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
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/12—Water-insoluble compounds
  • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
  • C11D3/1246—Silicates, e.g. diatomaceous earth
  • C11D3/128—Aluminium silicates, e.g. zeolites
• • 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
• • 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
  • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
• • 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
  • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
  • C11D17/065—High-density particulate detergent compositions
• • 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
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/12—Water-insoluble compounds
  • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
  • C11D3/1246—Silicates, e.g. diatomaceous earth
  • C11D3/1253—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite
  • C11D3/126—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite in solid compositions

Definitions

• the present invention relates to a process for the production of moldings which have washing and cleaning properties.
• the invention relates to a method for producing detergent tablets for textile washing in a household washing machine, which are briefly referred to as detergent tablets.
• the dichotomy between a sufficiently hard molded body and a sufficiently fast disintegration time is a central problem. Since sufficiently stable, i.e. Shaped and unbreakable moldings can only be produced by relatively high pressure, there is a strong compression of the mold components and a consequent delayed disintegration of the molded body in the aqueous liquor and thus to a slow release of the active substances in the washing or cleaning process .
• the delayed disintegration of the moldings has the further disadvantage that conventional detergent tablets cannot be washed in via the washing-in chamber of household washing machines, since the tablets do not disintegrate into secondary particles that are small enough to be washed into the washing drum from the washing-in chamber to become.
• EP-A-0 466 484 discloses detergent tablets in which the premix to be compressed has particle sizes between 200 and 1200 ⁇ m, the upper and lower limits of the particle sizes not differing by more than 700 ⁇ m. None is said in this document about the surface treatment of individual ingredients.
• EP-A-0 522 766 also relates to moldings made from a compact, particulate detergent composition containing surfactants, builders and disintegration aids (for example based on cellulose), at least some of the particles being coated with the disintegration agent, which is both binder - As well as disintegration effect when dissolving the moldings in water.
• This font also shows the general difficulty towards producing shaped bodies with adequate stability and at the same time good solubility.
• the particle size in the mixture to be ve ⁇ ress should be above 200 microns, the upper and lower limits of the individual particle sizes should not differ by more than 700 microns.
• DE 40 10 533 (Henkel KGaA) discloses a process for the production of compacts from pre-compressed granules.
• the granules produced by extrusion and cutting in a first stage are mixed with other ingredients and auxiliaries and tabletted, if necessary.
• the proportion of the pre-compacted granules in the compacts is up to 100% in this document.
• Pretreatment of the optionally used admixing components is not disclosed.
• detergent tablets produced according to the documents mentioned have sufficient hardness, they have disintegration speeds which do not allow metering via a dispenser of a household washing machine.
• dissolution times of less than 10 minutes and residue values of less than 50% are designated as good, such values being completely inadequate for the use of detergent tablets via the dispenser.
• the present invention was based on the object of providing a process for the production of detergent tablets which makes it possible to to produce bodies that are free from the disadvantages mentioned. It should be easy and highly reproducible to be able to produce detergent tablets which have a high level of hardness, are distinguished by a rapid dissolution rate and can also be used via the induction chamber of household washing machines. The hardness should not only be limited to a high diametrical breaking stress, but also ensure the stability of the molded body during transport (rubbing / shaking stress) and falling.
• the molded articles produced by the process to be provided should not experience any change in their advantageous property profile even when stored open, so that airtight packaging of individual tablets can be dispensed with.
• detergent tablets can be produced with the advantages mentioned if premixes are pressed which consist of granules containing surfactant which contain zeolite P and / or zeolite X and further processing components.
• the invention therefore relates to a process for producing detergent tablets by mixing a surfactant-containing granulate with finely divided preparation components and subsequent shaping in a manner known per se, in which the surfactant-containing granulate is a zeolite of the P and / or X type contains.
• press agglomeration processes can also be used, for example.
• the granulation can be carried out in a large number of apparatuses customarily used in the detergent and cleaning agent industry. For example, it is possible to use the rounding agents commonly used in pharmacy. In such turntable devices, the residence time of the granules is usually less than 20 seconds.
• Conventional mixers and mixing granulators are also suitable for granulation. Both high-intensity mixers (“high-shear mixers”) and normal mixers with lower circulation speeds can be used as mixers.
• Suitable mixers are, for example Eirich ® mixer Series R or RV (trademark of Maschinenfabrik Gustav Eirich, Hardheim), the Schugi ® Flexomix, the Fukae ® FS-G mixers (trade marks of Fukae Powtech, Kogyo Co., Japan), the Lödige ® FM, KM and CB mixers (trademark of Lödige Maschinenbau GmbH, Paderborn) or the Drais ® series T or KT (trademark of Drais-Werke GmbH, Mannheim).
• the residence times of the granules in the mixers are in the range of less than 60 seconds, the residence time also being dependent on the circulation speed of the mixer. The dwell times are reduced accordingly the faster the mixer runs.
• the residence times of the granules in the mixer / rounder are preferably less than one minute, preferably less than 15 seconds. Dwell times of up to 20 minutes are set in slow-running mixers, for example a Lödige KM, dwell times below 10 minutes being preferred because of the process economy.
• the surfactant-containing granules are compressed under pressure and under the action of shear forces, homogenized in the process and then discharged from the apparatus in a shaping manner.
• the most technically significant press agglomeration processes are extrusion, roller compaction, pelleting and tableting.
• Press agglomeration processes containing granules are extrusion, roller compacting and pelletizing.
• the surfactant-containing granulate is preferably fed continuously to a planetary roller extruder or a 2-shaft extruder or 2-screw extruder with co-rotating or counter-rotating screw guide, the housing and the extruder granulating head of which are heated to the predetermined extrusion temperature could be.
• the premix is compressed, plasticized, extruded in the form of fine strands through the perforated die plate in the extruder head and finally, under pressure, which is preferably at least 25 bar, but can also be lower at extremely high throughputs depending on the apparatus used the extrudate is preferably reduced to approximately spherical to cylindrical granules by means of a rotating knife.
• the hole diameter of the perforated nozzle plate and the strand cut length are matched to the selected granulate dimension.
• the production of granules of an essentially uniformly predeterminable particle size succeeds, and in particular the absolute particle sizes can be adapted to the intended use.
