles. The detergent portion unit preferably has a weight of 14 g to 42 g, preferably 18 g to 38 g, and in particular 20 g to 34 g.
[0014] The detergent portion unit comprises a gel body. The detergent portion unit can consist of the gel body. In this case, the gel body preferably has a weight of 14 g to 42 g, preferably 18 g to 38 g, in particular 20 g to 34 g. If the detergent portion unit comprises further components in addition to the gel body, the weight of the gel body is preferably 10 g to 28 g, preferably 12 g to 23 g, and in particular 15 g to 20 g.
[0015] Gel bodies are bodies that exhibit elastic deformation behavior under the application of force. Bodies are considered dimensionally stable if they have an intrinsic shape stability that enables them to assume a non-disintegrating spatial shape under normal conditions of production, storage, transport, and handling by the consumer. This spatial shape does not change under these conditions even over a prolonged period, preferably 4 weeks, more preferably 8 weeks, and especially 32 weeks. This means that under the normal conditions of production, storage, transport, and handling by the consumer, they remain in the spatial-geometric shape determined by production, i.e., they do not melt.
[0016] The spatial shape of the gel body is fundamentally freely selectable; its side surfaces can be convex, concave, or flat, for example. However, certain spatial configurations have proven particularly advantageous in terms of manufacturability, storage, and use of the gel bodies.
[0017] In correspondingly advantageous detergent portion units, the gel body has a flat underside whose largest diagonal is greater than the height of the gel body. These bodies are not only easy to produce, for example, by means of a casting process, they can also be packaged easily and in a space-saving manner and are suitable for dosing via the dosing or dispensing chambers of electronic cleaning appliances. It is preferred if the gel body has a flat underside whose largest diagonal is more than 1.5 times, preferably more than 2 times, the height of the gel body.
[0018] For manufacturability, for example, with regard to demolding the gel body from a mold, it has proven advantageous if the underside of the gel body has no corners. Preferred gel bodies are therefore characterized by oval undersides or, alternatively, by ellipsoidal or round, preferably round, undersides. Corresponding gel bodies with a non-square underside are also preferred by many consumers due to their appearance. Therefore, preferred gel bodies are, for example, those that have a bottom and a top side connected by a cylindrical outer surface.
[0019] Advantages in terms of space utilization during production and packaging are realized by angular undersides. If, for example, the gel bodies are cast in the form of sheets, which are subsequently cut into gel bodies, angular undersides are advantageous because such gel bodies can be cut without creating any residue and can be packaged in a space-saving manner. In an alternative embodiment, preferred gel bodies therefore have angular undersides, in particular triangular, square, or hexagonal undersides. For further processing or packaging, it can be advantageous if the gel body has a angular underside with rounded corners.
[0020] With regard to the production, packaging and use of the detergent portion units, it has also proven advantageous if the gel bodies have an upper side that is plane-parallel to the underside.
[0021] In a first preferred geometric embodiment, the gel body has a bottom side and a top side which have the same geometric shape, wherein the bottom side and the top side have the same surface area. Corresponding gel bodies can, as already described above, be produced in a simple manner, for example by casting sheets and subsequently cutting the sheets into individual gel bodies. Moreover, these gel bodies can be spatially aligned more easily in any subsequent process steps, during packaging or use by the user due to the geometric identity of the bottom and top sides than gel bodies with a lower body symmetry. This applies in particular to gel bodies which simultaneously have a top side that is plane-parallel to the bottom side.Examples of such gel bodies are circular cylinders, elliptical cylinders, parallelepipeds, rhombohedrons, straight or oblique prisms, cuboids, or cubes. The group of circular cylinders and elliptical cylinders includes vertical circular cylinders and elliptical cylinders, as well as oblique circular cylinders and elliptical cylinders. Due to their ease of production by singulation from a single sheet, gel bodies in the form of vertical circular cylinders, vertical elliptical cylinders, straight prisms, straight cuboids, or cubes are preferred.
[0022] In an alternative embodiment, the gel body has a bottom and a top surface that have the same geometric shape, with the bottom and top surfaces having different surface areas. Such gel bodies may be preferred due to their attractive appearance or optimized fit, coupled with comparatively simple manufacturing. Examples of such gel bodies are circular cylinders or elliptical cylinders with a convex or concave bottom surface and a flat top surface. Further examples are truncated cones or truncated pyramids.
[0023] In summary, preferred subject matters of the application can be characterized as detergent portion units comprising a gel body with a bottom side and a top side, wherein the area of the top side is 80 to 100%, preferably 90 to 100% and in particular 98 to 100% of the bottom side.
[0024] The process is particularly suitable for the manufacture of gel bodies with a high surfactant content. In preferred embodiments, the first flowable surfactant-containing composition contains, based on its total weight, 30 to 70 wt.%, preferably 40 to 60 wt.%, and in particular 45 to 55 wt.% surfactant.
[0025] For the producibility and subsequent dissolving power of the gel bodies, it has proven advantageous if they contain 15 to 35 wt.%, preferably 20 to 30 wt.%, of an aqueous-organic solvent. The aqueous-organic solvent of the gel body is preferably introduced via the first and second flowable compositions. Thus, it is preferred if the second flowable gel-forming agent-containing composition also contains an organic solvent. Particularly preferred flowable gel-forming agent-containing compositions contain gel-forming agent and organic solvent in a total weight proportion above 50 wt.%, preferably above 70 wt.%, and in particular above 90 wt.%.
