Method for producing detergents or cleaning agents

Abstract

The invention relates to a method for producing a detergent or cleaning agent, containing, based on the total weight, a) 4 to 40 wt.% of a gelling agent; b) 0.1 to 40 wt.% of a detergent- or cleaning-active ingredient; and c) 30 to 90 wt% of an organic solvent, having the steps of: i) providing the organic solvent at a temperature T1 above 10°C, ii) providing a first gelling agent preparation and introducing the first gelling agent preparation into the organic solvent; and iii) providing a second gelling agent preparation which differs from the first gelling agent preparation and introducing the second gelling agent preparation into the organic solvent, wherein the detergent- or cleaning-active ingredient is introduced into the organic solvent after step i), thereby forming a detergent- and cleaning-active composition.

Description

[0001] Manufacturing process for washing or cleaning agents'

[0002] The present invention relates to a process for producing detergents or cleaning agents. In particular, the application relates to a multi-stage production process in which gelling agents are dosed into a liquid mixture at a time lag.

[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 solution is pre-portioned detergents and cleaning agents, for example, foil pouches with one or more compartments for solid or liquid compositions. From a technical perspective, a key focus is on the development and production of liquid or gel detergents suitable for packaging in water-soluble foil pouches.

[0004] To be commercially successful, a detergent or cleaning agent portion unit must meet consumer interests in the best possible way. A key means of communicating product quality and product promise is the appearance of a portion unit, including shape, color, and transparency. This applies in particular to water-soluble film pouches, whose soluble films are generally transparent and reveal the solid or liquid detergent or cleaning agent contained within. While clear, i.e. non-white, liquid detergents can be easily obtained by adding appropriate dyes, the provision of white or cloudy liquid detergents or detergent or cleaning agent gels is more challenging because the opacifiers used in their production are increasingly being viewed critically from an ecological perspective.Against this background, the provision of an ecologically acceptable opacifier is a relevant development goal in the field of liquid detergents or cleaning agents.

[0005] The production of liquid detergents or cleaning agents typically involves a sequential process in which the detergent ingredients are mixed together in a timed sequence. To achieve a homogeneous end product, the respective intermediates and the final product are mixed with energy input. The final product is characterized not only by the most homogeneous distribution of active ingredients possible, but also by rheological properties suitable for handling by the consumer.The type and timing of adjustment of these rheological properties during the manufacturing process influences the efficiency of the process as well as the final product quality, as the rheological properties of the intermediate and final products are closely related to the energy input required for homogenization during production and the mechanical stress on the intermediate and final products and their components.

[0006] Another characteristic of efficient manufacturing processes for detergent or cleaning agent portion units is the volume of returns and waste generated in these processes and the potential for their recycling. Returns include portion units with insufficient fill levels or poor appearance, for example, and waste generated, for example, as offcuts from packaging the portion units in water-soluble film bags.

[0007] Processes for the reuse of detergents from water-soluble film bags are described, for example, in European patents EP 1 462 513 B1, EP 2 941 479 B1 and EP 3 037 512 B1.

[0008] The object of the present application was to provide an efficient process for the production of gel-like washing or cleaning agents, whereby the process products should be characterized by good solubility as well as an appealing feel and appearance.

[0009] To achieve this object, there is provided a process for producing a washing or cleaning agent containing, based on its total weight, a) 4 to 40% by weight of gelling agent; b) 0.1 to 40% by weight of washing or cleaning active ingredient; c) 30 to 90% by weight of organic solvent; comprising the steps: i) providing the organic solvent having a temperature Ti above 10°C, ii) providing a first gelling agent preparation and introducing the first gelling agent preparation into the organic solvent; iii) providing a second gelling agent preparation different from the first gelling agent preparation and introducing the second gelling agent preparation into the organic solvent, wherein the washing or cleaning active ingredient is introduced into the organic solvent following step i) to form a washing and cleaning active composition.

[0010] The process according to the invention is used to produce detergents or cleaning agents. The liquefaction point of the detergents or cleaning agents is preferably above 80°C (1013 mbar), particularly preferably above 100°C (1013 mbar), and in particular above 115°C (1013 mbar).

[0011] The rheological properties of the washing or cleaning agent are influenced, among other ingredients, in particular by the gelling agent it contains. In preferred washing or cleaning agents, the weight fraction of the gelling agent in the total weight is 6 to 30 wt.%, preferably 7 to 24 wt.%, and especially 8 to 22 wt.%. Preferred gelling agents are selected from the group of polymeric gelling agents, preferably from the group of optionally acetalized polyvinyl alcohol, gelatin, and xanthan gum, or mixtures thereof. The use of optionally acetalized polyvinyl alcohol is very particularly preferred.

[0012] Preferably, the gelling agent from the first gelling agent preparation and the gelling agent from the second gelling agent preparation are selected from the group of polymeric gelling agents, preferably from the group of optionally acetalised polyvinyl alcohol, gelatin and xanthan or mixtures thereof, very particularly preferably from the group of optionally acetalised polyvinyl alcohols.

[0013] Preferred gel formers are preferably based on a polyvinyl alcohol or a polyvinyl alcohol copolymer whose molecular weight is in the range of 10,000 to 1,000,000 gmol -1 , preferably from 20,000 to 500,000 gmol -1 , particularly preferably from 30,000 to 100,000 gmol -1 and especially from 40,000 to 80,000 gmol -1 lies.

[0014] The production of polyvinyl alcohol and polyvinyl alcohol copolymers generally involves the hydrolysis of intermediate polyvinyl acetate. Preferred polyvinyl alcohols and polyvinyl alcohol copolymers have a degree of hydrolysis of 70 to 100 mol%, preferably 80 to 90 mol%, particularly preferably 81 to 89 mol%, and especially 82 to 88 mol%.