• Important embodiments provide for the production of uniform granules in the millimeter range, for example in the range from 0.8 to 5 mm and in particular in the range from approximately 1.0 to 3 mm.
• the length / diameter ratio of the chipped primary granules is in the range from about 1: 1 to about 3: 1.
• extrusions / pressings can also be carried out in low-pressure extruders, in the Kahl press or in the extruder.
• the production process for the surfactant-containing granules is carried out by means of roller compaction.
• the surfactant-containing granulate is deliberately placed between two smooth or Rolls of defined shape are metered in and rolled out under pressure between the two rolls to form a leaf-shaped compact, the so-called Schülpe.
• the rollers exert a high line pressure on the premix and can be additionally heated or cooled as required.
• smooth rollers smooth, unstructured sliver belts are obtained, while by using structured rollers, correspondingly structured slugs or individual pellets can be produced, in which, for example, certain shapes of the later granules or moldings can be specified.
• the sliver belt is subsequently broken up into smaller pieces by a knocking-off and crushing process and can be processed into granules in this way, which can be further tempered, in particular in an approximately spherical shape, by further known surface treatment processes.
• the preparation of the surfactant-containing granules is carried out by means of pelleting.
• the granules containing surfactant are applied to a perforated surface and pressed through the holes by means of a pressure-producing body.
• the surfactant-containing granules are compressed under pressure, plasticized, pressed through a perforated surface in the form of fine strands by means of a rotating roller and finally comminuted to granules with a knock-off device.
• the most varied configurations of the pressure roller and perforated die are conceivable here.
• the press rolls can also be conical in the plate devices, in the ring-shaped devices dies and press roll (s) can have the same or opposite direction of rotation.
• An apparatus suitable for carrying out the method according to the invention is described, for example, in German laid-open specification DE 38 16 842 (Schlüter GmbH).
• the ring die press disclosed in this document consists of a rotating ring die penetrated by press channels and at least one press roller which is operatively connected to its inner surface and which presses the material supplied to the die space through the press channels into a material discharge.
• ring die and press roller can be driven in the same direction, so that a reduced shear stress and thus a lower temperature increase of the premix can be achieved.
• heatable or coolable rollers in the pelletizing in order to set a desired temperature of the premix.
• the surfactant-containing granules contain surfactants.
• surfactants come from the group of anionic, nonionic, zwitterionic or cationic surfactants, anionic surfactants being clearly preferred for economic reasons and because of their range of services.
• Anionic surfactants used are, for example, those of the sulfonate and sulfate type.
• the surfactants of the sulfonate type are preferably C 9 . 13 - Alkylbenzenesulfonates, olefinsulfonates, ie mixtures of alkene and hydroxyalkanesulfonates and disulfonates, such as those obtained from C 12 . 18- Monoolefmen with terminal or internal double bond by sulfonation with gaseous sulfur trioxide and subsequent alkaline or acidic hydrolysis of the sulfonation products. Alkanesulfonates which are derived from C 12 are also suitable.
• esters of ⁇ -sulfofatty acids for example the ⁇ -sulfonated methyl esters of hydrogenated coconut, palm kernel or tallow fatty acids, are also suitable.
• sulfonated fatty acid glycerol esters are sulfonated fatty acid glycerol esters.
• Fatty acid glycerol esters are to be understood as meaning the mono-, di- and triesters and their mixtures as obtained in the production by esterification of a monoglycerol with 1 to 3 moles of fatty acid or in the transesterification of triglycerides with 0.3 to 2 moles of glycerol become.
• Preferred sulfated fatty acid glycerol esters are the sulfate products of saturated fatty acids having 6 to 22 carbon atoms, for example caproic acid, caprylic acid, capric acid, myristic acid, lauric acid, palmitic acid, stearic acid or behenic acid.
• Alk (en) yl sulfates are the alkali and especially the sodium salts of the sulfuric acid half-esters of C 12 -C 18 fatty alcohols, for example from coconut oil alcohol, tallow fatty alcohol, lauryl, myristyl, cetyl or stearyl alcohol or C 10 -C 20 -Oxo alcohols and those half esters of secondary alcohols of this chain length are preferred. Also preferred are alk (en) yl sulfates of the chain length mentioned which contain a synthetic, straight-chain alkyl radical which is produced on a petrochemical basis and which have a degradation behavior analogous to that of the adequate compounds based on oleochemical raw materials.
• C 12 -C 16 alkyl sulfates and C 12 -C 15 alkyl sulfates as well as C ] 4 -C 15 alkyl sulfates are preferred for reasons of washing technology.
• 2,3-alkyl sulfates which are produced for example in accordance with US Patent No. 3,234,258 or 5,075,041 and can be obtained as commercial products from Shell Oil Company under the name DAN ®, are suitable anionic surfactants.
• the sulfuric acid monoesters of the straight-chain or branched C 7.21 alcohols ethoxylated with 1 to 6 mol of ethylene oxide, such as 2-methyl-branched C 9 . ⁇ alcohols with an average of 3.5 moles of ethylene oxide (EO) or C 12.18 fatty alcohols with 1 to 4 EO are suitable. Because of their high foaming behavior, they are used in cleaning agents only in relatively small amounts, for example in amounts of 1 to 5% by weight.
• Suitable anionic surfactants are also the salts of alkylsulfosuccinic acid, which are also referred to as sulfosuccinates or as sulfosuccinic acid esters and which are monoesters and / or diesters of sulfosuccinic acid with alcohols, preferably fatty alcohols and especially ethoxylated fatty alcohols.
• Preferred sulfosuccinates contain C 8 _ 18 fatty alcohol radicals or mixtures thereof.
• Particularly preferred sulfosuccinates contain a fatty alcohol residue which is derived from ethoxylated fatty alcohols, which in themselves are nonionic surfactants (description see below).
• sulfosuccinates whose fatty alcohol residues are derived from ethoxylated fatty alcohols with a narrow homolog distribution are particularly preferred. It is also possible to use alk (en) ylsuccinic acid with preferably 8 to 18 carbon atoms in the alk (en) yl chain or salts thereof. Soaps are particularly suitable as further anionic surfactants. Saturated fatty acid soaps are suitable, such as the salts of lauric acid, myristic acid, palmitic acid, stearic acid, hydrogenated erucic acid and behenic acid, and in particular soap mixtures derived from natural fatty acids, for example coconut, palm kernel or tallow fatty acids.
