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
  • C11D3/39—Organic or inorganic per-compounds
  • C11D3/3902—Organic or inorganic per-compounds combined with specific additives
  • C11D3/3905—Bleach activators or bleach catalysts
  • C11D3/3907—Organic compounds
• • 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
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/02—Anionic compounds
  • C11D1/04—Carboxylic acids or salts thereof
  • C11D1/10—Amino carboxylic acids; Imino carboxylic acids; Fatty acid condensates thereof
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/38—Cationic compounds
  • C11D1/42—Amino alcohols or amino ethers
  • C11D1/44—Ethers of polyoxyalkylenes with amino alcohols; Condensation products of epoxyalkanes with amines
• • 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
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/38—Cationic compounds
  • C11D1/62—Quaternary ammonium compounds
• • 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
  • C11D17/0039—Coated compositions or coated components in the compositions, (micro)capsules
• • 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
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/39—Organic or inorganic per-compounds
  • C11D3/3902—Organic or inorganic per-compounds combined with specific additives
  • C11D3/3905—Bleach activators or bleach catalysts
  • C11D3/3935—Bleach activators or bleach catalysts granulated, coated or protected

Definitions

• the present invention relates to a process for the preparation of a washing additive with active ingredients for improving the washability of bleachable stains, of greasy or oily stains and of pigment stains, the washing additive being obtained in the form of a tablet in the production by the process according to the invention.
• the detergent tablets often contain, as active ingredients, alone or in combination with other active ingredients and conventional tabletting aids, a bleach activator for per compounds.
• a bleach activator for per compounds.
• Such a product is described for example in DE-OS 22 63 939.
• Bleach activators in combination with the compounds normally found in modern universal detergents, improve the removal of bleachable stains.
• the detergents In addition to per-compounds, the detergents generally also contain bleach activators; When storing the detergents which contain per-compounds and activators at the same time, difficulties often arise because the bleach activator acts prematurely on the per-compounds and thus becomes one Per compounds may lose their effectiveness.
• washing additives which, in addition to a bleach activator, additionally contain nonionic surfactants, certain quaternary ammonium compounds for strengthening the washing power and, if appropriate, organic phosphonic acid derivatives (see DE-OS 28 57 153).
• the last-mentioned patent application relates to washing additives in which the active ingredient combination mentioned is applied to a flexible carrier.
• the carrier loaded with active substances is added to the washing machine when washing the laundry, where it develops its effect in the course of the washing process. After the washing process has ended, the flexible carrier for the active ingredients remains in the laundry and must be sorted out from it.
• Tablet-like washing additives are often sensitive to mechanical stress or they do not dissolve quickly enough or only incompletely if the tablet composition and preparation are chosen so that the tablets are mechanically sufficiently stable.
• the object of the present invention is therefore to provide a process for the preparation of a washing additive in tablet form, in which an activator for per compounds and customary tableting aids are mixed with one another and molded.
• the washing additive according to the invention is intended to contain the active ingredients in coordinated proportions and in terms of their capacity contain a coordinated amount in a washing machine and do not have to be removed from the laundry after washing.
• the washing additive should also be so stable that it can be handled comfortably; it must also dissolve quickly and completely in the wash liquor.
• the powdered activator is granulated together with nonionic surfactants, with nitrogen-containing compounds from the group comprising quaternary ammonium compounds, fatty amine derivatives or aminopropionic acid derivatives, with the tabletting aids and, if appropriate, with the water-soluble salt of an alkane polyphosphonic acid, with the granules being mixed powdered a powdered adsorbent and sprayed with a liquid binder, then drying the granules to a water content of at most 6 wt .-% and from this after adding a tablet disintegrant tablets, their shape, weight and density is selected so that the tablets one for a wash have sufficient content of active ingredients to increase washing power and the tablets are circulated from the laundry items during the washing process, so that the tablets dissolve quickly and completely, presses.
• the features of the method according to the invention ensure that on the one hand the tablet has a stability which prevents the tablet from disintegrating before use in the washing machine.
• washing additives produced according to the invention in the washing machine have sufficient security against dissolution.