[0015] Preferred polyvinyl alcohol copolymers comprise, in addition to vinyl alcohol, an ethylenically unsaturated carboxylic acid, its salt, or its ester. Particularly preferably, such polyvinyl alcohol copolymers contain, in addition to vinyl alcohol, sulfonic acids such as 2-acrylamido-2-methyl-1-propanesulfonic acid (AMPS), acrylic acid, methacrylic acid, acrylic esters, methacrylic esters, or mixtures thereof; among the esters, C1-4 alkyl esters or hydroxyalkyl esters are preferred. Other suitable monomers include ethylenically unsaturated dicarboxylic acids, for example, itaconic acid, maleic acid, fumaric acid, and mixtures thereof.

[0016] The gelling agent is preferably selected from the group of hydrolyzed polyvinyl alcohol homopolymers and polyvinyl alcohol copolymers having a molecular weight of 30,000 to 60,000 g / mol.

[0017] As a second optional ingredient, the washing or cleaning agent contains a washing or cleaning active ingredient. The weight fraction of the washing or cleaning active ingredient in the total weight of the washing or cleaning agent is preferably 1 to 35 wt.%, preferably 5 to 30 wt.%, and in particular 10 to 25 wt.%.

[0018] Even if the selection of the washing or cleaning active ingredient is not subject to any significant restriction, washing or cleaning active ingredients selected from the group of washing or cleaning active polymers, surfactants, corrosion inhibitors and mixtures thereof are preferred because of their ease of processing in the washing or cleaning agent.

[0019] The group of washing or cleaning-active polymers includes, in particular, polycarboxylates. The washing or cleaning-active agent is preferably selected from the group of polycarboxylates, in particular the copolymer polyacrylates, particularly preferably the copolymer polyacrylates containing sulfonic acid groups.

[0020] The copolymers can have two, three, four, or more different monomer units. Preferred copolymeric polysulfonates contain, in addition to monomer(s) containing sulfonic acid groups, at least one monomer from the group of unsaturated carboxylic acids.

[0021] As unsaturated carboxylic acid(s), particularly preferred unsaturated carboxylic acids are those of the formula R 1 (R 2 )C=C(R 3 )COOH is used, in the R 1 to R 3independently of one another represent -H, -CH3, a straight-chain or branched saturated alkyl radical having 2 to 12 carbon atoms, a straight-chain or branched, mono- or polyunsaturated alkenyl radical having 2 to 12 carbon atoms, alkyl or alkenyl radicals substituted by -NH2, -OH or -COOH as defined above or -COOH or -COOR 4 where R 4 a saturated or unsaturated, straight-chain or branched hydrocarbon radical having 1 to 12 carbon atoms.

[0022] Particularly preferred unsaturated carboxylic acids are acrylic acid, methacrylic acid, ethacrylic acid, α-chloroacrylic acid, α-cyanoacrylic acid, crotonic acid, α-phenylacrylic acid, maleic acid, maleic anhydride, fumaric acid, itaconic acid, citraconic acid, methylenemalonic acid, sorbic acid, cinnamic acid, or mixtures thereof. Unsaturated dicarboxylic acids can, of course, also be used.

[0023] The monomers containing sulfonic acid groups are those of the formula R 5 (R e )C=C(R 7 )-X-SO3H is preferred, in which R 5 to R 7 independently of one another represent -H, -CH3, a straight-chain or branched saturated alkyl radical having 2 to 12 carbon atoms, a straight-chain or branched, mono- or polyunsaturated alkenyl radical having 2 to 12 carbon atoms, alkyl or alkenyl radicals substituted by -NH2, -OH or -COOH or -COOH or -COOR 4 where R 4 is a saturated or unsaturated, straight-chain or branched hydrocarbon radical having 1 to 12 carbon atoms, and X represents an optionally present spacer group selected from -(CH2)n- where n = 0 to 4, -COO-(CH2)k- where k = 1 to 6, -C(O)-NH-C(CH3)2-, -C(O)-NH-C(CH3)2-CH2- and -C(O)-NH-CH(CH3)-CH2-

[0024] Preferred monomers are those of the formulas

[0025] H2C=CH-X-SO3H, H2C=C(CH3)-X-SO3H 0der HO3S-X-(R 8 )C=C(R 7 )-X-SO3H, in which R e and R 7are independently selected from -H, -CH3, -CH2CH3, -CH2CH2CH3 and -CH(CH3)2 and X represents an optionally present spacer group selected from -(CH2)n- with n = 0 to 4, -COO-(CH2)k- with k = 1 to 6, -C(O)-NH-C(CH3)2-, -C(O)-NH-C(CH3)2-CH2- and -C(O)-NH- CH(CH3)-CH2-. Particularly preferred monomers containing sulfonic acid groups are 1-acrylamido-1-propanesulfonic acid, 2-acrylamido-2-propanesulfonic acid, 2-acrylamido-2-methyl-1-propanesulfonic acid, 2-methacrylamido-2-methyl-1-propanesulfonic acid, 3-methacrylamido-2-hydroxypropanesulfonic acid, allylsulfonic acid, methallylsulfonic acid, allyloxybenzenesulfonic acid, methallyloxybenzenesulfonic acid, 2-hydroxy-3-(2-propenyloxy)propanesulfonic acid, 2-methyl-2-propen1-sulfonic acid, styrenesulfonic acid, vinylsulfonic acid, 3-sulfopropyl acrylate, 3-sulfopropyl methacrylate, sulfomethacrylamide, sulfomethylmethacrylamide and mixtures of the acids mentioned or their water-soluble salts.In the polymers, the sulfonic acid groups can be present in fully or partially neutralized form, meaning that the acidic hydrogen atom of the sulfonic acid group in some or all of the sulfonic acid groups can be exchanged for metal ions, preferably alkali metal ions and especially sodium ions. The use of partially or fully neutralized copolymers containing sulfonic acid groups is preferred according to the invention.