• the anionic surfactants can be in the form of their sodium, potassium or ammonium salts and also as soluble salts of organic bases, such as mono-, di- or triethanolamine.
• the anionic surfactants are preferably in the form of their sodium or potassium salts, in particular in the form of the sodium salts.
• surfactant granules are preferred as process end products of intermediate step a), which each contain 5 to 50% by weight, preferably 7.5 to 40% by weight and in particular 10 to 20% by weight of anionic surfactant (s) based on the granules.
• preferred surfactant granules have a soap content which exceeds 0.2% by weight, based on the total weight of the detergent tablets produced in step d).
• the preferred anionic surfactants are the alkylbenzenesulfonates and fatty alcohol sulfates, with preferred detergent tablets 2 to 20% by weight, preferably 2.5 to 15% by weight and in particular 5 to 10% by weight of fatty alcohol sulfate (s) in each case based on the weight of the detergent tablets
• the nonionic surfactants used are preferably alkoxy-hardened, advantageously ethoxylated, in particular primary alcohols having preferably 8 to 18 carbon atoms and an average of 1 to 12 moles of ethylene oxide (EO) per mole of alcohol, in which the alcohol radical is branched linearly or preferably in the 2-position methyl can be or linear and can contain methyl-branched radicals in the mixture, as are usually present in oxo alcohol residues.
• alcohol ethoxylates with linear residues of alcohols of native origin with 12 to 18 carbon atoms, for example from coconut, palm, tallow fat or oleyl alcohol, and an average of 2 to 8 EO per mole of alcohol are particularly preferred.
• the preferred ethoxylated alcohols include, for example, C 12 . 14 - alcohols with 3 EO or 4 EO, C 9 . n -Alcohol with 7 EO, C 13-l5 - alcohols with 3 EO, 5 EO, 7 EO or 8 EO, C 12 . 18 - alcohols with 3 EO, 5 EO or 7 EO and mixtures of these, such as mixtures of C 12 . 14 -alcohol with 3 EO and C 12.18 -alcohol with 5 EO.
• the degrees of ethoxylation given represent statistical averages, which can be an integer or a fraction for a specific product.
• Preferred alcohol ethoxylates have a narrow homolog distribution (narrow range ethoxylates, NRE).
• fatty alcohols with more than 12 EO can also be used. Examples of this are tallow fatty alcohol with 14 EO, 25 EO, 30 EO or 40 EO.
• nonionic surfactants which are used either as the sole nonionic surfactant or in combination with other nonionic surfactants, are alkoxy-hard, preferably ethoxylated or ethoxylated and propoxylated fatty acid alkyl esters, preferably with 1 to 4 carbon atoms in the alkyl chain, in particular Fatty acid methyl esters as described, for example, in Japanese patent application JP 58/217598 or which are preferably prepared by the process described in international patent application WO-A-90/13533.
• alkyl polyglycosides Another class of nonionic surfactants that can be used advantageously are the alkyl polyglycosides (APG).
• Alkypolyglycosides that can be used satisfy the general formula RO (G) z , in which R denotes a linear or branched, in particular methyl-branched, saturated or unsaturated, aliphatic radical having 8 to 22, preferably 12 to 18, C atoms and G is Is a symbol which stands for a glycose unit with 5 or 6 carbon atoms, preferably for glucose.
• the degree of glycosidation z is between 1.0 and 4.0, preferably between 1.0 and 2.0 and in particular between 1.1 and 1.4.
• Linear alkyl polyglucosides, ie alkyl polyglycosides, in which the polyglycosyl radical is a glucose radical and the alkyl radical is an n-alkyl radical are preferably used.
• the end products of the process in intermediate step a) can preferably contain alkyl polyglycosides, with APG contents of more than 0.2% by weight, based on the entire molded body, being preferred.
• Particularly preferred detergent tablets contain APG in amounts of 0.2 to 10% by weight, preferably 0.2 to 5% by weight and in particular 0.5 to 3% by weight.
• Nonionic surfactants of the amine oxide type for example N-coconut alkyl-N, N-dimethylamine oxide and N-tallow alkyl-N, N-dihydroxyethylamine oxide, and the fatty acid alkanolamides can also be suitable.
• the amount of these nonionic surfactants is preferably not more than that of the ethoxylated fatty alcohols, in particular not more than half of them.
• surfactants are polyhydroxy fatty acid amides of the formula (II),
• RCO stands for an aliphatic acyl radical with 6 to 22 carbon atoms
• R 1 for hydrogen, an alkyl or hydroxyalkyl radical with 1 to 4 carbon atoms
• [Z] for a linear or branched polyhydroxyalkyl radical with 3 to 10 carbon atoms and 3 to 10 hydroxyl groups.
• the polyhydroxy fatty acid amides are known substances which can usually be obtained by reductive amination of a reducing sugar with ammonia, an alkylamine or an alkanolamine and subsequent acylation with a fatty acid, a fatty acid alkyl ester or a fatty acid chloride.
• the group of polyhydroxy fatty acid amides also includes compounds of the formula (III)
• R represents a linear or branched alkyl or alkenyl radical having 7 to 12 carbon atoms
• R 1 represents a linear, branched or cyclic alkyl radical or an aryl radical having 2 to 8 carbon atoms
• R 2 represents a linear, branched or cyclic alkyl radical or an aryl radical or an oxyalkyl radical having 1 to 8 carbon atoms
• C - alkyl or phenyl radicals being preferred
• [Z] representing a linear polyhydroxyalkyl radical whose alkyl chain is substituted by at least two hydroxyl groups, or alkoxylated, preferably ethoxylated or propylated, derivatives of this rest.
• [Z] is preferably obtained by reductive amination of a reduced sugar, for example glucose, fructose, maltose, lactose, galactose, mannose or xylose.
• a reduced sugar for example glucose, fructose, maltose, lactose, galactose, mannose or xylose.
• the N-alkoxy- or N-aryloxy-substituted compounds can then, for example according to the teaching of international application WO-A-95/07331, be converted into the desired polyhydroxy fatty acid amides by reaction with fatty acid methyl esters in the presence of an alkoxide as catalyst.