[0026] Preferred gel bodies also contain dye.
[0027] Preferred gel bodies are transparent. Gel bodies are referred to as "transparent" if they have a transmission above 50%, preferably above 60%, and in particular above 80% in the wavelength range from 410 to 800 nm at at least one wavelength, preferably at 600 nm. The transmission is determined by means of VIS spectrometry at a sample temperature of 20°C and a cuvette length of 10 mm. For the production and subsequent storage and transport properties of the gel bodies, it has proven advantageous to use low-molecular-weight gel formers with a molar mass of up to 2000 g / mol in the gel body, wherein their weight proportion of the total weight of the gel body is preferably less than 5 wt.%, preferably 0.1 to 5 wt.%, and particularly preferably 0.1 to 2.5 wt.%.Furthermore, the advantages of the process according to the invention are particularly evident in the processing of these low-molecular-weight gelling agents with their specific gelling properties.
[0028] In a preferred embodiment, the low-molecular-weight gelling agent has a water solubility of less than 0.1 g / L (20°C). The solubility of the organic gelling agent is determined at 20°C in double-distilled, demineralized water.
[0029] Furthermore, gel formers are preferably suitable which have a structure containing at least one hydrocarbon structural unit having 6 to 20 carbon atoms (preferably at least one carbocyclic, aromatic structural unit) and additionally an organic structural unit covalently bonded to the aforementioned hydrocarbon unit, which has at least two groups selected from -OH, -NH-, or mixtures thereof.
[0030] Particularly preferred gel bodies are characterized in that said gel bodies contain at least one benzylidene alditol compound of the formula (GB-I) as gelling agent wherein
[0031] *- represents a covalent single bond between an oxygen atom of the alditol backbone and the intended radical, n represents 0 or 1, preferably 1, m represents 0 or 1, preferably 1,
[0032] R 1 , R 2 and R 3 independently of one another represents a hydrogen atom, a halogen atom, a C1-C4 alkyl group, a cyano group, a nitro group, an amino group, a carboxyl group, a hydroxy group, a -C(=O)-NH-NH2 group, a -NH-C(=O)-(C2-C4 alkyl) group, a C1-C4 alkoxy group, a C1-C4 alkoxy-C2-C4 alkyl group, two of the radicals together with the residual molecule form a 5- or 6-membered ring,
[0033] R 4 , R 5 and R eindependently of one another represent a hydrogen atom, a halogen atom, a Ci-C4 alkyl group, a cyano group, a nitro group, an amino group, a carboxyl group, a hydroxy group, a -C(=O)-NH-NH2 group, a -NH-C(=O)-(C2-C4 alkyl) group, a Ci-C4 alkoxy group, a Ci-C4 alkoxy-C2-C4 alkyl group, two of the radicals together with the residual molecule form a 5- or 6-membered ring.
[0034] Due to the stereochemistry of the alditols, it should be noted that both the said benzylidene alditols in the L-configuration or in the D-configuration, or a mixture of both, are suitable according to the invention. Due to their natural availability, the benzylidene alditol compounds in the D-configuration are preferably used according to the invention. It has been found to be preferred if the alditol backbone of the benzylidene alditol compound according to formula (GB-I) contained in the shaped body is derived from D-glucitol, D-mannitol, D-arabinitol, D-ribitol, D-xylitol, L-glucitol, L-mannitol, L-arabinitol, L-ribitol, or L-xylitol.
[0035] Particularly preferred are those gel bodies which are characterized in that R 1 , R 2 , R 3 , R 4 , R 5 and R eaccording to the benzylidenealditol compound of the formula (GB-I), independently of one another, represents a hydrogen atom, methyl, ethyl, chlorine, fluorine or methoxy, preferably a hydrogen atom. n according to the benzylidenealditol compound of the formula (GB-I) preferably represents 1. m according to the benzylidenealditol compound of the formula (GB-I) preferably represents 1.
[0036] Most preferably, the gel body contains as benzylidene alditol compound of formula (GB-I) at least one compound of formula (GB-11) where R 1 , R 2 , R 3 , R 4 , R 5 and R e as defined in formula (I). Most preferably, according to formula (GB-11) R 1 , R 2 , R 3 , R 4 , R 5 and R eindependently of one another represent a hydrogen atom, methyl, ethyl, chlorine, fluorine or methoxy, preferably a hydrogen atom. Most preferably, the benzylidene alditol compound of formula (GB-I) is selected from 1,3:2,4-di-O-benzylidene-D-sorbitol; 1,3:2,4-di-O-(p-methylbenzylidene)-D-sorbitol; 1,3:2,4-di-O-(p-chlorobenzylidene)-D-sorbitol; 1,3:2,4-di-O-(2,4-dimethylbenzylidene)-D-sorbitol; 1,3:2,4-di-O-(p-ethylbenzylidene)-D-sorbitol; 1,3:2,4-di-O-(3,4-dimethylbenzylidene)-D-sorbitol or mixtures thereof.