[0026] The monomer distribution of the copolymers preferably used according to the invention is preferably 5 to 95 wt.% in copolymers containing only carboxylic acid group-containing monomers and sulfonic acid group-containing monomers, particularly preferably 50 to 90 wt.% and 10 to 50 wt.% in monomers containing carboxylic acid groups, the monomers being preferably selected from those mentioned above. The molar mass of the sulfo-copolymers preferably used according to the invention can be varied in order to adapt the properties of the polymers to the desired application. Preferred cleaning agents are characterized in that the copolymers have molar masses of 2000 to 200,000 g mol -1 , preferably from 4000 to 25,000 g mol -1 and in particular from 5000 to 15,000 g mol -1 have.

[0027] In a further preferred embodiment, the copolymers comprise, in addition to the carboxyl-containing monomer and the sulfonic acid-containing monomer, at least one nonionic, preferably hydrophobic monomer. The use of these hydrophobically modified polymers has been shown to improve, in particular, the rinse performance of dishwashing detergents according to the invention.

[0028] Particularly preferably, the at least one second phase further comprises an anionic copolymer, wherein the anionic copolymer used is a copolymer comprising i) monomers containing carboxylic acid groups, ii) monomers containing sulfonic acid groups, iii) non-ionic monomers, in particular hydrophobic monomers.

[0029] As non-ionic monomers, monomers of the general formula

[0030] R 1 (R 2 )C=C(R 3 )-XR 4 used in the R 1 to R 3independently represents -H, -CH3 or -C2H5, X represents an optionally present spacer group selected from -CH2-, -C(O)O- and -C(O)-NH-, and R 4 represents a straight-chain or branched saturated alkyl radical having 2 to 22 carbon atoms or an unsaturated, preferably aromatic radical having 6 to 22 carbon atoms.

[0031] Particularly preferred non-ionic monomers are butene, isobutene, pentene, 3-methylbutene, 2-methylbutene, cyclopentene, hexene, hexene-1, 2-methylpentene-1, 3-methylpentene-1, cyclohexene, methylcyclopentene, cycloheptene, methylcyclohexene, 2,4,4-trimethylpentene-1, 2,4,4-trimethylpentene-2,2,3-dimethylhexene-1, 2,4-dimethylhexene-1, 2,5-dimethylhexene-1, 3,5-dimethylhexene-1, 4,4-dimethylhexane-1, ethylcyclohexyne, 1-octene, a-olefins having 10 or more carbon atoms such as 1-decene, 1-dodecene, 1-Hexadecene, 1-Octadecene and C22- a-olefin, 2-styrene, a-methylstyrene, 3-methylstyrene, 4-propylstyrene, 4-cyclohexylstyrene, 4-dodecylstyrene, 2-ethyl-4-benzylstyrene, 1-vinylnaphthalene, 2-vinylnaphthalene, methyl acrylate, ethyl acrylate,

[0032] Acrylic acid propyl ester, acrylate butyl ester, acrylate pentyl ester, acrylate hexyl ester, methacrylate methyl ester, A / -(methyl)acrylamide, acrylate 2-ethylhexyl ester, methacrylate 2-ethylhexyl ester, A / -(2-ethylhexyl)acrylamide, acrylate octyl ester, methacrylate octyl ester, N-(octyl)acrylamide, acrylate lauryl ester, methacrylate lauryl ester, A / -(lauryl)acrylamide, acrylate stearyl ester, methacrylate stearyl ester, A / -(stearyl)acrylamide, acrylate behenyl ester, methacrylate behenyl ester and A / -(behenyl)acrylamide or mixtures thereof, in particular acrylic acid, ethyl acrylate, 2-acrylamido-2-methylpropanesulfonic acid (AMPS) and mixtures thereof.

[0033] The weight proportion of the washing or cleaning active ingredient from the group of polycarboxylates, in particular the copolymer polyacrylates, particularly preferably the copolymer polyacrylates containing sulfonic acid groups, in the total weight of the washing or cleaning agent is preferably 1 to 18 wt.%, preferably 2 to 16 wt.% and in particular 4 to 14 wt.%.

[0034] Another group of preferred washing or cleaning active ingredients consists of nonionic surfactants, preferably nonionic surfactants with a melting point above 30°C, particularly preferably in the range of 40 to 60°C. The melting point of the surfactant (in °C) is determined using differential scanning calorimetry (DSC) according to ISO standard 11357. For the purposes of the invention, the melting point is considered to be the peak temperature determined by DSC in the second heating run. This is the temperature at which the apex / maximum deflection (on the y-axis) in the DSC diagram is present. If multiple peaks—within 5% of the maximum deflection observed in the second heating run—are present in a surfactant (commercial product), the temperature of the first peak is considered the melting point according to the invention.

[0035] Suitable surfactants are in particular linear, saturated fatty acid alcohol ethoxylates with 14 to 18 C atoms in the alkyl chain and 10 to 100 ethylene oxide units, which are preferably not end-capped.

[0036] Further preferred nonionic surfactants are ethoxylated monohydroxyalkanols or alkylphenols, which additionally contain polyoxyethylene-polyoxypropylene block copolymer units. The alcohol or alkylphenol moiety of such nonionic surfactant molecules preferably makes up more than 30 wt.%, particularly preferably more than 50 wt.%, and especially more than 70 wt.% of the total molar mass of such nonionic surfactants. Preferred agents are characterized by containing ethoxylated and propoxylated nonionic surfactants in which the propylene oxide units in the molecule make up up to 25 wt.%, preferably up to 20 wt.%, and especially up to 15 wt.% of the total molar mass of the nonionic surfactant.