• the surfactant content of the surfactant-containing granules produced in step a) is 5 to 60% by weight. , preferably 10 to 50 wt .-% and in particular 15 to 40 wt .-%, each based on the surfactant granules.
• the surfactant granules can be used in the detergent tablets in varying amounts. Processes according to the invention in which the proportion of the surfactant Granules containing the detergent tablets 40 to 95 wt .-%, preferably 45 to 85 wt .-% and in particular 55 to 75 wt .-%, each based on the weight of the detergent tablets, are preferred .
• the surfactant granules used in the process according to the invention contain a zeolite of the P and / or X type.
• Zeolite P belongs to the zeolite structure group 1 (compare Donald W. Breck: "Zeolite Molecular Sieves", John Wiley & Sons, New York, London, Sydney, Toronto, 1974, page 72) and can by the secondary formation unit of a single four-ring (S4R).
• the zeolites of the zeolite structure group 1 are interchangeable, so that, in addition to the synthetic zeolite P, the mineral or synthetic zeolites Analcime, Wairakit, Viseit, Kehoeit, Harmotom, Phillipsit, Gismondin, Garronit, Paulingit, Laumonit and Yugawaralit can be used as a P-type zeolite.
• pure zeolite P is preferably used, which can be described by the formula Na 6 [(AlO 2 ) 6 (SiO 2 ) 10 ] '15 H 2 O.
• the two most common types of zeolite P are a cubic and a tetragonal modification, whereby the cubic zeolite P is also referred to in the literature as zeolite B or zeolite P c , while the teragonal type is called P t .
• Zeolite P preferably has a density of 2.01 "3 , and the structure has a void volume of 41%.
• the three-dimensional network of the zeolite P used in the process according to the invention has pores of 2.6 ⁇ (dehydrated) or 3.1 '4.4 ⁇ and 2.8' 4.9 ⁇ (hydrated) Zeolite MAP® (commercial product from Crosfield) is particularly preferred as zeolite P.
• the mineral faujasite belongs to the faujasite types within the zeolite structure group 4, which is characterized by the double six-ring subunit D6R (compare Donald W. Breck: "Zeolite Molecular Sieves", John Wiley & Sons, New York, London, Sydney, Toronto, 1974, page 92).
• D6R double six-ring subunit
• the latter two synthetic zeolites have no mineral analogues. All of the representatives of the zeolite structure group 4 mentioned can be exchanged for the zeolite X in the context of the present, whereby, as with the P-type zeolites, the use of the zeolite X is clearly preferred.
• Faujasite-type zeolites are made up of ß-cages which are tetrahedral linked by D6R subunits, the ß-cages being arranged similar to the carbon atoms in the diamond.
• the three-dimensional network of the faujasite-type zeolites used in the process according to the invention has pores of 2.2 and 7.4 ⁇ , the unit cell also contains 8 cavities with a diameter of approximately 13 ⁇ and can be determined using the formula Na 86 [(AlO 2 ) 86 (SiO 2 ) 106 ] '264 H 2 O.
• the network of zeolite X contains a void volume of approximately 50%, based on the dehydrated crystal, which represents the largest empty space of all known zeolites (zeolite Y: approx. 48% o void volume, faujasite: approx. 47% void volume). (All data from: Donald W. Breck: "Zeolite Molecular Sieves", John Wiley & Sons, New York, London, Sydney, Toronto, 1974, pages 145, 176, 177).
• Mixtures or cocrystallisates of zeolites of the P and / or X type with other zeolites which do not necessarily have to belong to the zeolite structural group 1 or 4 can be used according to the invention, the advantages of the process according to the invention being particularly evident if at least 50 wt .-% of the zeolite contained in the surfactant granules consist of one or more zeolites of the P and / or X type.
• the aluminum silicates used in the process according to the invention are commercially available and the methods for their preparation are described in standard monographs.
• Examples of commercially available X-type zeolites can be described by the following formulas: Na 86 [(AlO 2 ) 86 (SiO 2 ) 106 ] - ⁇ H 2 O,
• x can have values between 0 and 276 and the pore sizes range from 8.0 to 8.4 ⁇ .
• zeolite X and zeolite A (ca. 80 wt .-% zeolite X) which is marketed by CONDEA Augusta SpA under the trade name VEGOBOND AX ® and through the formula
• the P and / or X type zeolite content of the surfactant-containing granules can vary depending on other optional ingredients.
• methods are preferred in which the content of zeolite P and / or zeolite X in the granules containing surfactant is 20 to 80% by weight, preferably 25 to 70% by weight and in particular 30 to 50% by weight, each based on the surfactant granules.
• the surfactant granules containing zeolite P and / or X are then mixed with further preparation components to form a premix which can then be pressed into detergent tablets.
• the premix to be treated can be used as processing components, as well as other ingredients customary in washing and cleaning agents, in particular from Group of builders, disintegration aids, bleaching agents, bleach activators, enzymes, pH regulators, fragrances, perfume carriers, fluorescent agents, dyes, foam inhibitors, silicone oils, anti-redeposition agents, optical brighteners, graying inhibitors, color transfer inhibitors and corrosion inhibitors.
• the washing and cleaning agent shaped bodies according to the invention can contain all of the builders normally used in washing and cleaning agents, in particular thus zeolites, silicates, carbonates, organic cobuilders and - where there are no ecological prejudices against their use - the phosphates.
• Suitable crystalline, layered sodium silicates have the general formula NaMSi x O 2x + 1 'H 2 O, where M is sodium or hydrogen, x is a number from 1.9 to 4 and y is a number from 0 to 20 and preferred values for x 2, 3 or 4.
• M sodium or hydrogen
• x is a number from 1.9 to 4
• y is a number from 0 to 20 and preferred values for x 2, 3 or 4.
• Such crystalline layered silicates are described, for example, in European patent application EP-A-0 164 514.
• Preferred crystalline layered silicates of the formula given are those in which M represents sodium and x assumes the values 2 or 3.
• both ⁇ - and ⁇ -sodium disilicate Na 2 Si 2 O 5 "yH 2 O are preferred, wherein ⁇ -sodium disilicate can be obtained, for example, by the method described in international patent application WO-A-91/08171 .
