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WO2021013409A1 - Corps moulés polyphasiques et procédé de fabrication de ceux-ci - Google Patents

Corps moulés polyphasiques et procédé de fabrication de ceux-ci Download PDF

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Publication number
WO2021013409A1
WO2021013409A1 PCT/EP2020/064988 EP2020064988W WO2021013409A1 WO 2021013409 A1 WO2021013409 A1 WO 2021013409A1 EP 2020064988 W EP2020064988 W EP 2020064988W WO 2021013409 A1 WO2021013409 A1 WO 2021013409A1
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WO
WIPO (PCT)
Prior art keywords
phase
gel
group
weight
shaped body
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/EP2020/064988
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German (de)
English (en)
Inventor
Boray TORUN
Peter Schmiedel
Ines Baranski
Yvonne Willemsen
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Henkel AG and Co KGaA
Original Assignee
Henkel AG and Co KGaA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Henkel AG and Co KGaA filed Critical Henkel AG and Co KGaA
Priority to EP20729731.8A priority Critical patent/EP4004171A1/fr
Publication of WO2021013409A1 publication Critical patent/WO2021013409A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0047—Detergents in the form of bars or tablets
    • C11D17/0065—Solid detergents containing builders
    • C11D17/0069—Laundry bars
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0047—Detergents in the form of bars or tablets
    • C11D17/0065—Solid detergents containing builders
    • C11D17/0073—Tablets
    • C11D17/0078—Multilayered tablets
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/43—Solvents
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • C08J3/075—Macromolecular gels
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/20—Organic compounds containing oxygen
    • C11D3/2068—Ethers
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/37—Polymers
    • C11D3/3746—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C11D3/3753—Polyvinylalcohol; Ethers or esters thereof

Definitions

  • the present invention describes multiphase moldings, their use as detergents or cleaning agents and processes for their production.
  • Detergents and cleaning agents are offered to consumers in the form of solid or liquid products.
  • the solid and liquid detergents or cleaning agents were originally packaged in the form of larger containers (e.g. bags or bottles). These large containers have recently been at least partially replaced by pre-dosed packaging forms (“unit dose”). These dosage units are, for example, tablets or water-soluble bags.
  • the metering units can in turn be configured with one or more phases.
  • Multi-phase detergent or cleaning agent metering units offer manufacturers and consumers a number of advantages over single-phase metering units. In this way, mutually incompatible ingredients can be separated from each other in the phases of multiphase dosage units that are separated from each other. In addition, the multiphase nature of a dosing unit can be used, for example, to visualize and communicate the different aspects of its washing or cleaning effect.
  • the dosing units can be packaged in a water-insoluble film or a water-soluble film. While the water-insoluble film must be removed by the consumer before the dosing unit is used, the film which is soluble when it is added to the aqueous washing or cleaning liquor can remain on the dosing unit. This simplified handling is offset by any leaky film seams and possibly unpleasant product feel as disadvantages.
  • the task was to provide a multiphase dosing unit for detergents or cleaning agents, which is characterized by good dissolution behavior, an attractive product look and feel.
  • the dosing unit should also be able to be stored and transported well even under high mechanical loads.
  • a first subject matter is a molded body comprising
  • a2) preferably at least one polymeric gel former with a molar mass of 10,000 g / mol to 200,000 g / mol;
  • first gel-like phase and the second phase form a common phase boundary
  • the shaped bodies are preferably dimensionally stable.
  • “Dimensionally stable”, as used herein, refers to the property of the molded body to maintain its three-dimensional shape under the conditions customary for storage and transport, i.e. in the temperature ranges customary for storage and transport and under the action of the forces customary for storage and transport, neither to disintegrate nor to be irreversible Enter into deformations.
  • Particularly preferred molded bodies comprise a translucent and / or transparent, particularly preferably a transparent, first gel-like phase. If a gel-like phase in the spectral range between 380 nm and 780 nm has a residual light output (transmission) of at least 20% based on the reference measurement, it is considered transparent within the meaning of the invention.
  • the transparency of the first gel phase can be determined using various methods.
  • the nephelometric turbidity unit (nephelometric turbidity value; NTU) is often used as a measured value for transparency. It is a unit used e.g. in water treatment for turbidity measurements e.g. in liquids. It is the unit of turbidity measured with a calibrated nephelometer. High NTU values are measured for opaque compositions, whereas low values are determined for clear compositions.
  • the HACH Turbidimeter 2100Q from the Hach Company, Loveland, Colorado (USA) is used using the calibration tools StabICal Solution HACH (20 NTU), StabICal Solution HACH (100 NTU) and StabICal Solution HACH (800 NTU) , all can also be ordered from Hach Company.
  • the measurement is filled in a 10 ml measuring cuvette with a cap with the composition to be examined and the measurement is carried out at 20 ° C.
  • gel-like phases At an NTU value (at 20 ° C.) of 60 or more, gel-like phases have a perceptible cloudiness that can be recognized by the naked eye within the meaning of the invention. It is therefore preferred if the first gel-like phase have an NTU value (at 20 ° C.) of at most 120, more preferably at most 110, more preferably at most 100, particularly preferably at most 80.