[0037] Preferably, the washing or cleaning active ingredient is selected from the group of non-ionic surfactants of the formula (I)

[0038] R 1 O[CH2CH(CH3)O]x[CH2CH2O]y[CH2CH(CH3)O]zR 2 in the

[0039] R 1 represents a linear or branched aliphatic hydrocarbon radical having 4 to 22 carbon atoms,

[0040] R 2 denotes a preferably hydroylated linear or branched hydrocarbon radical having 2 to 26 carbon atoms, x and z are values ​​from 0 to 40 and y is a value of at least 15.

[0041] In a further preferred embodiment, the washing or cleaning active ingredient is selected from the group of non-ionic surfactants of the formula (II)

[0042] R 1 O[CH2CH2O]yR 2 in the

[0043] R 1represents a linear or branched aliphatic hydrocarbon radical having 4 to 22 carbon atoms,

[0044] R 2 denotes a preferably hydroxylated, linear or branched hydrocarbon radical having 2 to 26 carbon atoms, y stands for a value of 15 to 120, preferably 20 to 100 and in particular 35 to 85.

[0045] Preferred classes of such surfactants have as R 1 or R 2 independently of one another in the alkyl chain have 6 to 20, preferably 8 to 14, carbon atoms, and comprise 40 to 150, preferably 40 to 80 alkoxyl units, preferably ethylene oxide (EO) and / or propylene oxide (PO) units, in particular ethylene oxide units. Particularly preferred surfactants of the formula (II) are those in which R 1 represents a linear or branched aliphatic hydrocarbon radical having 8 to 14 carbon atoms, R 2a linear or branched hydrocarbon radical having 8 to 20 carbon atoms and having 40 to 80 ethylene oxide units.

[0046] The nonionic surfactants described above have a particularly advantageous effect on the processability, for example, the dosability or the setting behavior of the detergents or cleaning agents. Based on their total weight, preferred detergents or cleaning agents contain the nonionic surfactant in amounts of 0.5 to 15 wt.%, preferably 2 to 12 wt.%, and in particular 4 to 10 wt.%.

[0047] As a further preferred washing or cleaning active ingredient, preferred washing or cleaning agents contain a washing or cleaning active ingredient from the group of glass corrosion inhibitors, preferably the water-soluble zinc salts, particularly preferably zinc sulfate and zinc acetate, in particular zinc acetate.

[0048] The weight proportion of the glass corrosion inhibitor in the total weight of the washing or cleaning agent is preferably 0.05 to 3 wt.%, preferably 0.1 to 2.4 wt.% and in particular 0.21 to 1 wt.%.

[0049] The washing or cleaning agents preferably further contain a consistency regulator from the group of polyethylene glycols, preferably from the group of polyethylene glycols with an average molecular weight of 200 to 600 g / mol, preferably from the group of polyethylene glycols with an average molecular weight of 300 to 500 g / mol. The weight fraction of the consistency regulator in the total weight of the washing or cleaning agent is preferably 5 to 30 wt.%, preferably 8 to 26 wt.%, and in particular 10 to 22 wt.%.

[0050] As in the case of the non-ionic surfactants described above, the use of the consistency regulator has proven advantageous with regard to processability, for example dosability or setting behavior of the washing or cleaning agents.

[0051] The third essential component of the washing or cleaning agent is an organic solvent. The proportion of the organic solvent in the total weight of the washing or cleaning agent is preferably 35 to 80 wt.% and in particular 40 to 70 wt.%.

[0052] The use of organic solvents from the group of polyhydric alcohols has proven to be particularly advantageous for processability and setting behavior.

[0053] Polyhydric alcohols, within the meaning of the present invention, are hydrocarbons in which two, three, or more hydrogen atoms are replaced by OH groups. The OH groups are bonded to different carbon atoms. No carbon atom contains two OH groups.

[0054] Particularly preferably, the at least one gel phase comprises at least one alkanetriol and / or at least one alkanediol, in particular at least one C3- to C10-alkanetriol and / or at least one C3- to C10-alkanediol, preferably at least one C3- to C8-alkanetriol and / or at least one C3- to C8-alkanediol, in particular at least one C3- to C9-alkanetriol and / or at least one C3- to C5-alkanediol as polyhydric alcohol. The combination of a C9- to C10-alkanediol with a C3- to C10-alkanetriol is particularly preferred. The use of an organic solvent selected from the group consisting of 1,3-propanediol and glycerol is very particularly preferred.

[0055] Preferred washing or cleaning agents contain, based on their total weight, water in an amount by weight below 5% by weight, preferably below 2% by weight and in particular below 0.5% by weight.

[0056] The composition of the basic formulation of a washing or cleaning agent produced using the process can be found in the table below.

[0057] In step i) of the process, organic solvent is provided with a temperature Ti above 10°C. It has been found to be advantageous for the process duration and the properties of the process product if the organic solvent provided in step i) has a temperature Ti above 40°C, preferably above 60°C and in particular in the range from 70 to 120°C.

[0058] It is further advantageous for the process if the organic solvent provided in step i) comprises a consistency regulator from the group of polyethylene glycols, preferably from the group of polyethylene glycols with an average molecular weight of 200 to 600 g / mol, preferably from the group of polyethylene glycols with an average molecular weight of 300 to 500 g / mol.

[0059] The weight proportion of the consistency agent in the total weight of the organic solvent provided in step i) is preferably 5 to 30 wt.%, in particular 10 to 25 wt.%.

[0060] The washing or cleaning agent is introduced after step i). The washing or cleaning agent introduced can be in liquid or solid form. However, in view of the desired solidification of the washing or cleaning agent in the subsequent course of the process, it is preferred if the washing or cleaning agent is introduced in solid form or at least in a partially solid form.