[0037] Preferred gel bodies contain as gelling agent at least one 2,5-diketopiperazine compound of the formula (GB-I I) wherein
[0038] R 1 , R 2 , R 3 and R 4independently of one another represent a hydrogen atom, a hydroxy group, a (Ci-C6) alkyl group, a (C2-C6) alkenyl group, a (C2-C6) acyl group, a (C2-C6) acyloxy group, a (Ci-C6) alkoxy group, an amino group, a (C2-C6) acylamino group, a (Ci-C6) alkylaminocarbonyl group, an aryl group, an aroyl group, an aroyloxy group, an aryloxy group, an aryl-(Ci-C4) alkyloxy group, an aryl-(Ci-C3) alkyl group, a heteroaryl group, a heteroaryl-(Ci-C3) alkyl group, a (C1-C4) hydroxyalkyl group, a (Ci-C4) aminoalkyl group, a carboxy-(Ci-C3) alkyl group, where at least two of the radicals R 1 to R 4 together with the remaining molecule can form a 5 or 6-membered ring,
[0039] R 5represents a hydrogen atom, a linear (Ci to C6) alkyl group, a branched (C3 to C10) alkyl group, a (C3 to C6) cycloalkyl group, a (C2-C6) alkenyl group, a (C2-C6) alkynyl group, a (Ci-C4) hydroxyalkyl group, a (Ci-C4) alkoxy-(Ci-C4) alkyl group, a (C1-C4) acyloxy-(Ci-C4) alkyl group, an aryloxy-(Ci-C4) alkyl group, an O-(aryl-(Ci-C4) alkyl)oxy-(Ci-C4) alkyl group, a (Ci-C4) alkylsulfanyl-(Ci-C4) alkyl group, an aryl group, an aryl-(Ci-C3) alkyl group, a heteroaryl group, a Heteroaryl-(Ci-C3)-alkyl group, a (C1-C4)-hydroxyalkyl group, a (Ci-C4)-aminoalkyl group, an N-(Ci-C4)-alkylamino-(Ci-C4)-alkyl group, an N,N-(Ci-C4)-dialkylamino-(Ci-C4)-alkyl group, an N-(C2-C8)-acylamino-(Ci-C4)-alkyl group, an N-(C2-C8)-acyl-N-(Ci-C4)-alkylamino-(Ci-C4)-alkyl group, an N-(C2-C8)-aroyl-N-(Ci-C4)-alkylamino-(Ci-C4)-alkyl group, an N,N-(C2-C8)-diacylamino-(Ci-C4)-alkyl group,an N-(aryl-(Ci-C4)-alkyl)amino-(Ci-C4)-alkyl group, an N,N-di(aryl-(Ci-C4)-alkyl)amino-(Ci-C4)-alkyl group, a (Ci-C4)-carboxyalkyl group, a (Ci-C4)-alkoxycarbonyl-(Ci-C3)-alkyl group, a (Ci-C4)-acyloxy-(Ci-C3)-alkyl group, a guanidino-(Ci-C3)-alkyl group, an aminocarbonyl-(Ci-C4)-alkyl group, an N-(Ci-C4)-alkylaminocarbonyl-(Ci-C4)-alkyl group, an N,N-di((Ci-C4)-alkyl)aminocarbonyl-(Ci-C4)-alkyl group, an N-(C2-C8)-acylaminocarbonyl-(Ci- C4) alkyl group, an N,N-(C2-C8)-diacylaminocarbonyl-(Ci-C4)-alkyl group, an N-(C2-Cs)-acyl-N-(Ci-C4)-alkylaminocarbonyl-(Ci-C4)-alkyl group, a N-(aryl-(Ci-C4)-alkyl)aminocarbonyl-(Ci-C4)-alkyl group, an N-(aryl-(Ci-C4)-alkyl)-N-(Ci-C6)-alkylaminocarbonyl-(Ci-C4)-alkyl group or one N,N-Di(aryl-(Ci-C4)-alkyl)aminocarbonyl-(Ci-C4)-alkyl group.,
[0040] It is preferred according to the invention if R 3 and R 4according to formula (GB-II) represents a hydrogen atom. It is particularly preferred according to the invention if R 2 , R 3 and R 4 according to formula (GB-II) represents a hydrogen atom. Therefore, very particularly preferred shaped bodies according to the invention contain at least one 2,5-diketopiperazine compound according to formula (GB-IIa) where R 1 and R 5 as defined under formula (GB-II) (vide supra).
[0041] It has been found to be preferable if the residue R 1 according to formula (GB-II) and according to formula (GB-IIa) in the para-position of the phenyl ring. Therefore, for the purposes of the present invention, preferred shaped bodies according to the invention are those which contain at least one 2,5-diketopiperazine compound according to formula (GB-IIb), where R 1 and R 5as previously defined under formula (GB-II) (vide supra). The numbers 3 and 6 positioned on the ring atoms in formula (GB-IIb) merely mark positions 3 and 6 of the diketopiperazine ring for illustrative purposes, as they are generally used within the scope of the invention for the naming of all 2,5-diketopiperazines according to the invention.
[0042] The 2,5-diketopiperazine compounds of formula (GB-II) have chiral centers at least at the carbon atoms of positions 3 and 6 of the 2,5-diketopiperazine ring. The numbering of ring positions 3 and 6 was illustrated by way of example in formula (GB-IIb). The 2,5-diketopiperazine compound of formula (GB-II) of the compositions according to the invention is preferably, based on the stereochemistry of the carbon atoms at positions 3 and 6 of the 2,5-diketopiperazine ring, the configurational isomer 3S,6S, 3R,6S, 3S,6R, 3R,6R or mixtures thereof, particularly preferably 3S,6S.