  • the transparency of the first gel-like phase is determined by a transmission measurement in the visual light spectrum over a wavelength range from 380 nm to 780 nm determined at 20 ° C.
  • a reference sample water, fully demineralized
  • a cuvette layer thickness 10 mm
  • the cuvette is then filled with a sample of the shaped body according to the invention and measured again.
  • the sample is filled in a liquid state at 80 ° C and solidified in the cuvette and then measured.
  • the first gel-like phase has a transmission (20 ° C.) of more preferably at least 25%, more preferably at least 30%, more preferably at least 40%, in particular at least 50%, particularly preferably at least 60%.
  • the first gel-like phase has a transmission (at 20 ° C.) of at least 30% (in particular of at least 40%, more preferably of at least 50%, particularly preferably of at least 60%) and an NTU value (at 20 ° C) of at most 120 (more preferably at most 1 10, more preferably at most 100, particularly preferably at most 80).
  • the weight of an individual molding is preferably 0.1 to 30 g, more preferably from 0.2 to 25 g, preferably from 5 to 20 g and in particular 15 to 17 g.
  • the shaped bodies can be designed in numerous different shapes, of which some particularly preferred shapes are described further below in the text.
  • the volume ratio of the first gel-like phase to the second phase is 4: 1 to 1:20, preferably 2: 1 to 1:12 and in particular 1: 1 to 1: 8 is.
  • the weight ratio of low molecular weight gel former to polymeric gel former in the first gel phase is 10: 1 to 1:20, preferably 8: 1 to 1:15 and in particular 6: 1 to 1 : 10 is.
  • the active substance-containing shaped bodies contain as a first essential component at least one low molecular weight gel former with a molar mass of up to 2000 g / mol, preferably with a molar mass of 200 g / mol to 2000 g / mol.
  • the use of gel formers with a molar mass of 200 g / mol to 1000 g / mol has proven to be particularly advantageous with regard to producibility, packability and subsequent use.
  • the proportion by weight of the low molecular weight gel former in the total weight of the first gel-like phase is preferably from 0.01 to 15% by weight, preferably from 0.1 to 10% by weight and in particular from 1 to 4% by weight.
  • the low molecular weight gel former has a solubility in water of less than 0.1 g / L (20 ° C.). The solubility of the organic gelator compound is determined at 20 ° C in double-distilled, demineralized water.
  • gel formers are preferably suitable which have a structure containing at least one hydrocarbon structural unit with 6 to 20 carbon atoms (preferably at least one carbocyclic, aromatic structural unit) and in addition an organic structural unit covalently bonded to the aforementioned hydrocarbon unit, the at least two groups selected from -OH, -NH-, or mixtures thereof.
  • Particularly preferred shaped bodies are characterized in that said shaped body contains at least one benzylidene alditol compound of the formula (GB-I) as a gel former
  • * - stands for a covalent single bond between an oxygen atom of the alditol backbone and the intended residue
  • n 0 or 1, preferably 1,
  • n 0 or 1, preferably 1,
  • both 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 the natural availability, the are preferred according to the invention Benzylidene alditol compounds used in the D configuration.
  • the alditol basic structure of the benzylidene alditol compound according to formula (GB-I) contained in the molded 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.
  • Particularly preferred moldings are those which are characterized in that R 1 , R 2 , R 3 , R 4 , R 5 and R 6 according to the benzylidene alditol compound of the formula (GB-I) independently represent a hydrogen atom, methyl, ethyl, chlorine , Fluorine or methoxy, preferably a hydrogen atom.
  • R 1 , R 2 , R 3 , R 4 , R 5 and R 6 independently represent a hydrogen atom, methyl, ethyl, chlorine , Fluorine or methoxy, preferably a hydrogen atom.
  • n is preferably 1.
  • m preferably represents 1.
  • the molding according to the invention very particularly preferably contains at least one compound of the formula (GB-11) as the benzylidene alditol compound of the formula (GB-I)
  • R 1 , R 2 , R 3 , R 4 , R 5 and R 6 are as defined in formula (I).
  • R 1 , R 2 , R 3 , R 4 , R 5 and R 6 independently of one another represent a hydrogen atom, methyl, ethyl, chlorine, fluorine or methoxy, preferably a hydrogen atom.
  • 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-0- (p-methylbenzylidene) -D-sorbitol; 1, 3: 2,4-di-0- (p-chlorobenzylidene) -D-sorbitol; 1, 3: 2,4-di-0- (2,4-dimethylbenzylidene) -D-sorbitol; 1, 3: 2,4-di-0- (p-ethylbenzylidene) -D-sorbitol; 1, 3: 2,4-di-0- (3,4-dimethylbenzylidene) -D-sorbitol or mixtures thereof.