[0061] The washing or cleaning active ingredient can be added in one step (as a total amount) or stepwise (in partial amounts). The addition takes place after step i), i.e., for example, after step i) and before step ii), at the same time as step ii), after step ii) and before step iii), at the same time as step iii), or after step iii). It is particularly preferred to add the washing or cleaning active ingredient after step i) and before step ii) or after step ii).

[0062] In step ii) of the process, the first gelling agent preparation is prepared and introduced into the organic solvent prepared in step i). In the first gelling agent preparation, the gelling agent can be in solid form, for example, as a powder, or in liquid form, for example, as a solution or dispersion.

[0063] A first preferred process variant comprises the steps of i) providing the organic solvent having a temperature Ti above 10°C, ii) providing a first solid gelling agent preparation and introducing the first gelling agent preparation into the organic solvent; iii) providing a second liquid gelling agent preparation different from the first gelling agent preparation and introducing the second gelling agent preparation into the organic solvent, wherein the washing or cleaning active ingredient is introduced into the organic solvent following step i) to form a washing and cleaning composition.

[0064] A second preferred process variant comprises the steps of i) providing the organic solvent having a temperature Ti above 10°C, ii) providing a first liquid gelling agent preparation and introducing the first gelling agent preparation into the organic solvent; iii) providing a second solid gelling agent preparation different from the first gelling agent preparation and introducing the second gelling agent preparation into the organic solvent, wherein the washing or cleaning-active ingredient is introduced into the organic solvent following step i) to form a washing and cleaning-active composition.

[0065] The process utilizes a solid gelling agent preparation. A preferred solid gelling agent preparation has a particle size distribution in which at least 70% by weight of the particles, preferably at least 80% by weight of the particles, have a particle size below 1000 μm, preferably below 800 μm, and in particular below 200 μm. This particle size distribution has proven particularly advantageous with regard to the homogeneous incorporation of the gelling agent into the organic solvent.

[0066] Preferably, the solid gelling agent preparation which is introduced into the organic solvent has, based on its total weight, a weight fraction of gelling agent above 60 wt.%, preferably above 80 wt.% and in particular in the range from 85 to 99 wt.%.

[0067] In addition to the solid gelling agent preparation, a liquid gelling agent preparation is also used in the process. It is particularly preferred to introduce the liquid gelling agent preparation into the organic solvent in the form of a solution or a dispersion of the gelling agent in an organic solvent.

[0068] If the liquid gelling agent preparation is in the form of a dispersion, it preferably contains the gelling agent in the form of particles with a maximum dimension of 2 to 100 mm, preferably 5 to 60 mm, and especially 10 to 30 mm. The use of film particles is particularly preferred.

[0069] The incorporation of particles, such as film particles, of the aforementioned dimensions has proven particularly advantageous in achieving a transparent, opacified appearance. Surprisingly, this appearance can be achieved using the described process without the use of additional opacifiers.

[0070] If the liquid gelling agent preparation is in the form of a solution, the solution of the gelling agent has a temperature of 30 to 120°C, preferably 50 to 110°C and in particular 70 to 100°C when introduced into the organic solvent provided in step i).

[0071] The weight proportion of the gelling agent in the total weight of the liquid gelling agent preparation is preferably 1 to 20 wt.%, more preferably 2 to 15 wt.% and in particular 4 to 12 wt.%.

[0072] The weight ratio of the gelling agent introduced by means of a solid gelling agent preparation to the gelling agent introduced by means of a liquid gelling agent preparation is preferably in the range from 1000:1 to 20:1, preferably 800:1 to 40:1 and in particular 600:1 to 60:1.

[0073] While process step i) precedes the other process steps, process steps ii) and iii) can be carried out sequentially or simultaneously. With regard to the process duration, the required energy input, and the properties of the process product, it has proven advantageous to carry out steps ii) and iii) sequentially.

[0074] To reduce process complexity and improve control of the process products, it is advantageous to introduce the same gelling agent into the liquid washing or cleaning agent mixture in both steps ii) and iii). "Same" refers to gelling agents that have the same functional groups. It has proven particularly advantageous to incorporate gelling agents from the group of polyvinyl alcohols in steps ii) and iii).

[0075] To accelerate the process, the temperature of the organic solvent can be heated to a temperature T2 above the temperature Ti after introduction of the first gelling agent preparation in step ii) or after introduction of the second gelling agent preparation in step iii) or after introduction of washing or cleaning active ingredient, wherein the temperature difference between T2 and Ti is preferably at least 20°C, preferably at least 25°C and in particular at least 30°C.

[0076] Preferably, the gelling agent-containing organic solvent is stirred for a period ti of 0.5 to 12 hours, preferably 1 to 6 hours, and in particular 1 to 3 hours, following step ii) or after introducing the second gelling agent preparation in step iii) or after introducing the washing or cleaning agent. In preferred process variants, the gelling agent-containing organic solvent has a temperature above the temperature Ti during the period ti, wherein the temperature difference between T2 and Ti is preferably at least 15°C, preferably at least 20°C, and in particular at least 40°C.

[0077] To improve the product appearance, a dye can be introduced into the liquid washing or cleaning preparation in a further step iv) following step iii).

[0078] The process is preferably carried out discontinuously, for example, in a stirred tank. The quantities provided by the process are naturally higher than those required for a single washing or cleaning cycle. In a preferred process variant, the liquid washing or cleaning preparation is portioned in a further step v) following step iii). For this purpose, the liquid washing or cleaning preparation is poured, for example, into a trough or into a receiving chamber obtained by deforming a water-soluble film following step iii), preferably following step iv), in a further step v).

[0079] Preferably, the liquid washing or cleaning-active preparation solidifies after step iii), preferably after step v) upon cooling to form a gel-like body.