[0043] Preferred gel bodies contain at least one 2,5-diketopiperazine compound of the formula (GB-II) as a gelling agent, selected from 3-benzyl-6-carboxyethyl-2,5-diketopiperazine, 3-benzyl-6-carboxymethyl-2,5-diketopiperazine, 3-benzyl-6-(p-hydroxybenzyl)-2,5-diketopiperazine, 3-benzyl-6-isopropyl-2,5-diketopiperazine, 3-benzyl-6-(4-aminobutyl)-2,5-diketopiperazine, 3,6-di(benzyl)-2,5-diketopiperazine, 3,6-di(p-hydroxybenzyl)-2,5-diketopiperazine, 3,6-di(p-(benzyloxy)benzyl)-2,5-diketopiperazine, 3-Benzyl-6-(4-imidazolyl)methyl-2,5-diketopiperazine, 3-benzyl-6-methyl-2,5-diketopiperazine, 3-benzyl-6-(2-(benzyloxycarbonyl)ethyl)-2,5-diketopiperazine, or mixtures thereof. Compounds with the aforementioned configurational isomers are preferred for selection.
[0044] It is also possible for the gel bodies according to the invention to contain as gelling agents a) at least one diarylamidocystin compound of the formula (GB-III) wherein
[0045] X + independently represents a hydrogen atom or an equivalent of a cation,
[0046] R 1 , R 2 , R 3 and R 4 independently of one another represent a hydrogen atom, a halogen atom, a C1-C4 alkyl group, a C1-C4 alkoxy group, a C2-C4 hydroxyalkyl group, a hydroxyl group, an amino group, an N-(C1-C4 alkyl)amino group, an N,N-di(C1-C4 alkyl)amino group, an N-(C2-C4 hydroxyalkyl)amino group, an N,N-di(C2-C4 hydroxyalkyl)amino group or R 1 with R 2 or R 3 with R 4 forms a 5- or 6-membered fused ring, which in turn can be substituted by at least one group selected from the group consisting of Ci-C4 alkyl group, Ci-C4 alkoxy group, C2-C4 hydroxyalkyl group, hydroxyl group, amino group, N-(Ci-C4 alkyl)amino group, N,N-di(Ci-C4 alkyl)amino group, N-(C2-C4 hydroxyalkyl)amino group, N,N-di(C2-C4 hydroxyalkyl)amino group.
[0047] Each of the stereocenters contained in the compound of formula (GB-III) can independently represent the L- or D-stereoisomer. According to the invention, it is preferred if said cystine compound of formula (GB-III) is derived from the L-stereoisomer of cysteine. Said gel bodies can contain at least one compound of formula (GB-III) in which R 1 , R 2 , R 3 and R 4 independently of one another represent a hydrogen atom, a halogen atom, a C1-C4 alkyl group, a C1-C4 alkoxy group, a C2-C4 hydroxyalkyl group, a hydroxyl group, or R 1 with R 2 or R 3 with R 4forms a 5- or 6-membered fused ring, which in turn may be substituted by at least one group selected from the group consisting of Ci-C4 alkyl group, Ci-C4 alkoxy group, C2-C4 hydroxyalkyl group, or hydroxyl group. Shaped bodies which are particularly suitable as diarylamidocystine compounds of the formula (GB-III) N,N'-dibenzoylcystine (R 1 = R 2 = R 3 = R 4 = hydrogen atom; X + = independently of one another represent hydrogen atom or an equivalent of a cation), in particular N,N'-dibenzoyl-L-cystine.
[0048] The N-(C8-C24)-hydrocarbylglyconamide compounds suitable as gel formers a) preferably have the formula (GB-IV) where n is 2 to 4, preferably 3 or 4, especially 4;
[0049] R 1is selected from hydrogen, C1-C16 alkyl radicals, C1-C3 hydroxy or methoxyalkyl radicals, preferably C1-C3 alkyl, hydroxyalkyl or methoxyalkyl radicals, particularly preferably methyl;
[0050] R 2 is selected from C8-C24 alkyl radicals, C8-C24 monoalkenyl radicals, C8-C24 dialkenyl radicals, C8-C24 trialkenyl radicals, C8-C24 hydroxyalkyl radicals, C8-C24 hydroxyalkenyl radicals, C1-C3 hydroxyalkyl radicals or methoxy-Ci-Cs alkyl radicals, preferably Cs-Cis alkyl radicals and mixtures thereof, more preferably Cs, C10, C12, C16, C18, C19 and C21 alkyl radicals and mixtures thereof, most preferably C12 and C20 alkyl radicals or a mixture thereof.
[0051] In particularly preferred embodiments, the radical is HO-CH2-(CHOH) n -C- one of a II O
[0052] Glycuronic acid, in particular the glycuronic acid of a hexose (n=4), derived residue. Glucuronic acid is particularly preferred here. R 1is preferably H or a short-chain alkyl radical, especially methyl. R 2 is preferably a long-chain alkyl radical, for example a Cs-Cis alkyl radical.
[0053] Compounds of the formula (GB-IV1) are therefore particularly preferred. where R 2 has the meanings given for formula (GB-IV). In a particularly preferred embodiment, the at least one low-molecular-weight gelling agent of the second flowable gelling agent-containing composition is selected from the group consisting of cyclic dipeptides, cyclic dipeptide derivatives, and dibenzylidene sorbitols. Due to its technical effect, the at least one gelling agent of the second flowable gelling agent-containing composition is particularly preferred to be dibenzylidene sorbitol (DBS).