• the delay in dissolution compared to conventional amorphous sodium silicates can be caused in various ways, for example by surface treatment, compounding, compacting / compression or by overdrying.
• the term “amo ⁇ h” is also understood to mean “roentgenamo ⁇ h”.
• silicates in X-ray diffraction experiments do not provide sharp X-ray reflections as are typical for crystalline substances, but at most one or more maxima of the scattered ones X-rays having a width of several degree units of the diffraction angle.
• it can very well lead to particularly good builder properties if the silicate particles provide washed-out or even sharp diffraction maxima in electron diffraction experiments.
• This is to be integrated in such a way that the products have microcrystalline areas of size 10 to a few hundred nm, values up to max. 50 nm and in particular up to max. 20 nm are preferred.
• Such so-called X-ray amorphous silicates which also have a delay in dissolution compared to conventional water glasses, are described, for example, in German patent application DE-A-44 00 024. Particularly preferred are compressed / compacted amorphous silicates, compounded amorphous silicates and over-dried X-ray silicates.
• zeolite of the P and / or X type introduced by the surfactant granules can be inco ⁇ orated into the premix by adding zeolite as a treatment component.
• the finely crystalline, synthetic and bound water-containing zeolite used is preferably a type A, P, X or Y zeolite.
• zeolite X and mixtures of A, X and / or P are also suitable.
• Suitable zeolites have an average particle size of less than 10 ⁇ m (volume distribution; measurement method: Coulter Counter) and preferably contain 18 to 22% by weight, in particular 20 to 22% by weight, of bound water.
• phosphates as builder substances, provided that such use should not be avoided for ecological reasons.
• the sodium salts of orthophosphates, pyrophosphates and in particular tripolyphosphates are particularly suitable.
• Usable organic builders are, for example, the polycarboxylic acids which can be used in the form of their sodium salts, such as citric acid, adipic acid, succinic acid, glutaric acid, tartaric acid, sugar acids, aminocarboxylic acids, nitrilotriacetic acid (NTA), provided that such use is not objectionable for ecological reasons, and mixtures of these this.
• Preferred salts are the salts of polycarboxylic acids such as citric acid, Adipic acid, succinic acid, glutaric acid, tartaric acid, sugar acids and mixtures of these.
• tablet disintegrants In order to facilitate the disintegration of highly compressed moldings, it is possible to incorporate disintegration aids, so-called tablet disintegrants, in order to shorten the disintegration times.
• tablet disintegrants or accelerators of decay are understood as auxiliary substances which are necessary for rapid disintegration of tablets in water or gastric juice and ensure the release of the pharmaceuticals in absorbable form.
• Preferred detergent tablets contain 0.5 to 10% by weight, preferably 3 to 8% by weight and in particular 4 to 6% by weight of a disintegration aid, in each case based on the molded article weight.
• Disintegrants based on cellulose are used as preferred disintegrants in the context of the present invention, so that preferred detergent tablets form such a disintegrant based on cellulose in amounts of 0.5 to 10% by weight, preferably 3 to 8% by weight and in particular Contain 4 to 6 wt .-%.
• Pure cellulose has the formal gross composition (C 6 H 10 O 5 ) n and, viewed formally, is a ß-1,4-polyacetal of cellobiose, which in turn consists of two Molecules of glucose is built up. Suitable celluloses consist of approximately 500 to 5000 glucose units and consequently have average molecular weights of 50,000 to 500,000.
• Cellulose-based disintegrants which can be used in the context of the present invention are also cellulose derivatives which can be obtained from cellulose by polymer-analogous reactions.
• Such chemically modified celluloses include, for example, products from esterifications or etherifications in which hydroxyl hydrogen atoms have been substituted.
• celluloses in which the hydroxyl groups have been replaced by functional groups which are not bound via an oxygen atom can also be used as cellulose derivatives.
• the group of cellulose derivatives includes, for example, alkali celluloses, carboxymethyl cellulose (CMC), cellulose esters and ethers and aminocelluloses.
• the cellulose derivatives mentioned are preferably not used alone as a cellulose-based disintegrant, but are used in a mixture with cellulose.
• the content of cellulose derivatives in these mixtures is preferably below 50% by weight, particularly preferably below 20% by weight, based on the cellulose-based disintegrant. Pure cellulose which is free of cellulose derivatives is particularly preferably used as the cellulose-based disintegrant.
• Microcrystalline cellulose can be used as a further cellulose-based disintegrant or as a component of this component.
• This microcrystalline cellulose is obtained by partial hydrolysis of celluloses under conditions which only attack and completely dissolve the amorphous areas (approx. 30% of the total cellulose mass) of the celluloses, but leave the crystalline areas (approx. 70%) undamaged.
• a subsequent disaggregation of the microfine celluloses resulting from the hydrolysis provides the microcrystalline celluloses, which have primary particle sizes of approximately 5 ⁇ m and can be compacted, for example, to granules with an average particle size of 200 ⁇ m.
• the premix to be treated has a bulk density. points that comes close to the usual compact detergent.
• the premix to be ve ⁇ ress has a bulk density of at least 500 g / 1, preferably at least 600 g / 1 and in particular above 700 g / 1.
• bleaching agents that serve as bleaching agents and supply H 2 O 2 in water
• sodium perborate tetrahydrate and sodium perborate monohydrate are of particular importance.
• Further bleaching agents that can be used are, for example, sodium percarbonate, peroxypyrophosphates, citrate perhydrates and H 2 O 2 -producing peracid salts or peracids, such as perbenzoates, peroxophthalates, diperazelaic acid, phthaloiminoperacid or diperdodecanedioic acid.
• Even when using the bleaching agents it is possible to dispense with the use of surfactants and / or builders, so that pure bleach tablets can be produced.
• bleaching agents from the group of organic bleaching agents can also be used.
• Typical organic bleaching agents are the diacyl peroxides, such as dibenzoyl peroxide.
• Other typical organic bleaching agents are peroxy acids, examples of which include alkyl peroxy acids and aryl peroxy acids.