[0080] This registration provides, among other things, the following items:

[0081] 1. A process for producing a washing or cleaning agent containing, based on its total weight a) 4 to 40 wt. % gelling agent; b) 0.1 to 40 wt. % washing or cleaning active ingredient; c) 30 to 90 wt. % organic solvent; comprising the steps: i) providing the organic solvent having a temperature Ti above 10°C, ii) providing a first gelling agent preparation and introducing the first gelling agent preparation into the organic solvent; iii) providing a second gelling agent preparation different from the first gelling agent preparation and introducing the second gelling agent preparation into the organic solvent, wherein the washing or cleaning active ingredient is introduced into the organic solvent following step i) to form a washing and cleaning active composition.

[0082] 2. Process according to point 1, wherein the weight proportion of the gelling agent in the total weight of the washing or cleaning agent is 6 to 30 wt.%, preferably 7 to 24 wt.% and in particular 8 to 22 wt.%.

[0083] 3. Method according to one of the preceding points, wherein the gelling agent, preferably the gelling agent from the first gelling agent preparation and the gelling agent from the second gelling agent preparation, is selected from the group of polymeric gelling agents, preferably from the group of polyvinyl alcohol, gelatin and xanthan or mixtures thereof.

[0084] 4. Process according to one of the preceding points, wherein the gelling agent is selected from the group of hydrolyzed polyvinyl alcohol homopolymers and polyvinyl alcohol copolymers having a molecular weight of 30,000 to 60,000 g / mol.

[0085] 5. Process according to one of the preceding points, wherein the weight proportion of the washing or cleaning active ingredient in the total weight of the washing or cleaning agent is 1 to 35 wt.%, preferably 5 to 30 wt.% and in particular 10 to 25 wt.%.

[0086] 6. Process according to one of the preceding points, wherein the washing or cleaning active ingredient is selected from the group of washing or cleaning active polymers, surfactants, corrosion inhibitors and mixtures thereof.

[0087] 7. Process according to one of the preceding points, wherein the washing or cleaning active ingredient is selected from the group of polycarboxylates, in particular the copolymer polyacrylates, particularly preferably the copolymer polyacrylates containing sulfonic acid groups.

[0088] 8. The process according to item 7, wherein the weight fraction of the washing or cleaning active ingredient from the group of polycarboxylates in the total weight of the washing or cleaning agent is 1 to 18 wt.%, preferably 2 to 16 wt.%, and in particular 4 to 14 wt.%. 9. The process according to any one of the preceding items, wherein the washing or cleaning active ingredient is selected from the group of nonionic surfactants, preferably nonionic surfactants with a melting point above 30°C, preferably in the range from 40 to 60°C.

[0089] 10. Process according to one of the preceding points, wherein the washing or cleaning active ingredient is selected from the group of non-ionic surfactants of the formula (I)

[0090] R 1 O[CH2CH(CH3)O]x[CH2CH2O]y[CH2CH(CH3)O]zR 2 in the

[0091] R 1 represents a linear or branched aliphatic hydrocarbon radical having 4 to 22 carbon atoms,

[0092] R 2 denotes a preferably hydroxylated, linear or branched hydrocarbon radical having 2 to 26 carbon atoms, x and z are values ​​from 0 to 40 and y is a value of at least 15.

[0093] 11. Process according to one of the preceding points, wherein the washing or cleaning active ingredient is selected from the group of non-ionic surfactants of the formula (II)

[0094] R 1 O[CH2CH2O]yR 2 in the

[0095] R 1 represents a linear or branched aliphatic hydrocarbon radical having 4 to 22 carbon atoms,

[0096] R 2 denotes a preferably hydroxylated, linear or branched hydrocarbon radical having 2 to 26 carbon atoms, y represents a value from 15 to 120, preferably 20 to 100 and in particular 35 to 85.

[0097] 12. Process according to one of points 9 to 11, wherein the weight proportion of the non-ionic surfactant in the total weight of the washing or cleaning agent is 0.5 to 15 wt.%, preferably 2 to 12 wt.%, and in particular 4 to 10 wt.%.

[0098] 13. Process according to one of the preceding points, wherein the washing or cleaning active ingredient is selected from the group of glass corrosion inhibitors, preferably water-soluble zinc salts, particularly preferably zinc sulfate and zinc acetate, in particular zinc acetate.

[0099] 14. Process according to item 13, wherein the weight proportion of the glass corrosion inhibitor in the total weight of the washing or cleaning agent is 0.05 to 3 wt.%, preferably 0.1 to 2.4 wt.% and in particular 0.21 to 1 wt.%.

[0100] 15. The process according to any one of the preceding points, wherein the washing or cleaning agent further contains a consistency regulator from the group of polyethylene glycols, preferably from the group of polyethylene glycols with an average molecular weight of 200 to 600 g / mol, more preferably from the group of polyethylene glycols with an average molecular weight of 300 to 500 g / mol. 16. The process according to point 15, wherein the weight fraction of the consistency regulator in the total weight of the washing or cleaning agent is 5 to 30 wt.%, preferably 8 to 26 wt.%, and in particular 10 to 22 wt.%.

[0101] 17. Process according to one of the preceding points, wherein the weight proportion of the organic solvent in the total weight of the washing or cleaning agent is 35 to 80 wt.%, preferably 40 to 70 wt.%.

[0102] 18. Process according to one of the preceding points, wherein the organic solvent is selected from the group of polyhydric alcohols.

[0103] 19. A process according to any one of the preceding items, wherein the organic solvent comprises a C3 to C10 alkanediol and a C3 to C10 alkanetriol.

[0104] 20. Process according to one of the preceding points, wherein the organic solvent is selected from the group 1,3-propanediol and glycerol.

[0105] 21. Method according to one of the preceding points, wherein the washing or cleaning agent, based on its total weight, contains water in an amount by weight below 5 wt.%, preferably below 2 wt.% and in particular below 0.5 wt.%.