• the procedural measures also result in tablets being obtained which ensure perfect storage over a long period even in the moist air of a laundry room.
• the powdering and spraying of the granules with a liquid binder also has the effect that the surface of the granules containing the active ingredients is largely or completely covered.
• a granulate containing the active ingredients is first prepared, which optionally additionally contains a water-soluble or water-insoluble powdery carrier material for the liquid or pasty active ingredient components and optionally a granule disintegrant.
• This granulate therefore already contains all active ingredients and, in addition, aids that serve the safe manufacture and handling.
• the granulate can be produced by known granulation processes, for example in a mixer or in a fluidized bed.
• a mixer from Lödige, Paderborn, Federal Republic of Germany has proven itself.
• the liquid or dissolved active ingredients or auxiliaries liquefied or liquefied by heating are preferably sprayed onto the powdered active ingredients or auxiliaries. It forms a granulate that contains all the active ingredients, which will be discussed in more detail later, and some auxiliary substances, such as.
• a granule disintegrant causes the granule grain to disintegrate more quickly in the wash liquor and is therefore preferred. In many cases, it is advisable to mix up to 30 seconds after the granulate has formed; post-mixing for longer than a maximum of 30 seconds often leads to pulpy products.
• The. Finished granules, which should contain no or only small amounts of dust-fine fractions, are then dusted with a finely divided inert material and / or a finely divided adsorbent, for example highly disperse silica and / or starch, e.g. B. potato starch and then sprayed a liquid binder, such as a sugar solution.
• a finely divided inert material and / or a finely divided adsorbent for example highly disperse silica and / or starch, e.g. B. potato starch and then sprayed a liquid binder, such as a sugar solution.
• the active ingredient granules are coated with a protective layer of binder and sugar that is largely or completely closed after drying.
• a tablet disintegrant is added to the dried granules, combinations of two different tablet disintegrants having proven particularly useful. The addition of a tablet disintegrant causes the tablet to disintegrate quickly into the granules when the tablet comes into contact with the wash liquor. After mixing with tablet disintegrant, the tablets are compressed.
• the pressing tools are expediently polished in order to prevent sticking. However, it is advantageous to use pressing tools that are coated with a non-stick layer.
• the pressing conditions and the composition of the tablets ensure the mechanical stability on the one hand and the rapid disintegration of the tablets when used on the other.
• the process product contains a mixture of at least one activator for per-compounds, at least one C 12 to C 18 alcohol ethoxylate, at least one nitrogen-containing compound from the quaternary ammonium compounds with a C 10 to C 20 alkyl or alkenyl radical, and the rest C 1 - to C 4 -alkyl radicals, adducts of 1 to 6 mol of ethylene oxide with 1 mol of a primary fatty amine with a long-chain alkyl or alkenyl radical with 10 to 16 carbon atoms, ⁇ -aminoalkyl or alkenylpropionic acid sodium salt
• R-NH-CH 2 -CH 2 -COONa in which R is an alkyl or alkenyl group having 10 to 20 carbon atoms, in particular 12 to 14 carbon atoms, pe comprehensive Gru p-, which, if appropriate, with an aqueous solution of a water-soluble salt an alkane polyphosphonic acid granulated.
• N-acyl and 0-acyl compounds are suitable as activators for per compounds.
• Acetyl compounds have proven particularly useful. Examples include tetraacetylglycoluril or pentaacetylglucose or in particular tetraacetylethylenediamine.
• the bleach activators mentioned lead to an improved removal of bleachable textile soiling.
• Addition products of ethylene oxide with fatty alcohols or, in particular, oxo alcohols, which have 12 to 18, preferably 14 to 15, carbon atoms are particularly suitable as nonionic surfactants.
• the best effects are achieved with oxo alcohol ethoxylates which contain 3 to 10, preferably 6 to 8 and in particular about 7 moles of ethylene oxide per mole of alcohol.
• foam regulators most of the time, the development of foam must be dampened.
• Suitable foam suppressants are, for example, the known silicone oils.