• Preferred representatives are (a) peroxybenzoic acid and its ring-substituted derivatives, such as alkylperoxybenzoic acids, but also peroxy- ⁇ -naphthoic acid and magnesium monophthalate, (b) the aliphatic or substituted aliphatic peroxyacids, such as peroxylauric acid, peroxystearic acid, ⁇ -phthalimidopercapid [Phthaloiminoperoxyhexanoic acid (PAP)], o-carboxybenzamidoperoxycaproic acid, N-nonenylamidoperadipic acid and N-nonenylamidopersuccinate, and (c) aliphatic and araliphatic peroxydicarboxylic acids, such as 1,12-diperoxycarboxylic acid, 1, 9-diperoxyacelysacidacidacidacid, 2-decyldiperoxybutane-1,4-diacid, N, N-terephthaloy
• Chlorine or bromine-releasing substances can also be used as bleaching agents in molded articles for automatic dishwashing.
• appropriate chlorine or bromine releasing materials come, for example, heterocyclic N-bromo- and N-chloramides, for example trichloroisocyanuric acid, tribromoisocyanuric acid,
• Dibromo isocyanuric acid and / or dichloroisocyanuric acid (DICA) and / or their salts with cations such as potassium and sodium are considered.
• Hydantoin compounds such as 1,3-dichloro-5,5-dimethylhydanthoin are also suitable.
• bleach activators can be incorporated as the sole component or as an ingredient of component b).
• Compounds which, under perhydrolysis conditions, give ahphatic peroxocarboxylic acids with preferably 1 to 10 C atoms, in particular 2 to 4 C atoms, and / or optionally substituted perbenzoic acid can be used as bleach activators.
• Suitable substances are those which carry O- and / or N-acyl groups of the number of carbon atoms mentioned and / or optionally substituted benzoyl groups.
• Multi-acylated alkylenediamines in particular tetraacetylethylene diamine (TAED), acylated triazine derivatives, in particular 1,5-diacetyl-2,4-dioxohexahydro-1,3,5-triazine (DADHT), acylated glycolurils, in particular tetraacetylglycoluril (TAGU), N- Acylimides, especially N-nonanoylsuccinimide (NOSI), acylated phenolsulfonates, especially n-nonanoyl- or isononanoyloxybenzenesulfonate (n- or iso-NOBS), carboxylic acid anhydrides, especially phthalic anhydride, acylated polyhydric alcohols, especially triacetate, ethylene glycol, Diacetoxy-2,5-dihydrofuran.
• TAED tetraacetylethylene diamine
• DADHT 1,5
• bleach catalysts can also be incorporated into the moldings.
• These substances are bleach-enhancing transition metal salts or transition metal complexes such as, for example, Mn, Fe, Co, Ru or Mo salt complexes or carbonyl complexes.
• Mn, Fe, Co, Ru, Mo, Ti, V and Cu complexes with N-containing tripod ligands as well as Co, Fe, Cu and Ru amine complexes can also be used as bleaching catalysts.
• Suitable enzymes are those from the class of proteases, lipases, amylases, cellulases or mixtures thereof.
• Enzymes obtained from bacterial strains or fungi such as Bacillus subtilis, Bacillus licheniformis and Streptomyces griseus are particularly suitable. Proteases of the subtilisin type and in particular proteases which are obtained from Bacillus lentus are preferably used. Enzyme mixtures, for example of protease and amylase or protease and lipase or protease and cellulase or of cellulase and lipase or of protease, amylase and lipase or protease, lipase and cellulase, but in particular mixtures containing cellulase, are of particular interest. Peroxidases or oxidases have also proven to be suitable in some cases.
• the enzymes can be adsorbed on carriers and / or embedded in coating substances in order to protect them against premature decomposition.
• the proportion of enzymes, enzyme mixtures or enzyme granules in the shaped bodies according to the invention can be, for example, about 0.1 to 5% by weight, preferably 0.1 to about 2% by weight.
• the detergent tablets can also contain components that positively influence the oil and fat washability from textiles (so-called soil repellents). This effect becomes particularly clear when a textile is soiled that has already been washed several times beforehand with a detergent according to the invention which contains this oil and fat-dissolving component.
• the preferred oil and fat-dissolving components include, for example, nonionic cellulose ethers such as methyl cellulose and methyl hydroxypropyl cellulose with a proportion of methoxyl groups of 15 to 30% by weight and of hydroxypropoxyl groups of 1 to 15% by weight, in each case based on the nonionic cellulose ether and the polymers of phthalic acid and / or terephthalic acid or their derivatives known from the prior art, in particular polymers of ethylene terephthalates and or polyethylene glycol terephthalates or anionically and / or nonionically modified derivatives thereof. Of these, the sulfonated derivatives of phthalic acid and terephthalic acid polymers are particularly preferred.
• the shaped bodies can contain derivatives of diaminostilbenedisulfonic acid or their alkali metal salts as optical brighteners. Suitable are, for example, salts of 4,4'-bis (2-anilino-4-mo ⁇ holino-l, 3,5-triazinyl-6-amino) stilbene-2,2'-disulfonic acid or compounds of similar structure which instead of the Mo ⁇ holino- Group carry a diethanolamino group, a methylamino group, an anilino group or a 2-methoxyethylamino group.
• Brighteners of the substituted diphenylstyryl type may also be present, for example the alkali salts of 4,4'-bis (2-sulfostyryl) diphenyl, 4,4'-bis (4-chloro-3-sulfostyryl) diphenyl, or 4- (4-chlorostyryl) -4 '- (2-sulfostyryl) diphenyl. Mixtures of the aforementioned brighteners can also be used.
• Dyes and fragrances are added to the detergent tablets according to the invention in order to improve the aesthetic impression of the products and, in addition to the softness, provide the consumer with a visually and sensorially "typical and unmistakable" product.
• Individual fragrance compounds for example the synthetic products of the ester, ether, aldehyde, ketone, alcohol and hydrocarbon type, can be used as perfume oils or fragrances.
• Fragrance compounds of the ester type are, for example, benzyl acetate, phenoxyethyl isobutyrate, p-tert-butylcyclohexyl acetate, linalyl acetate, dimethylbenzyl-carbinyl acetate, phenylethyl acetate, linalyl benzoate, benzyl formate, ethyl methylphenyl glycate, allyl cyclohexyl propyl propylate loxyl propyl.