  • Preferred moldings contain at least one 2,5-diketopiperazine compound of the formula (GB-II) as a gel former
  • R 1 , R 2 , R 3 and R 4 independently of one another represent a hydrogen atom, a hydroxyl 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, a Aryl (Ci-C 4 ) alkyloxy group, an aryl (Ci-C3) alkyl group, a heteroaryl group, a heteroaryl (Ci-C3) alkyl group, a (Ci-C 4 ) hydroxyalkyl group, a (Ci- C 4 )
  • R 5 stands for 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-C 4 ) -hydroxyalkyl group, a (Ci-C 4 ) -alkoxy- (Ci-C 4 ) -alkyl group, a (Ci-C 4 ) -acyloxy- (Ci- C 4 ) - alkyl group, an aryloxy (Ci-C 4 ) -alkyl group, an 0- (aryl- (Ci-C 4 ) -alkyl) oxy- (Ci-C 4 ) -alkyl group, a (Ci-C 4 ) -Alkylsulfanyl- (
  • R 3 and R 4 according to formula (GB-II) represent a hydrogen atom. It is particularly preferred according to the invention if R 2 , R 3 and R 4 according to formula (GB-II) represent a hydrogen atom. Therefore, particularly preferred moldings according to the invention contain at least one 2,5-diketopiperazine compound according to formula (GB-Ila)
  • R 1 and R 5 are as defined under formula (GB-II) (vide supra). It has been found to be preferred if the radical R 1 according to formula (GB-II) and according to formula (GB-Ila) binds in the para position of the phenyl ring. For the purposes of the present invention, therefore, those moldings according to the invention are preferred which contain at least one 2,5-diketopiperazine compound of the formula (GB-IIb),
  • R 1 and R 5 are defined as above under formula (GB-II) (vide supra).
  • the numbers 3 and 6 positioned on the ring atoms in formula (GB-IIb) only mark positions 3 and 6 of the diketopiperazine ring, as they are generally used in the context of the invention for naming all 2,5-diketopiperazines according to the invention.
  • the 2,5-diketopiperazine compounds of the formula (GB-II) have centers of chirality at least on the carbon atoms in positions 3 and 6 of the 2,5-diketopiperazine ring.
  • the numbering of the ring positions 3 and 6 was illustrated by way of example in formula (GB-Ilb).
  • the 2,5-diketopiperazine compound of the formula (GB-II) of the compositions according to the invention is preferably the configuration isomer 3S, 6S, 3R, 6S, 3S based on the stereochemistry of the carbon atoms at the 3- and 6-position of the 2,5-diketopiperazine ring , 6R, 3R, 6R or mixtures thereof, particularly preferably 3S, 6S.
  • Preferred molded articles contain at least one 2,5-diketopiperazine compound of the formula (GB-II) as a gel former, 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
  • the shaped bodies according to the invention may contain at least one diarylamidocystine compound of the formula (GB-III) as gel former a)
  • X + independently represent a hydrogen atom or an equivalent of a cation
  • 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 Ci-C 4 alkoxy group, a C 2 -C 4 hydroxyalkyl group, a hydroxyl group, an amino group, an N- (Ci-C 4 -alkyl) amino group, an N, N-di (Ci-C 4 -alkyl) amino group, an N- (C 2 -C 4 - hydroxyalkyl) amino group, an N, N-di ( C 2 -C 4 -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 each with at least one group from Ci-C 4 -alkyl group, Ci-C 4 -alkoxy group, C 2 -C 4 -hydroxyalkyl group, hydroxyl group, amino group, N- (Ci-C 4
  • Each of the stereocenters contained in the compound of the formula (GB-III) can, independently of one another, stand for the L or D stereoisomer. It is preferred according to the invention if the said cystine compound of the formula (GB-III) is derived from the L-stereoisomer of cysteine.
  • Said shaped bodies can contain at least one compound of the 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 Ci-C 4 -alkyl group, a Ci-C 4 -Alkoxy group, a C 2 -C 4 -hydroxyalkyl group, a hydroxyl group, or R 1 with R 2 or R 3 with R 4 forms a 5- or 6-membered fused ring, which in turn each with at least one group from Ci-C 4 -Alkyl group, Ci-C 4 alkoxy group, C 2 -C 4 hydroxyalkyl group, hydroxyl group can be substituted.
  • R 1 , R 2 , R 3 and R 4 independently of one another represent a hydrogen atom, a halogen atom, a Ci-C 4 -alkyl group, a Ci-C 4 -Alkoxy group, a C 2 -C 4 -hydroxy
  • N- (C8-C 24 ) -hydrocarbylglyconamide compounds suitable as gel formers a) preferably have the formula (GB-IV)
  • n 2 to 4, preferably 3 or 4, especially 4;
  • R 1 is selected from hydrogen, C1-C16 alkyl radicals, C1-C3 hydroxy or methoxyalkyl radicals, preferably C1-C3 alkyl, hydroxyalkyl or methoxyalkyl radicals, particularly preferably methyl;
  • R 2 is selected from C8-C 24 -alkyl radicals, C8-C 24 -monoalkenyl radicals, C8-C 24 -dialkenyl radicals, Cs-
  • the HO-CH2- (CHOH) n -C- radical is one of one
  • Glucuronic acid in particular is to be mentioned as a preferred radical.
  • R 1 is preferably H or a short-chain alkyl radical, in particular methyl.
  • R 2 is preferably a long-chain alkyl radical, for example a Cs-Cis alkyl radical.
  • R 2 has the meanings given for formula (GB-IV).