[0054] In step iii) of the process, the first and second flowable compositions are fed to the dynamic mixer. In one embodiment of the process, the first flowable composition and the second flowable composition are fed to the mold in the same line. This process is characterized by a reduced equipment structure. With this process, a partial mixing of the first and second flowable compositions can already take place in the feed line leading to the mold. The disadvantages of this process are reduced control of the gelation process and, in the event of a production interruption, increased cleaning effort before restarting the production equipment.
[0055] For the latter reasons, it is preferable to feed the first flowable composition and the second flowable composition to the dynamic mixer in separate lines.
[0056] The process according to the invention is particularly suitable for processes in which flowable compositions are mixed in widely differing weight proportions. Thus, in the process according to the invention, the first flowable composition and the second flowable composition are preferably mixed in a weight ratio of 50:1 to 5:1, preferably 35:1 to 8:1.
[0057] For the mixing but also for the further transfer into the forming device, it has proven advantageous if the flowable compositions in the dynamic mixer are subjected to a shear rate of 50 to 5000 s-1, preferably of 80 to 2000 s-1 and in particular of 100 to 1200 s-1.
[0058] The dynamic mixer is preferably selected from the group of rotor-stator mixers. Static-dynamic mixers are particularly preferred.
[0059] Upon exiting the dynamic mixer, the surfactant-containing and gel-forming agent-containing mixture preferably has a temperature above 23°C, particularly preferably a temperature in the range of 23°C to 60°C. The time interval between the exit of the surfactant-containing and gel-forming agent-containing mixture from the dynamic mixer and its entry into the forming device is preferably 1 to 20 seconds, particularly preferably 1 to 10 seconds.
[0060] A number of different devices are suitable as forming devices, for example a rotating forming roller, an extruder or a casting mold.
[0061] When using a forming roller, the mixture is pressed into the indentations of the forming roller by a pressure roller and formed. Excess material can be removed using a scraper, for example. An extraction belt can be used to extrude the mixture from the indentations of the forming roller.
[0062] In an extruder, the mixture is continuously pressed out of a molding opening under pressure. The resulting extruded strand is then cut to length to form individual molded bodies.
[0063] A casting mold is particularly preferred as the forming device. Materials known to those skilled in the art for the manufacture of casting molds are suitable for manufacturing the casting mold, for example, materials from the group of metals, polymers, or rubbers. Materials from the group of silicones have proven particularly suitable for removing the gel body from the mold.
[0064] In step iv) of the process, the mixture is introduced into the forming device, for example, the casting mold. In a preferred embodiment of the process, the surfactant- and gelling agent-containing mixture is introduced into the casting mold by means of an injector.
[0065] The surfactant-containing and gelling agent-containing mixture is preferably introduced into the casting mold at a filling rate of 1 ml / s to 25 ml / s.
[0066] To avoid contamination in the vicinity of the casting mold, particularly in its edge area, it has proven advantageous to lower the injector before introducing the surfactant-containing and gelling agent-containing mixture into the casting mold. The outlet opening of the injector is preferably located above the center of volume of the mold. To assist in filling the casting mold with the surfactant-containing and gelling agent-containing mixture in step v), the injector and the casting mold can be moved relative to each other. Such relative movement can be achieved by moving the injector, moving the mold, or moving both the injector and the mold.
[0067] A technically simple, preferred process variant provides for the injector to be moved within the mold in step v). The movement can occur horizontally, vertically, or both horizontally and vertically within the mold. During a horizontal movement, the injector's direction of movement is parallel to the opening surface of the mold; during a vertical movement, the direction of movement is orthogonal to this surface.
[0068] Alternatively, or in conjunction with the movement of the mixing element, the mold can be moved in step v). A corresponding relative movement can result, for example, from transporting the mold on a conveyor belt or from a vibrating movement of the mold. The mold can also move horizontally, vertically, or both horizontally and vertically. During a horizontal movement, the direction of movement of the mold is parallel to its opening surface; during a vertical movement, the direction of movement is orthogonal to this surface.
[0069] In step vi) of the process, the surfactant- and gel-forming agent-containing mixture solidifies, forming a dimensionally stable gel. To accelerate the solidification process, the surfactant- and gel-forming agent-containing mixture can be cooled in step vi). Cooling preferably takes place under defined climatic conditions, where, in addition to the temperature, the humidity in the process chamber is also controlled and regulated.
[0070] Finally, the dimensionally stable gel body can be removed from the mold.
[0071] For the production of detergent portion units which comprise further components in addition to the gel body, a procedure in which the gel body is combined with a prefabricated molded body is suitable.
[0072] In a first preferred method, the previously described casting mold is partially filled with a prefabricated molded body. The prefabricated molded body preferably covers at least partially, particularly preferably completely, the bottom surface of the mold into which the first and second flowable preparations are introduced in step iv).
[0073] In an alternative procedure, or in conjunction with the procedure described above, a second preferred procedure, the surfactant-containing and gelling agent-containing mixture is covered with a prefabricated molded body before, during, or after solidification in step vi). It is preferred that the surface of the surfactant-containing and gelling agent-containing mixture visible in the mold be completely covered with a prefabricated molded body.