[0106] 22. Process according to one of the preceding points, wherein the organic solvent provided in step i) has a temperature Ti above 40°C, preferably above 60°C and in particular in the range from 70 to 120°C.

[0107] 23. Process according to one of the preceding points, wherein the organic solvent provided in step i) comprises a consistency regulator from the group of polyethylene glycols, preferably from the group of polyethylene glycols with an average molecular weight of 200 to 600 g / mol, preferably from the group of polyethylene glycols with an average molecular weight of 300 to 500 g / mol.

[0108] 24. Process according to one of the preceding points, wherein the organic solvent provided in step i) contains a bodying agent in a weight proportion of 5 to 30 wt.%, preferably 10 to 25 wt.%.

[0109] 25. Process according to one of the preceding points, wherein the washing or cleaning active ingredient is introduced into the organic solvent at least partially, preferably completely, in solid form following step i).

[0110] 26. Process according to any of the preceding points, wherein the washing or cleaning active ingredient is introduced into the organic solvent in partial amounts. 27. Process according to any of the preceding points, wherein the washing or cleaning active ingredient is introduced into the organic solvent after step i) and provision ii).

[0111] 28. Process according to any one of the preceding points, wherein the washing or cleaning active ingredient is introduced into the organic solvent after step ii).

[0112] 29. The method according to any one of the preceding points, comprising the steps of i) providing the organic solvent having a temperature Ti above 10°C, ii) providing a first solid gelling agent preparation and introducing the first gelling agent preparation into the organic solvent; iii) providing a second liquid gelling agent preparation different from the first gelling agent preparation and introducing the second gelling agent preparation into the organic solvent, wherein the washing or cleaning-active ingredient is introduced into the organic solvent following step i) to form a washing and cleaning-active composition.

[0113] 30. The method according to any one of the preceding points, comprising the steps of i) providing the organic solvent having a temperature Ti above 10°C, ii) providing a first liquid gelling agent preparation and introducing the first gelling agent preparation into the organic solvent; iii) providing a second solid gelling agent preparation different from the first gelling agent preparation and introducing the second gelling agent preparation into the organic solvent, wherein the washing or cleaning-active ingredient is introduced into the organic solvent following step i) to form a washing and cleaning-active composition.

[0114] 31. Method according to one of the preceding points, wherein a gelling agent preparation is introduced into the organic solvent as a solid gelling agent preparation and the solid gelling agent preparation has a particle size distribution in which at least 70% by weight of the particles, preferably at least 80% by weight of the particles have a particle size below 1000 pm, preferably below 800 pm and in particular below 200 pm.

[0115] 32. The process according to any one of the preceding points, wherein a gelling agent preparation is introduced into the organic solvent as a solid gelling agent preparation, and the solid gelling agent preparation, based on its total weight, has a weight fraction of gelling agent above 60 wt.%, preferably above 80 wt.%, and in particular in the range from 85 to 99 wt.%. 33. The process according to any one of the preceding points, wherein a gelling agent preparation is introduced into the organic solvent as a liquid gelling agent preparation.

[0116] 34. Process according to one of the preceding points, wherein a gelling agent preparation is introduced into the organic solvent as a liquid gelling agent preparation and the liquid gelling agent preparation has, based on its total weight, a weight fraction of gelling agent of 1 to 20 wt.%, preferably of 2 to 15 wt.% and in particular of 4 to 12 wt.%.

[0117] 35. Process according to one of the preceding points, wherein a gelling agent preparation is introduced into the organic solvent as a liquid gelling agent preparation and the gelling agent preparation is in the form of a dispersion of the gelling agent in an organic solvent.

[0118] 36. Process according to item 35, wherein the gelling agent is in the form of particles having a maximum dimension of 2 to 100 mm, preferably 5 to 60 mm and in particular 10 to 30 mm.

[0119] 37. A process according to item 35 or 36, wherein the gelling agent is in the form of film particles.

[0120] 38. Process according to one of items 1 to 34, wherein a gelling agent preparation is introduced into the organic solvent as a liquid gelling agent preparation and the gelling agent preparation is in the form of a solution of the gelling agent in an organic solvent.

[0121] 39. Process according to item 38, wherein the solution of the gelling agent, when introduced into the organic solvent initially introduced in step i), has a temperature of 30 to 120°C, preferably of 50 to 110°C and in particular of 70 to 100°C.

[0122] 40. Process according to one of the preceding points, wherein the weight ratio of the gelling agent introduced by means of a solid gelling agent preparation to the gelling agent introduced by means of a liquid gelling agent preparation is 1000:1 to 20:1, preferably 800:1 to 40:1 and in particular 600:1 to 60:1.

[0123] 41 . Method according to one of the preceding points, wherein the method steps ii) and iii) are carried out successively.

[0124] 42. A process according to any one of the preceding points, wherein in step ii) and step iii) the same gelling agent is introduced into the organic solvent.

[0125] 43. The process according to any one of the preceding points, wherein in step ii) and step iii), a gelling agent from the group of polyvinyl alcohols is introduced into the organic solvent. 44. The process according to any one of the preceding points, wherein the temperature of the organic solvent is heated to a temperature T2 above the temperature Ti after introduction of the first gelling agent preparation in step ii) or after introduction of the second gelling agent preparation in step iii) or after introduction of the washing or cleaning agent.

[0126] 45. Process according to item 39, wherein the temperature difference between T2 and Ti is at least 20°C, preferably at least 25°C and in particular at least 30°C.

[0127] 46. ​​Process according to one of the preceding points, wherein the organic solvent is stirred for a period of 0.5 to 12 hours, preferably 1 to 6 hours and in particular 1 to 3 hours, following step ii) or after introduction of the second gelling agent preparation in step iii) or after introduction of washing or cleaning active ingredient.