• the ethers include, for example, benzylethyl ether, the aldehydes, for example, the linear alkanals with 8-18 C atoms, citral, citronellal, citronellyloxyacetaldehyde, cyclamenaldehyde, hydroxycitronellal, lilial and bourgeonal, the ketones, for example, the jonones, cc -Isomethyl ionone and methyl cedryl ketone, the alcohols anethole, citronellol, eugenol, geraniol, linalool, phenylethyl alcohol and te ⁇ ineol, the hydrocarbons mainly include tephenols such as limonene and pinene.
• Perfume oils of this type can also contain natural fragrance mixtures such as are obtainable from plant sources, for example pine, citrus, jasmine, patchouly, rose or ylang-ylang oil. Also suitable are muscatel, sage oil, chamomile oil, clove oil, lemon balm oil, mint oil, cinnamon leaf oil, linseed oil denflower oil, juniper berry oil, vetiver oil, olibanum oil, galbanum oil and labdanum oil as well as orange blossom oil, neroliol, orange peel oil and sandalwood oil.
• the dye content of the plasticizers according to the invention is usually below 0.01% by weight, while fragrances can make up up to 2% by weight of the entire formulation.
• the fragrances can be incorporated directly into the agents according to the invention, but it can also be advantageous to apply the fragrances to carriers which increase the adhesion of the perfume to the laundry and ensure a long-lasting fragrance of the textiles due to a slower fragrance release.
• Cyclodextrins for example, have proven useful as such carrier materials, and the cyclodextrin-perfume complexes can additionally be coated with further auxiliaries.
• the agents according to the invention can be colored with suitable dyes.
• Preferred dyes the selection of which is not difficult for the person skilled in the art, have a high storage stability and insensitivity to the other ingredients of the compositions and to light, and no pronounced substantivity to textile fibers, in order not to dye them.
• the premix Before the particulate premix is pressed into detergent tablets, the premix can be "powdered” with finely divided surface treatment agents. This can be of advantage for the quality and physical properties of both the premix (storage, pressing) and the finished detergent tablets.
• Finely divided powdering agents are well known in the art, mostly zeolites, silicates or other inorganic salts being used.
• the premix is preferably “powdered” with finely divided zeolite, zeolites of the faujasite type being preferred.
• the term “faujasite-type zeolite” denotes all three zeolites which form the faujasite subgroup of the zeolite structure group 4 (see Donald W.
• the or one of the subsequently mixed fine-particle treatment components is a faujasite-type zeolite with particle sizes below 100 ⁇ m, preferably below 100 ⁇ m and in particular below 5 ⁇ m and at least 0.1 2% by weight, preferably at least 0.5% by weight and in particular more than 1% by weight of the premix to be treated.
• the premix is compacted in a so-called die between two punches to form a solid compact.
• This process which is briefly referred to as tableting in the following, is divided into four sections: metering, compression (elastic deformation), plastic deformation and ejection.
• the premix is introduced into the die, the filling quantity and thus the weight and the shape of the molded body being formed being determined by the position of the lower punch and the shape of the pressing tool.
• the constant dosing, even at high mold throughputs, is preferably achieved by volumetric dosing of the premix.
• the upper punch touches the premix and lowers further in the direction of the lower punch.
• the particles of the premix are pressed closer together, the void volume within the filling between the punches continuously decreasing. From a certain position of the upper punch (and thus from a certain pressure on the premix), the plastic deformation begins, in which the particles flow together and the molded body is formed.
• the premix particles are also crushed and sintering of the premix occurs at even higher pressures.
• the phase of the elastic deformation is shortened further and further, so that the resulting molded body more or may have smaller cavities.
• the finished molded body is pressed out of the die by the lower punch and transported away by subsequent transport devices. At this point in time, only the weight of the molded body is finally determined, since the compacts can still change their shape and size due to physical processes (stretching, crystallographic effects, cooling, etc.).
• Tableting takes place in commercially available tablet presses, which can in principle be equipped with single or double punches. In the latter case, not only is the upper stamp used to build up pressure, the lower stamp also moves towards the upper stamp during the pressing process, while the upper stamp presses down.
• eccentric tablet presses are preferably used, in which the punch or stamps are fastened to an eccentric disc, which in turn is mounted on an axis with a certain rotational speed. The movement of these rams is comparable to that of a conventional four-stroke engine.
• the pressing can take place with one upper and one lower punch, but several punches can also be attached to one eccentric disk, the number of die holes being increased accordingly.
• the throughputs of eccentric presses vary depending on the type from a few hundred to a maximum of 3000 tablets per hour.
• rotary tablet presses are selected in which a larger number of dies is arranged in a circle on a so-called die table.
• the number of matrices varies between 6 and 55 depending on the model, although larger matrices are also commercially available.
• Each die on the die table is assigned an upper and lower punch, and again the pressure can be built up actively only by the upper or lower punch, but also by both stamps.
• the die table and the stamps move about a common vertical axis, the stamps being brought into the positions for filling, compaction, plastic deformation and ejection by means of rail-like cam tracks during the rotation.
• these cam tracks are before supporting low-pressure pieces, low-tension rails and lifting tracks.
• the die is filled via a rigidly arranged feed device, the so-called filling shoe, which is connected to a storage container for the premix.
• the pressing pressure on the premix can be individually adjusted via the pressing paths for the upper and lower punches, the pressure being built up by rolling the punch shaft heads past adjustable pressure rollers.
• Rotary presses can also be provided with two filling shoes to increase the throughput, with only a semicircle having to be run through to produce a tablet.
• several filling shoes are arranged one behind the other without the slightly pressed first layer being ejected before further filling.
• jacket and dot tablets can also be produced in this way, which have an onion-shell-like structure, the top side of the core or the core layers not being covered in the case of the dot tablets and thus remaining visible.
• Rotary tablet presses can also be equipped with single or multiple tools, so that, for example, an outer circle with 50 and an inner circle with 35 holes can be used simultaneously for pressing.
• the throughputs of modern rotary tablet presses are over one million molded articles per hour.
• Tableting machines suitable within the scope of the present invention are available, for example, from the companies Apparatebau Holzwarth GbR, Asperg, Wilhelm Fette GmbH, Schwarzenbek, Hofer GmbH, Weil, KILIAN, Cologne, KOMAGE, Kell am See, KORSCH Pressen GmbH, Berlin, Mapag Maschinenbau AG, Bern (CH) and Courtoy NV, Halle (BE / LU).