  • the at least one low molecular weight gel former is selected from the group consisting of benzylidene alditol compound, hydroxystearic acid, hydrogenated castor oil, diarylamidocystine compound, N- (Cs-C24) -hydrocarbylglyconamide, diketopiperazine compound, 2-methyl-acrylic acid- 2-ureido-ethyl ester and mixtures thereof.
  • the at least one gelling agent dibenzylidene sorbitol (DBS) is particularly preferred because of its technical effect.
  • a second essential component of the first gel phase is the polymeric gel former with a molar mass of 10,000 g / mol to 200,000 g / mol. It has proven to be particularly advantageous in relation to the production, packaging and handling of the shaped bodies to use polymeric gel formers with a molar mass of 10,000 to 40,000 g / mol.
  • the proportion by weight of polymeric compound in the total weight of the first gel-like phase is preferably from 0.01 to 15% by weight, more preferably from 0.1 to 12% by weight and in particular from 1 to 10% by weight.
  • Polymeric gel formers from the group of:
  • - Starch in particular potato starch, corn starch, wheat starch, pea starch or tapioca starch;
  • Suitable polyacrylates are homopolymers and copolymers of acrylic acid, in particular acrylic acid copolymers such as acrylic acid-methacrylic acid copolymers, and polysaccharides, especially heteropolysaccharides, and other customary polymer thickeners.
  • Suitable acrylic acid polymers are, for example, high molecular weight homopolymers of acrylic acid (INCI Carbomer) crosslinked with a polyalkenyl polyether, in particular an allyl ether of sucrose, pentaerythritol or propylene, which are also referred to as carboxyvinyl polymers.
  • a polyalkenyl polyether in particular an allyl ether of sucrose, pentaerythritol or propylene, which are also referred to as carboxyvinyl polymers.
  • Such polyacrylic acids are available inter alia from the company. BF Goodrich under the trade names Carbopof ®.
  • acrylic acid copolymers are the following acrylic acid copolymers: (i) Copolymers of two or more monomers from the group of acrylic acid, methacrylic acid and their simple esters, preferably formed with Ci- 4 alkanols (INCI Acrylates Copolymers), to which about the copolymers of methacrylic acid, butyl acrylate and methyl methacrylate and include (CAS 25035-69-2) or of butyl acrylate and methyl methacrylate (CAS 25852-37-3) is the example of the company.
  • Ci- 4 alkanols ICI Acrylates Copolymers
  • Suitable acrylate are also available under the trade name Sk ⁇ lan ® AT 120 and AT 120 Rheovis ® by the company BASF. If acrylic acid polymers and especially acrylic acid esters are used as polymeric thickeners, the pH is preferably more than 7, in particular at least 7.5, preferably 8 or more.
  • Preferred polyvinyl alcohols have a molecular weight of 10,000 g / mol to 150,000 g / mol, particularly preferably 10,000 g / mol to 80,000 g / mol and in particular 10,000 g / mol to 40,000 g / mol.
  • the degree of hydrolysis of preferred polyvinyl alcohols is 70 to 100 mol%, preferably 80 to 90 mol%, particularly preferably 81 to 89 mol% and in particular 82 to 88 mol%
  • the first gel-like phase contains at least one solvent as a third essential component.
  • Suitable solvents are selected from the group consisting of ethanol, n-propanol, i-propanol, butanols, glycol, propanediol, butanediol, methylpropanediol, glycerol, propylene carbonate, diglycol, propyl diglycol, butyl diglycol, hexylene glycol, diethylene glycol ethyl ether, diethylene glycol methyl ether, diethylene glycol methyl ether, diethylene glycol ether, diethylene glycol , Diethylene glycol n-butyl ether acetate, ethylene glycol propyl ether, ethylene glycol n-butyl ether, ethylene glycol hexyl ether, ethylene glycol n-butyl ether acetate, triethylene glycol, triethylene glycol methyl ether, triethylene glycol ethyl ether, triethylene glycol ether,
  • a first group of particularly preferred molded bodies is characterized in that a solvent from the group of polyalkylene glycols that are liquid at room temperature (20 ° C.), in particular of the polyalkylene glycols that are liquid at room temperature (20 ° C.), particularly preferably from the group of PEG 200 and PEG 400, is used becomes.
  • a second group of particularly preferred molded bodies is characterized in that the solvent is a solvent from the group of organic polyols liquid at room temperature (20 ° C.), in particular diols liquid at room temperature (20 ° C.), particularly preferably from the 2-methyl group -1, 3-propanediol (MPDiol) and 3-methyl-1,3-butanediol (isopentyldiol) includes.
  • the solvent is a solvent from the group of organic polyols liquid at room temperature (20 ° C.), in particular diols liquid at room temperature (20 ° C.), particularly preferably from the 2-methyl group -1, 3-propanediol (MPDiol) and 3-methyl-1,3-butanediol (isopentyldiol) includes.
  • molded bodies include glycerol or triacetin or water as solvents.
  • solvents have proven to be technically particularly advantageous, in particular the combination of water and 3-methyl-1,3-butanediol (isopentyldiol), but in particular the combination of water, glycerol and 3-methyl-1,3-butanediol are called.