[0074] If the surfactant-containing and gelling agent-containing mixture is introduced into the mold onto a first prefabricated molded body and the side opposite the side covered with the first prefabricated molded body is covered with a second prefabricated molded body, a sandwich-like detergent portion unit is obtained which is particularly advantageous in terms of handling and appearance.
[0075] A particularly preferred process variant for producing a detergent portion unit, comprising a) a dimensionally stable gel body b) two shaped bodies, comprises the steps: i) providing a first flowable surfactant-containing composition; ii) providing a second flowable gel-forming agent-containing composition different from the first flowable composition; iii) continuously feeding the first and second flowable compositions to a dynamic mixer; iv) mixing the first and second flowable compositions by means of the dynamic mixer to form a surfactant-containing and gel-forming agent-containing mixture; v) introducing the surfactant-containing and gel-forming agent-containing mixture into a casting mold whose bottom surface is at least partially covered with a first prefabricated shaped body;vi) covering the side of the surfactant-containing and gelling agent-containing mixture opposite the side covered by the first prefabricated molded body with a second prefabricated molded body; vii) allowing the surfactant-containing and gelling agent-containing mixture to solidify to form a dimensionally stable gel body. viii) shaping the gel body to form a detergent portion unit comprising a gel body and the first and second prefabricated molded bodies;
[0076] Preferred molded bodies fill 5 to 45 vol.%, preferably 10 to 25 vol.% of the mold.
[0077] The molded body can be manufactured in a variety of ways. The use of cast bodies has proven to be a technically simpler method. The production of the molded body by casting processes has the advantage of allowing the production of a wide variety of geometries. The cast bodies are preferably solidified melts. Due to their ease of large-scale production, compressed bodies, especially tablets, are particularly preferred as molded bodies.
[0078] Regardless of the process used for its production, the shaped body preferably has a breaking strength of 50 N to 300 N, in particular 50 N to 150 N. This breaking strength ensures, on the one hand, sufficient stability of the shaped body during production, transport, and handling by the consumer, and, on the other hand, satisfactory dissolution behavior of the shaped body in an aqueous liquor. The hardness of the shaped body is measured by deformation until fracture, whereby the force acts on the side surfaces of the shaped body and the maximum force it can withstand is determined. A tablet testing device from Sotax, for example, is suitable for determining the hardness of the shaped body.
[0079] Preferred molded bodies have a print.
[0080] If the gel body is combined with a molded body as described above, the dimensionally stable gel body, partially covered by a molded body, is finally removed from the mold. The gel body and the molded body are preferably bonded together.
[0081] In a preferred embodiment of the detergent portion units, the shaped body also contributes to the washing and cleaning action. Corresponding detergent portion units comprise a shaped body that, based on its total weight, contains more than 40% by weight, preferably more than 60% by weight, particularly preferably more than 80% by weight of washing or cleaning active ingredient.
[0082] The first group of active washing or cleaning ingredients integrated into the molded body are fragrances. Their incorporation into the molded body ensures a perceptible fragrance experience for the consumer, which cannot be achieved to the same extent when the fragrances are incorporated into the gel body.
[0083] Another group of washing or cleaning-active ingredients preferably incorporated into the coating substance consists of builders, in particular citrates, zeolites, silicates, and carbonates, particularly preferably citrates and zeolites. The weight fraction of these active substances in the total weight of the coating substance is preferably 5 to 60 wt.%, in particular 10 to 50 wt.%. Particularly preferred are coating substances which, based on their total weight, contain 5 to 60 wt.%, in particular 10 to 50 wt.% citrate and / or zeolite. These active substances not only contribute to the intended washing and cleaning action, but, in the case of printing on the molded body surface, also improve the contour sharpness and durability of the printed image.
[0084] For the sharpness of the contours and durability of the printed image, the use of active ingredients from the group of polymeric detergent or cleaning agents, preferably from the group of celluloses and cellulose derivatives and anionic or non-ionic aromatic polyesters, preferably from the group of celluloses, microcrystalline celluloses and carboxymethylcelluloses, and anionic or non-ionic aromatic polyesters, is also advantageous. The weight proportion of these cellulose-based active ingredients to the total weight of the coating substance is preferably 2 to 50% by weight.
[0085] The composition of some preferred detergent portion units can be found in the following tables (data in wt.% based on the total weight of the gel body or the coating substance unless otherwise stated). In summary, this application provides, among other things, the following items:
[0086] 1. A method for producing a detergent portion unit, comprising a) a dimensionally stable gel body, comprising the steps of: i) providing a first flowable surfactant-containing composition; ii) providing a second flowable gel-forming agent-containing composition different from the first flowable composition; iii) continuously feeding the first and second flowable compositions to a dynamic mixer; iv) mixing the first and second flowable compositions by means of the dynamic mixer to form a surfactant-containing and gel-forming agent-containing mixture; v) introducing the surfactant-containing and gel-forming agent-containing mixture into a
[0087] Forming device; vi) allowing the surfactant-containing and gelling agent-containing mixture to solidify to form a dimensionally stable gel body.
[0088] 2. Process according to point 1, wherein the gel body has a weight of 14 g to 42 g, preferably of 18 g to 38 g, in particular of 20 g to 34 g.
[0089] 3. Method according to one of the preceding points, wherein the gel body has a flat bottom whose largest diagonal is greater than the height of the gel body.
[0090] 4. Method according to one of the preceding points, wherein the gel body has a flat underside whose largest diagonal is more than 1.5 times, preferably more than 2 times the height of the gel body.