[0128] 47. Process according to one of the preceding points, wherein following step iii) in a further step iv) a dye is introduced into the liquid washing or cleaning preparation.

[0129] 48. Method according to one of the preceding points, wherein the liquid washing or cleaning preparation is portioned in a further step v).

[0130] 49. Process according to one of the preceding points, wherein the liquid washing or cleaning-active preparation is poured into a trough in a further step v) following step iii), preferably following step iv).

[0131] 50. Method according to one of the preceding points, wherein the liquid washing or cleaning-active preparation is poured into a receiving chamber obtained by deformation of a water-soluble film following step iii), preferably following step iv), in a further step v).

[0132] 51. A process according to any one of the preceding points, wherein the liquid washing or cleaning preparation solidifies into a gel-like body upon cooling following step iii), preferably following step v). Examples

[0133] Washing or cleaning agents with the following composition were produced (information in

[0134] % by weight based on the total weight of the washing or cleaning agent):

[0135] Procedure 1

[0136] To produce the detergent or cleaning agent, a mixture of glycerin and 1,3-propanediol was heated to a temperature in the range of 65 to 90°C. Subsequently, nonionic surfactant, acrylic acid-amidopropyl sulfonic acid copolymer, and optionally zinc acetate were introduced into the solvent mixture. After adding PEG 400, solid polyvinyl alcohol was first added, followed by a dispersion of polyvinyl alcohol film particles in glycerin (4 wt.% polyvinyl alcohol). The temperature of the mixture was increased to 110 to 140°C. After stirring for three hours, the detergent or cleaning agent was mixed with dye.

[0137] Procedure 2

[0138] To prepare the detergents or cleaning agents, a mixture of glycerin and 1,3-propanediol was heated to a temperature in the range of 30 to 50°C. After adding PEG 400, a solution of polyvinyl alcohol in glycerin at a temperature of 85°C was introduced into the organic solvent. After stirring for two hours, solid polyvinyl alcohol, nonionic surfactant, acrylic acid-amidopropyl sulfonic acid copolymer, and, if desired, zinc acetate were added to the solvent mixture. The temperature of the mixture was increased to 110 to 140°C. After stirring for three hours, the detergent or cleaning agent was mixed with dye.

[0139] The washing or cleaning agents resulting from processes 1 and 2 were cast into a receiving chamber obtained by deep drawing a water-soluble polyvinyl alcohol film and cured by cooling.

Claims

Patent claims 1. A process for producing a washing or cleaning agent containing, based on its total weight a) 4 to 40 wt. % gelling agent; b) 0.1 to 40 wt. % washing or cleaning active ingredient; c) 30 to 90 wt. % organic solvent; comprising the steps: i) providing the organic solvent having a temperature Ti above 10°C, ii) providing a first gelling agent preparation and introducing the first gelling agent preparation into the organic solvent; iii) providing a second gelling agent preparation different from the first gelling agent preparation and introducing the second gelling agent preparation into the organic solvent, wherein the washing or cleaning active ingredient is introduced into the organic solvent following step i) to form a washing and cleaning active composition.

2. The method according to claim 1, wherein the gelling agent is selected from the group of polymeric gelling agents, preferably from the group of optionally acetalised polyvinyl alcohol, gelatin and xanthan or mixtures thereof, very particularly preferably from the group of optionally acetalised polyvinyl alcohol.

3. The method according to any one of the preceding claims, comprising the steps of i) providing the organic solvent having a temperature Ti above 10°C, ii) providing a first solid gelling agent preparation and introducing the first gelling agent preparation into the organic solvent; iii) providing a second liquid gelling agent preparation different from the first gelling agent preparation and introducing the second gelling agent preparation into the organic solvent, wherein the washing or cleaning active ingredient is introduced into the organic solvent following step i) to form a washing and cleaning composition.

4. A process according to claim 1 or 2, comprising the steps of i) providing the organic solvent having a temperature Ti above 10°C, ii) providing a first liquid gelling agent preparation and introducing the first gelling agent preparation into the organic solvent; iii) providing a second solid gelling agent preparation different from the first gelling agent preparation and introducing the second gelling agent preparation into the organic solvent, wherein the washing or cleaning active ingredient is introduced into the organic solvent following step i) to form a washing and cleaning active composition.

5. The method according to any one of the preceding claims, wherein a gelling agent preparation is introduced into the organic solvent as a solid gelling agent preparation and the solid gelling agent preparation has a particle size distribution in which at least 70% by weight of the particles, preferably at least 80% by weight of the particles have a particle size below 1000 pm, preferably below 800 pm and in particular below 200 pm.

6. Process according to one of the preceding claims, wherein a gelling agent preparation is introduced into the organic solvent as a solid gelling agent preparation and the solid gelling agent preparation, based on its total weight, has a weight fraction of gelling agent above 60% by weight, preferably above 80% by weight and in particular in the range from 85 to 99% by weight.

7. A process according to any one of the preceding claims, wherein a gelling agent preparation is introduced into the organic solvent as a liquid gelling agent preparation.

8. Process according to one of the preceding claims, wherein a gelling agent preparation is introduced into the organic solvent as a liquid gelling agent preparation and the liquid gelling agent preparation, based on its total weight, has a weight fraction of gelling agent of 1 to 20 wt.%, preferably of 2 to 15 wt.% and in particular of 4 to 12 wt.%.

9. Process according to one of the preceding claims, wherein in step ii) and step iii) the same gelling agent is introduced into the liquid washing or cleaning active mixture.

10. Process according to one of the preceding claims, wherein in step ii) and step iii) a gelling agent from the group of polyvinyl alcohols is introduced into the liquid washing or cleaning-active mixture.

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