  • the proportion by weight of solvent in the total weight of the first gel-like phase is preferably 10 to 98% by weight, particularly preferably 40 to 97% by weight and in particular 60 to 96% by weight.
  • the first gel-like phase preferably comprises less than 10% by weight, preferably less than 8% by weight, particularly preferably less than 4% by weight and in particular less than 1% by weight of surfactant. It is very particularly preferred if the first gel-like phase does not comprise any surfactant.
  • the first gel-like phase preferably has a storage modulus G 'of 10 3 Pascal to 10 8 Pascal, more preferably 10 4 Pascal to 10 6 Pascal, measured with a rotational rheometer using a cone-plate measuring system with a diameter of 40 mm and an opening angle of 2 ° at a temperature of 20 ° C.
  • the rheological characterization is carried out in the context of this invention with a rotational rheometer, for example from TA-Instruments, type AR G2, from Malvern "Kinexus", using a cone-plate measuring system with a diameter of 40 mm and a 2 ° opening angle at a temperature of 20 ° C performed. These are shear stress controlled rheometers. The determination can, however, also be carried out with other instruments or measurement geometries with comparable specifications.
  • the measurement of the storage modulus (abbreviation: G mix) and the loss modulus (abbreviation: G “) (each unit: Pa) was carried out with the equipment described above in an experiment with oscillating deformation.
  • the linear viscoelastic range is first determined in a “stress sweep experiment”.
  • the shear stress amplitude is increased at a constant frequency of e.g. 1 Hz.
  • the modules G ‘and G“ are plotted in a double logarithmic plot.
  • the shear stress amplitude or the (resulting) deformation amplitude can optionally be plotted on the x-axis.
  • the kink point is expediently determined by applying tangents to the two curve sections.
  • Shear stress amplitude is usually referred to as “critical deformation” or “critical shear stress”.
  • a frequency ramp for example between 0.01 Hz and 10 Hz, is run at a constant deformation amplitude.
  • the deformation amplitude must be chosen so that it lies in the linear range, ie lies below the critical deformation mentioned above. In the case of the compositions according to the invention, a deformation amplitude of 0.1% has proven to be suitable.
  • the modules G 'and G “are plotted against the frequency in a double logarithmic plot.
  • particularly preferred moldings have a weight of 0.1 to 30 g and comprise
  • first gel-like phase and the second phase form a common phase boundary
  • the first gel-like phase furthermore comprises at least one dye, preferably at least one water-soluble dye, particularly preferably a water-soluble polymer dye.
  • Preferred dyes should have high storage stability and insensitivity to the other ingredients of the detergents or cleaning agents and to light and not have any pronounced substantivity towards textile fibers in order not to stain them.
  • the dye is a common dye that can be used for various detergents or cleaning agents.
  • the dye is preferably selected from Acid Red 18 (CI 16255), Acid Red 26, Acid Red 27, Acid Red 33, Acid Red 51, Acid Red 87, Acid Red 88, Acid Red 92, Acid Red 95, Acid Red 249 ( CI 18134), Acid Red 52 (CI 45100), Acid Violet 126, Acid Violet 48, Acid Violet 54, Acid Yellow 1, Acid Yellow 3 (CI 47005), Acid Yellow 1 1, Acid Yellow 23 (CI 19140), Acid Yellow 3, Direct Blue 199 (CI 74190), Direct Yellow 28 (CI 19555), Food Blue 2 (CI 42090), Food Blue 5: 2 (CI 42051: 2), Food Red 7 (01 16255), Food Yellow 13 (CI 47005), Food Yellow 3 (C1 15985), Food Yellow 4 (C1 19140), Reactive Green 12, Solvent Green 7 (CI 59040).
  • Particularly preferred dyes are water-soluble acid dyes, for example Food Yellow 13 (Acid Yellow 3, CI 47005), Food Yellow 4 (Acid Yellow 23, CI 19140), Food Red 7 (Acid Red 18, CI 16255), Food Blue 2 (Acid Blue 9, CI 42090), Food Blue 5 (Acid Blue 3, CI 42051), Acid Red 249 (CI 18134), Acid Red 52 (CI 45100), Acid Violet 126, Acid Violet48, Acid Blue 80 (01 61585), Acid Blue 182, Acid Blue 182, Acid Green 25 (CI 61570), Acid Green 81.
  • Food Yellow 13 Acid Yellow 3, CI 47005
  • Food Yellow 4 Acid Yellow 23, CI 19140
  • Food Red 7 Acid Red 18, CI 16255
  • Food Blue 2 Acid Blue 9, CI 42090
  • Food Blue 5 Acid Blue 3, CI 42051
  • Acid Red 249 CI 18134
  • Acid Red 52 CI 45100
  • Acid Violet 126 Acid Violet48
  • Acid Blue 80 01 61585
  • Acid Blue 182 Acid Blue 18
  • Water-soluble direct dyes for example Direct Yellow 28 (CI 19555), Direct Blue 199 (CI 74190) and water-soluble reactive dyes, for example Reactive Green 12, and the dyes Food Yellow 3 (CI 15985), Acid Yellow 184 are also preferably used.