[0091] 5. Method according to one of the preceding points, wherein the gel body has an oval underside.
[0092] 6. Method according to one of the preceding points, wherein the gel body has an ellipsoidal or round, preferably a round, bottom.
[0093] 7. Method according to one of the preceding points, wherein the gel body has a square bottom, preferably a square bottom with rounded corners.
[0094] 8. The method according to any one of the preceding points, wherein the gel body has a triangular, quadrangular, or hexagonal bottom side. 9. The method according to any one of the preceding points, wherein the gel body has a top side that is plane-parallel to the bottom side.
[0095] 10. Method according to one of the preceding points, wherein the gel body has a bottom side and a top side which have the same geometric shape and wherein the bottom side and the top side have the same surface area.
[0096] 11. Method according to one of the preceding points, wherein the gel body has a bottom side and a top side which have the same geometric shape and wherein the bottom side and the top side have different surface sizes.
[0097] 12. Method according to one of the preceding points, wherein the gel body has a bottom side and a top side which are connected to one another by a cylindrical outer surface.
[0098] 13. Method according to one of the preceding points, wherein the gel body has a bottom side and a top side and the area of the top side is 80 to 100%, preferably 90 to 100% and in particular 98 to 100% of the bottom side.
[0099] 14. Process according to one of the preceding points, wherein the first flowable surfactant-containing composition contains, based on its total weight, 30 to 70 wt.%, preferably 40 to 60 wt.% and in particular 45 to 55 wt.% surfactant.
[0100] 15. Process according to one of the preceding points, wherein the dimensionally stable gel body contains, based on its total weight, 15 to 35 wt.%, preferably 20 to 30 wt.% of an aqueous-organic solvent.
[0101] 16. Process according to one of the preceding points, wherein the second flowable gelling agent-containing composition contains low molecular weight gelling agent with a molar mass of up to 2000 g / mol, wherein its weight proportion of the total weight of the gel body is preferably less than 5 wt.%, preferably 0.1 to 5 wt.%, particularly preferably 0.1 to 2.5 wt.%.
[0102] 17. The method according to any one of the preceding points, wherein the second flowable gelling agent-containing composition contains low molecular weight gelling agent selected from the group of cyclic dipeptides, cyclic dipeptide derivatives and dibenzylidene sorbitols.
[0103] 18. The process according to any one of the preceding points, wherein the second flowable gel-forming composition contains dibenzylidene sorbitol as a low-molecular-weight gel-forming agent. 19. The process according to any one of the preceding points, wherein the second flowable gel-forming composition further contains an organic solvent.
[0104] 20. Process according to one of the preceding points, wherein the second flowable gelling agent-containing composition contains gelling agent and organic solvent in a total weight proportion above 50 wt.%, preferably above 70 wt.% and in particular above 90 wt.%.
[0105] 21. A method according to any one of the preceding items, wherein the first flowable composition and the second flowable composition are fed to the dynamic mixer in separate lines.
[0106] 22. A process according to any one of the preceding points, wherein the first flowable composition and the second flowable composition are mixed in a weight ratio of 50:1 to 5:1, preferably 35:1 to 8:1.
[0107] 23. Process according to one of the preceding points, wherein the flowable compositions are subjected in the dynamic mixer to a shear rate of 50 to 5000 s-1, preferably 80 to 2000 s-1 and in particular 100 to 1200 s-1.
[0108] 24. Method according to one of the preceding points, wherein the dynamic mixer is selected from the group of rotor-stator mixers.
[0109] 25. Method according to one of the preceding points, wherein dynamic mixers are selected from the group of static-dynamic mixers.
[0110] 26. Process according to one of the preceding points, wherein the surfactant-containing and gelling agent-containing mixture has a temperature above 23°C, preferably in the range from 23°C to 60°C, upon exiting the dynamic mixer.
[0111] 27. Method according to one of the preceding points, wherein the time period between the exit of the surfactant-containing and gelling agent-containing mixture from the dynamic mixer and its entry into the forming device is 1 to 20 seconds, preferably 1 to 10 seconds.
[0112] 28. Method according to one of the preceding points, wherein a rotating forming roller is used as the forming device.
[0113] 29. The method according to any one of items 1 to 27, wherein an extruder is used as the forming device. 30. The method according to any one of items 1 to 27, wherein a casting mold is used as the forming device.
[0114] 31. Process according to item 30, wherein the casting mould is made of a material selected from the group consisting of metals, polymers or rubbers.
[0115] 32. Process according to item 31, wherein the casting mould is made of a material from the group of silicones.
[0116] 33. Process according to one of items 30 to 32, wherein the surfactant-containing and gelling agent-containing mixture is introduced into the casting mould by means of an injector.
[0117] 34. Process according to any one of items 30 to 33, wherein the surfactant-containing and gelling agent-containing mixture is introduced into the casting mould at a filling rate of 1 ml / s to 25 ml / s.
[0118] 35. A process according to any one of items 30 to 34, wherein the injector is lowered into the casting mould before the surfactant-containing and gelling agent-containing mixture is introduced.
[0119] 36. Method according to one of items 30 to 35, wherein the outlet opening of the injector is located above the center of volume of the mold.
[0120] 37. Method according to one of items 30 to 36, wherein the surfactant-containing and gelling agent-containing mixture in step v) is filled into a casting mold by means of an injector and the injector and the casting mold are simultaneously moved relative to one another.