• the hydraulic double pressure press HPF 630 from LAEIS, D. is particularly suitable.
• the molded body can be manufactured in a predetermined spatial shape and a predetermined size. Practically all sensibly manageable configurations come into consideration as the spatial form, for example the design as a board, the rod or bar form, cubes, cuboids and corresponding spatial elements with flat side surfaces and in particular cylindrical configurations with a circular or oval cross section. This last embodiment covers the presentation form from the tablet to compact cylinder pieces with a ratio of height to diameter above 1.
• the portioned compacts can each be designed as separate individual elements that correspond to the predetermined dosage of the detergents and / or cleaning agents. It is also possible, however, to form compacts which connect a plurality of such mass units in one compact, the portioned smaller units being easy to separate, in particular by predetermined predetermined breaking points.
• the portioned compacts as tablets, in cylinder or cuboid form can be expedient, with a diameter / height ratio in the range from about 0.5: 2 to 2: 0.5 is preferred.
• Commercial hydraulic presses, eccentric presses or rotary presses are suitable devices, in particular for the production of such pressed articles.
• the spatial shape of another embodiment of the molded body is adapted in its dimensions to the detergent dispenser of commercially available household washing machines, so that the molded body can be metered directly into the dispenser without metering aid, where it dissolves during the dispensing process.
• the detergent tablets without problems using a metering aid and is preferred in the context of the present invention.
• Another preferred molded body that can be produced has a plate-like or plate-like structure with alternating thick long and thin short segments, so that individual segments of this "bolt" at the predetermined breaking points, which represent the short thin segments, broken off and into the Machine can be entered.
• This principle of the "bar-shaped" shaped body detergent can also be realized in other geometric shapes, for example vertically standing triangles, which are connected to one another only on one of their sides along the side.
• the various components are not pressed into a uniform tablet, but that shaped bodies are obtained which have several layers, that is to say at least two layers. It is also possible that these different layers have different dissolving speeds. This can result in advantageous application properties of the molded body.
• the layer structure of the molded body can take place in a stack-like manner, with the inner layer (s) already loosening at the edges of the molded body when the outer layers have not yet been completely removed, but it is also possible for the inner layer (s) to be completely encased ) can be achieved by the layer (s) lying further outwards, which leads to the premature dissolution of components of the inner layer (s).
• a molded body consists of at least three layers, i.e. two outer and at least one inner layer, at least one of the inner layers containing a peroxy bleaching agent, while in the case of the stacked molded body the two cover layers and in the case of the shell-shaped molded body the outermost layers, however, are free of peroxy bleach. Furthermore, it is also possible to spatially separate peroxy bleaching agents and any bleach activators and / or enzymes that may be present in a molded body.
• Such multilayer molded bodies have the advantage that they can be used not only via a dispensing chamber or via a metering device which is added to the washing liquor; rather, in such cases it is also possible to put the molded body into direct contact with the textiles in the machine without the risk of bleaching from bleaching agents and the like. Similar effects can also be achieved by coating individual constituents of the detergent and cleaning agent composition to be treated or the entire molded article.
• the bodies to be coated can, for example, be sprayed with aqueous solutions or emulsions, or else they can be coated using the melt coating method.
• the breaking strength of cylindrical shaped bodies can be determined via the measured variable of the diametrical breaking load. This can be determined according to
• ⁇ stands for diametral fracture stress (DFS) in Pa
• P is the force in N that leads to the pressure exerted on the molded body that causes the molded body to break
• D is the molded body diameter in meters and t the height of the molded body.
• Another object of the present invention is the use of zeolite of the P and / or X type in surfactant-containing granules which, after being mixed with finely divided preparation components, are pressed in a manner known per se to form detergent and shaped bodies for improving stability and solubility of detergent tablets.
• zeolite of the P and / or X type in surfactant-containing granules which, after being mixed with finely divided preparation components, are pressed in a manner known per se to form detergent and shaped bodies for improving stability and solubility of detergent tablets.
• a polymer compound was produced by spray drying and was used as the basis for a granulate containing tenside.
• the tower powder was granulated with other components (zeolite, fatty alcohol sulfate, NaOH, anionic surfactant, nonionic surfactant, silicate, polymer) in a 50 liter ploughshare mixer from Lödige.
• the amounts of the solids and liquids used and the order of addition to the mixer are given in Table 3.
• Zeolite P and X were used in the granulation batches El and E2 according to the invention; in comparative example V, the surfactant granules were produced using zeolite A.
• the granules were dried in a fluidized bed apparatus from Glatt at a supply air temperature of 60 ° C. over a period of 30 minutes. After drying, fine particles ⁇ 0.6 mm and coarse particles> 1.6 mm were screened off. To determine the water content of the granules, each 2 g of the granules were heated for 10 minutes at 130 ° C. on an MA 30 device from Sartorius and the drying loss was determined gravimetrically.
• the surfactant granules E1 and E2 or VI were then prepared with further components to form a compressible premix, after which the pressing into tablets (diameter: 44 mm, height: 22 mm, weight: 37.5 g) was carried out in a Korsch eccentric press . The pressure was adjusted so that two series of molded bodies were obtained (El, E2 and VI or El ', E2' and VI '), which differ in their hardness.
• the composition of the spray-dried polymer compound is shown in Table 1, and the composition of the premixes to be treated (and thus the molded article) is shown in Table 4.
• Table 1 Composition of the polymer compound [% by weight>]
• Sokalan ® CP5 is an acrylic acid-malien acid copolymer from BASF AG, Ludwigshafen
• composition 92 wt .-% C 12 _, 8 fatty alcohol sulfate 3 wt .-% of sodium carbonate 5 wt .-% water, salts
• the hardness of the tablets was measured by deforming the tablet until it broke, the force acting on the side surfaces of the tablet and the maximum force which the tablet withstood being determined.
• the detergent tablets that contain a surfactant-containing granulate which contain a zeolite of the P or X type, disintegrate significantly faster than detergent tablets; in which the surfactant granules used are zeolite A-based.

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• 1998
  • 1998-06-26 DE DE19828577A patent/DE19828577A1/de not_active Withdrawn
• 1999
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