  • Aqueous dispersions of the following pigment dyes Pigment Black 7 (CI 77266), Pigment Blue 15 (CI 74160), Pigment Blue 15: 1 (CI 74160), Pigment Blue 15: 3 (CI 74160), Pigment Green 7 are also preferably used (CI 74260), Pigment Orange 5, Pigment Red 1 12 (CI 12370), Pigment Red 1 12 (CI 12370), Pigment Red 122 (CI 73915), Pigment Red 179 (CI 71 130), Pigment Red 184 (CI 12487), Pigment Red 188 (CI 12467), Pigment Red 4 (CI 12085), Pigment Red 5 (CI 12490), Pigment Red 9, Pigment Violet 23 (CI 51319), Pigment Yellow 1 (CI 28 1 1680), Pigment Yellow 13 (CI 21 100), Pigment Yellow 154, Pigment Yellow 3 (CI 1 1710), Pigment Yellow 74, Pigment Yellow 83 (CI 21 108), Pigment Yellow 97.
  • the following pigment dyes are used in the form of dispersions: Pigment Yellow 1 (CI 1 1680), Pigment Yellow 3 (C1 1 1710), Pigment Red 1 12 (CI 12370), Pigment Red 5 (CI 12490), Pigment Red 181 (CI 73360), Pigment Violet 23 (CI 51319), Pigment Blue 15: 1 (CI 74160), Pigment Green 7 (CI 74260), Pigment Black 7 (CI 77266).
  • water-soluble polymer dyes for example Liquitint, Liquitint Blue HP, Liquitint Blue MC, Liquitint Blue 65, Liquitint Cyan 15, Liquitint Patent Blue, Liquitint Violet 129, Liquitint Royal Blue, Liquitint Experimental Yellow 8949-43, Liquitint Green HMC, Liquitint Yellow LP, Liquitint Yellow II and mixtures thereof are used.
  • the group of very particularly preferred dyes includes Acid Blue 3, Acid Yellow 23, Acid Red 33, Acid Violet 126, Liquitint Yellow LP, Liquitint Cyan 15, Liquitint Blue HP and Liquitint Blue MC.
  • the proportion by weight of the dye in the total weight of the first gel-like phase is preferably 0.001 to 0.5% by weight, more preferably 0.002 to 0.2% by weight.
  • bitter substances primarily serves to avoid oral ingestion of the tablets containing active substances.
  • Preferred first gel-like phases contain at least one bitter substance in an amount of 0.0001 to 0.1% by weight, based on the total weight of the phase. Quantities from 0.0005 to 0.02% by weight are particularly preferred. According to the present invention, those bitter substances are particularly preferred which are soluble in water at 20 ° C. to the extent of at least 5 g / l. With regard to an undesirable interaction with the fragrance components also contained in the composition, in particular a change in the fragrance note perceived by the consumer, the ionic bitter substances have proven to be superior to the non-ionic ones. Ionic bitter substances consisting of organic cation (s) and organic anion (s) are consequently preferred for the composition according to the invention.
  • the at least one bitter substance is therefore an ionogenic bitter substance.
  • quaternary ammonium compounds which contain an aromatic group both in the cation and in the anion are eminently suitable.
  • the at least one bitter substance is therefore a quaternary ammonium compound.
  • a suitable quaternary ammonium compound is, for example, without restriction, benzyldiethyl ((2,6-xylylcarbamoyl) methyl) ammonium benzoate, which is commercially available, for example, under the trademarks Bitrex® and Indige-stin®. This compound is also known as Denatonium Benzoate.
  • the at least one bitter substance is benzyl diethyl ((2,6-xylylcarbamoyl) methyl) ammonium benzoate (Bitrex®). If Bitrex® is used, most amounts up to 0.002% by weight are preferred. The information is based on the active substance content.
  • the shaped bodies also comprise a second phase which forms a common phase boundary with the first gel-like phase.
  • This second phase is preferably present as a gel or as a solidified melt or in particle form, but particularly preferably as a gel.
  • the second phase is particularly suitable for packaging ingredients with active washing or cleaning properties. Fragrances, enzymes or textile care substances are preferably used as washing or cleaning active ingredients.
  • the proportion by weight of active washing or cleaning ingredients in the total weight of the second phase is preferably 1 to 90% by weight, more preferably 2 to 80% by weight and in particular 5 to 60% by weight.
  • At least one encapsulated washing or cleaning active ingredient in the second phase is particularly preferred.
  • compositions for detergent tablets can be found in the tables below (data in% by weight based on the total weight of the first or second phase).
  • the shaped bodies have a weight of 0.2 to 20 g and the first phase has a common phase boundary with the second phase.
  • fragrances from the group of fragrances, enzymes and textile care products
  • fragrances from the group of fragrances, enzymes and textile care products
  • fragrances from the group of fragrances, enzymes and textile care products
  • fragrances from the group of fragrances, enzymes and textile care products
  • fragrances from the group of fragrances, enzymes and textile care products
  • fragrances from the group of fragrances, enzymes and textile care products
  • fragrances from the group of fragrances, enzymes and textile care products
  • the first gel-like phase is particularly suitable for at least partially enclosing the second phase. In other words, it is preferred if the first gel-like phase covers the surface of the second phase to a significant extent. It is preferred that the first gel-like phase covers at least 30%, preferably at least 50%, particularly preferably at least 70% and in particular at least 90% of the surface of the second phase.