[0121] 38. Method according to item 37, wherein the injector and the mold are moved horizontally relative to each other.
[0122] 39. Process according to any one of the preceding points, wherein the surfactant-containing and gelling agent-containing mixture is cooled in step vi).
[0123] 40. Method according to one of the preceding points, wherein the dimensionally stable gel body is formed following step vi).
[0124] 41. The method according to any one of items 30 to 40, wherein the casting mold is partially filled with a prefabricated molded body. 42. The method according to item 41, wherein the bottom surface of the mold, into which the surfactant-containing and gelling agent-containing mixture is introduced in step iv), is at least partially, preferably completely, covered with a prefabricated molded body.
[0125] 43. Process according to one of the preceding points, wherein the surfactant-containing and gelling agent-containing mixture is covered with a prefabricated shaped body before, during or after solidification in step vi).
[0126] 44. Method according to one of the preceding points, wherein the surface of the surfactant-containing and gelling agent-containing mixture is completely covered with a prefabricated shaped body.
[0127] 45. Process according to one of items 41 to 44, wherein the prefabricated shaped body fills 5 to 45 vol.%, preferably 10 to 25 vol.% of the mold.
[0128] 46. Method according to one of items 41 to 45, wherein the shaped body is in the form of a cast body.
[0129] 47. Process according to one of items 41 to 46, wherein the shaped body is in the form of a pressed body, preferably a tablet.
[0130] 48. Method according to one of items 41 to 47, wherein the shaped body has a breaking strength of 30 N to 300 N, preferably of 50 N to 150 N.
[0131] 49. Method according to one of items 41 to 48, wherein the shaped body has a print.
[0132] 50. Process according to any one of items 41 to 49, wherein the dimensionally stable gel body partially covered by a shaped body is removed from the mold following step vi).
[0133] 51. Process according to any one of items 41 to 50, wherein the shaped body contains, based on its total weight, more than 40% by weight, preferably more than 60% by weight, particularly preferably more than 80% by weight of washing or cleaning active ingredient.
[0134] 52. Process according to one of items 41 to 51, wherein the shaped body contains a washing or cleaning active ingredient from the group of fragrances.
[0135] 53. The process according to any one of items 41 to 52, wherein the shaped body contains a washing- or cleaning-active ingredient from the group of builders, in particular at least one active ingredient from the group of citrates, zeolites, silicates, and carbonates, preferably from the group of citrates and zeolites. 54. The process according to any one of items 41 to 53, wherein the shaped body contains a polymeric washing- or cleaning-active ingredient, preferably a polymeric washing- or cleaning-active ingredient from the group of celluloses and cellulose derivatives and anionic or nonionic aromatic polyesters, preferably from the group of celluloses, microcrystalline celluloses, and carboxymethylcelluloses, and anionic or nonionic aromatic polyesters.
[0136] 55. Method according to one of items 41 to 54, wherein the gel body and the shaped body are adhesively bonded to one another.
Claims
Patent claims 1. A method for producing a detergent portion unit, comprising: a) a shape-stable gel body, comprising the steps of: i) providing a first free-flowing surfactant-containing composition; ii) providing a second free-flowing gelling agent-containing composition, different from the first free-flowing composition; iii) continuously feeding the first and second free-flowing compositions to a dynamic mixer; iv) mixing the first and second free-flowing compositions by means of the dynamic mixer to form a surfactant-containing and gelling agent-containing mixture; v) introducing the surfactant-containing and gelling agent-containing mixture into a Forming device; vi) Allowing the surfactant-containing and gelling agent-containing mixture to solidify, forming a dimensionally stable gel body.
2. Method according to claim 1, wherein the gel body has a weight of 14 g to 42 g, preferably 18 g to 38 g, in particular 20 g to 34 g.
3. A method according to any of the preceding claims, wherein the first free-flowing surfactant-containing composition contains, based on its total weight, 30 to 70 wt.%, preferably 40 to 60 wt.% and particularly 45 to 55 wt.% surfactant.
4. A method according to any of the preceding claims, wherein the second flowable gelling agent-containing composition contains a low molecular weight gelling agent with a molar mass of up to 2000 g / mol, wherein the weight fraction of the gelling agent in relation to the total weight of the composition is preferably less than 5 wt.%, preferably 0.1 to 5 wt.%, and particularly preferably 0.1 to 2.5 wt.%.
5. Method according to one of the preceding claims, wherein the second flowable gelling agent-containing composition contains dibenzylidene sorbitol as a low molecular weight gelling agent.
6. Method according to one of the preceding claims, wherein the first flowable composition and the second flowable composition are supplied to the dynamic mixer in separate lines.
7. Method according to one of the preceding claims, wherein the first flowable composition and the second flowable composition are mixed in the dynamic mixer in a weight ratio of 50:1 to 5:1, preferably from 35:1 to 8:
1.
8. Method according to one of the preceding claims, wherein the time interval between the exit of the surfactant-containing and gelling agent-containing mixture from the dynamic mixer and its entry into the forming device is 1 to 20 seconds, preferably 1 to 10 seconds.
9. Method according to one of the preceding claims, wherein a rotating forming roller is used as the forming device.
10. Method according to any one of claims 1 to 8, wherein an extruder is used as the forming device.
Citation Information
Patent Citations
Method for producing gel detergent
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