  • a first embodiment is preferred in which the molded body has at least two layers, one of which is formed by the first gel-like phase and the second layer is formed by the second phase.
  • multilayer moldings can also be produced.
  • Three-layer moldings are particularly preferred, the upper and lower layers of which are formed by a first gel-like phase, while the middle layer corresponds to the second phase of moldings according to the invention (“sandwich”).
  • the first gel-like phase is in the form of a trough shaped body, the trough of which is at least partially filled with the second phase.
  • a core formed from the second phase for example a cylindrical core, is surrounded concentrically by the first gel-like phase on its outer surface, but not on its upper and lower sides.
  • Embodiments in which the first gel-like phase completely surrounds the second phase are very particularly preferred.
  • a spherical core is surrounded by a spherical shell.
  • polyhedral cores, in particular cube-shaped cores, which are surrounded by a polyhedral shell, in particular a cube-shaped shell are also conceivable.
  • the shaped bodies enable complete washing or cleaning agents to be packaged, but also washing or cleaning aids, for example fragrance additives, care aids or detergent boosters such as enzymes.
  • Corresponding aids can in turn be made up independently or in combination with detergents or cleaning agents.
  • Another preferred subject matter is detergent or cleaning agent combination products which, in addition to a solid or liquid detergent or cleaning agent, also comprise at least one of the shaped bodies described above.
  • a number of other particularly preferred formulations for detergent tablets can be found in the tables below (data in% by weight based on the total weight of the first or second phase).
  • the shaped bodies have a weight of 0.2 to 20 g and the first gel-like phase completely surrounds the second phase.
  • fragrances from the group of fragrances, enzymes and textile care products
  • fragrances from the group of fragrances, enzymes and textile care products
  • fragrances from the group of fragrances, enzymes and textile care products
  • fragrances from the group of fragrances, enzymes and textile care products
  • fragrances from the group of fragrances, enzymes and textile care products
  • fragrances from the group of fragrances, enzymes and textile care products
  • fragrances from the group of fragrances, enzymes and textile care products
  • fragrances from the group of fragrances, enzymes and textile care products
  • fragrances from the group of fragrances, enzymes, textile care products and encapsulated fragrances
  • This application also relates to a process for producing one of the above-described shaped bodies, comprising the steps
  • a2) preferably at least one polymeric gel former with a molar mass of 10,000 g / mol to 200,000 g / mol;
  • the first flowable preparation is preferably introduced into a mold in step c).
  • the first flowable preparation is preferably cooled in step c).
  • the molding can also be simplified by using a release agent, for example silicone oil.
  • the shaped bodies are particularly suitable as active substance carriers for substances with active washing or cleaning properties.
  • the use of the moldings described above in processes for cleaning or caring for textile surfaces are therefore further subjects of this application.
  • Shaped body comprising
  • a2) preferably at least one polymeric gel former with a molar mass of 10,000 g / mol to 200,000 g / mol;
  • first gel-like phase and the second phase form a common phase boundary
  • Shaped body according to item 1 wherein the shaped body has a weight of 0.1 to 30 g, preferably 0.2 to 25 g, preferably 5 to 20 g and in particular 15 to 17 g.
  • Shaped body according to one of the preceding points wherein the shaped body has a cubic three-dimensional shape.
  • the low molecular weight gel former having a molar mass of 200 g / mol to 2000 g / mol, preferably from 200 g / mol to 1000 g / mol.
  • the low molecular weight gel former is selected from the group of benzylidene alditol compounds, hydroxystearic acid, hydrogenated castor oil, diarylamidocystine compound, N- (C8-C 24 ) -hydrocarbylglyconamide, diketopiperazine compound, 2-methyl -acrylic acid-2-ureido-ethyl ester and mixtures thereof.
  • the first gel-like phase comprises a polymeric gel former with a molar mass of 10,000 g / mol to 40,000 g / mol.
  • Shaped body according to one of the preceding points wherein the first gel-like phase, based on its total weight, has a weight fraction of polymeric forming agent of 0.01 to 15% by weight, preferably 0.1 to 12% by weight and in particular 1 to 10% by weight.
  • Celluloses and cellulose derivatives especially methyl cellulose
  • Starch especially potato starch, corn starch, wheat starch, pea starch or
  • Polyvinyl alcohols Shaped body according to one of the preceding points, wherein the polymeric gel former is selected from the group of polyvinyl alcohols. Shaped body according to one of the preceding points, the weight ratio of low molecular weight gel former to polymeric gel former in the first gel phase being 10: 1 to 1:20, preferably 8: 1 to 1:15 and in particular 6: 1 to 1:10. Shaped body according to one of the preceding points, the weight ratio of
  • Dibenzylidene sorbitol to polyvinyl alcohol is 10: 1 to 1:20, preferably 8: 1 to 1:15 and in particular 6: 1 to 1:10. Shaped body according to one of the preceding points, wherein the solvent is selected from
  • Shaped body according to one of the preceding points, wherein the solvent d) is a solvent from the group of organic polyols liquid at room temperature (20 ° C), in particular the diols liquid at room temperature (20 ° C), particularly preferably from the group 2-methyl 1,3-propanediol (MPDiol) and 3-methyl-1,3-butanediol (isopentyldiol) includes.
  • Shaped body according to one of the preceding points the first gel-like phase having a weight fraction of solvent of 10 to 98% by weight, preferably 40 to 97% by weight and in particular 60 to 96% by weight, based on its total weight.
  • Shaped body according to one of the preceding points, wherein the first gel-like phase, based on its total weight, is less than 10% by weight, preferably less than 8% by weight, particularly preferably less than 4% by weight and in particular less than 1% by weight % Includes surfactant.
  • Shaped body according to one of the preceding points, wherein the first gel-like phase does not comprise a surfactant. Shaped body with a weight of 0.2 to 20 g, comprising,
  • first gel-like phase and the second phase form a common phase boundary.
  • shaped body according to one of the preceding points, the second phase being present as a gel or as a solidified melt or in particle form, preferably as a gel.
  • Shaped body according to one of the preceding points, the first gel-like phase covering at least 30%, preferably at least 50%, particularly preferably at least 70% and in particular at least 90% of the surface of the second phase.
  • Shaped body according to one of the preceding points, the first gel-like phase completely enclosing the second phase.
  • Shaped body according to one of the previous points the volume ratio of the first gel phase to the second phase being 4: 1 to 1:20, preferably 2: 1 to 1:12 and in particular 1: 1 to 1: 8.
  • the first gel-like phase further comprises at least one dye, preferably at least one water-soluble dye, particularly preferably a water-soluble polymer dye.
  • Shaped body according to one of the previous points wherein the first gel-like phase has a storage module G '(rotational rheometer using a cone-plate measuring system with 40 mm diameter and 2 ° opening angle at a temperature of 20 ° C) of 10 3 Pascal to 10 8 Pascal, preferably 10 4 Pascal to 10 6 Pascal.
  • Shaped body according to one of the preceding points the first gel-like phase being translucent and / or transparent, particularly preferably transparent.
  • a2) preferably at least one polymeric gel former with a molar mass of 10,000 g / mol to 200,000 g / mol;

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  • Wood Science & Technology (AREA)
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Abstract

L'invention concerne des corps moulés comprenant a) au moins une première phase sous forme de gel, contenant a1) au moins un gélifiant de bas poids moléculaire possédant une masse molaire allant jusqu'à 2000 g/mol ; a2) de préférence au moins un gélifiant polymère possédant une masse molaire de 10 000 g/mol à 200 000 g/mol ; a3) au moins un solvant, b) au moins une deuxième phase différente de la première phase sous forme gel, la première phase sous forme de gel et la deuxième phase formant ensemble une limite de phase commune, l'utilisation de ces corps moulés comme détergents ou produits de nettoyage et un procédé de fabrication de ceux-ci.
PCT/EP2020/064988 2019-07-23 2020-05-29 Corps moulés polyphasiques et procédé de fabrication de ceux-ci Ceased WO2021013409A1 (fr)

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DE102019210893.8A DE102019210893A1 (de) 2019-07-23 2019-07-23 Mehrphasige Formkörper und Verfahren zu deren Herstellung

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Cited By (3)

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WO2023198327A1 (fr) * 2022-04-13 2023-10-19 Henkel Ag & Co. Kgaa Procédé de fabrication d'une dose unitaire de détergent
WO2023198324A1 (fr) * 2022-04-13 2023-10-19 Henkel Ag & Co. Kgaa Procédé de fabrication d'une unité de partie détergente
EP4345155A1 (fr) * 2022-09-29 2024-04-03 Henkel AG & Co. KGaA Dose unitaire de détergent pour vaisselle en gel et phase comprimée

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EP4067466A1 (fr) * 2021-03-30 2022-10-05 Henkel AG & Co. KGaA Détergent ou nettoyant
DE102022203705A1 (de) * 2022-04-13 2023-10-19 Henkel Ag & Co. Kgaa Verfahren zur Herstellung einer Waschmittelportionseinheit
DE102023212739A1 (de) * 2023-12-14 2025-06-18 Henkel Ag & Co. Kgaa Wasch- oder Reinigungsmittelformkörper

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US20110220537A1 (en) * 2010-03-12 2011-09-15 Fernandez-Prieto Susana Liquid Detergent Compositions Comprising pH Tuneable Amido-Gellants, and Processes For Making
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WO2023198327A1 (fr) * 2022-04-13 2023-10-19 Henkel Ag & Co. Kgaa Procédé de fabrication d'une dose unitaire de détergent
WO2023198324A1 (fr) * 2022-04-13 2023-10-19 Henkel Ag & Co. Kgaa Procédé de fabrication d'une unité de partie détergente
EP4345155A1 (fr) * 2022-09-29 2024-04-03 Henkel AG & Co. KGaA Dose unitaire de détergent pour vaisselle en gel et phase comprimée

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