• the content of nonionic surfactants in the washing additives according to the invention primarily promotes the removal of greasy or oily soiling during washing.
• Suitable quaternary ammonium compounds contain as long-chain alkyl or alkenyl radical with 10 to 20, preferably alkyl groups with 10 to 16 and in particular about 14 carbon atoms.
• the suitable quaternary ammonium compounds contain 3 identical or different alkyl groups with 1 to 4 carbon atoms. In particular, these short alkyl groups are methyl groups.
• a particularly suitable and therefore preferred quaternary ammonium compound is tetradecyltrimethylammonium bromide.
• All or part of the quaternary ammonium compound can be replaced by the above-mentioned fatty amine ethoxylate.
• An example of a particularly suitable fatty amine ethoxylate is the adduct of 2 moles of ethylene oxide with primary coconut alkyl amine; this product is therefore also preferred.
• a compound of the formula R-NH-CH 2 -CH 2 -COONa can also be used.
• a compound in which R is a cocoalkyl radical is preferred.
• the washing additive advantageously contains small amounts of chelating agents.
• Water-soluble salts of alkane polyphosphonic acid from the group of the phosphonoalkane polycarboxylic acids and the amino- and hydroxy-substituted alkane polyphosphonic acids, in particular the alkali salts of amino-tris (methylenephosphonic acid), dimethyleneaminomethane diphosphonic acids, have been particularly suitable for this purpose ; 1-hydroxyethane-1,1-diphosphonic acid, 1-phosphonoethane-1,2-dicarbon acid, 2-phosphonobutane-1,2,3-tricarboxylic acid and in particular the hexasodium salt of ethylenediaminotetramethylenephosphonic acid.
• the granules are produced from the active substances mentioned by focusing on the solids, ie. H. to the bleach activator and the quaternary ammonium compound, to which, for example, highly disperse silica and granule disintegrant, for example, as a powdery carrier material for the liquid or pasty active ingredients, the liquid or liquefied or dissolved active ingredients, i. H. sprayed on the nonionic surfactant and optionally the heavy metal complexing agents dissolved in water.
• a disintegrant suitable as a granule component is, for example, swellable magnesium aluminum silicate.
• the amount of disintegrant in the granules is preferably in the range from 1 to 5% by weight and in the base material in the range from 5 to 20% by weight, based in each case on the granules without a protective layer.
• the granules are covered with a protective layer.
• the granules are dusted with the finely divided inert material and / or the finely divided adsorbent, the dusted granules are sprayed with an aqueous sugar solution, in particular cane sugar or sorbitol solution, and the granules are dried.
• the granules contain about 50 to 90% by weight of active ingredient; the rest are auxiliary substances.
• the bulk density of the granules sieved through a 2 mm sieve is 600 to 700 g per liter.
• the granules coated and dried with a protective layer are preferably mixed with 10 to 20% by weight, based on the granules, of a tablet disintegrant, preferably a mixture of two different tablet disintegrants, in particular a mixture of crosslinked polyvinylpyrrolidone and / or cellulose ethers and / or swellable magnesium aluminum silicate .
• a tablet disintegrant preferably a mixture of two different tablet disintegrants, in particular a mixture of crosslinked polyvinylpyrrolidone and / or cellulose ethers and / or swellable magnesium aluminum silicate .
• the effect of a single tablet disintegrant can be increased by adding up to 7% by weight (based on the tablet weight) of an alkali salt of short-chain organic mono- or polycarboxylic acids, e.g. B. Na acetate or Na citrate can be increased.
• the tablet preparation is carried out by adding from the dried granulate at a pressure of 500 to 1000 kp / cm 2 tablets with a diameter of more than 30 mm and a height, the fold 1,1-0.75 to the tablet diameter, at least but is 25 mm, with a density of 0.8 to 1.2 g per cm3 and a breaking strength of 6 to 12 kg.
• the dried granules were then mixed gently with so much crosslinked polyvinylpyrrolidone (PVP) and sodium carboxymethyl cellulose (CMC) as tablet disintegrants that 80 parts by weight of granules account for 15 parts by weight of PVP and 5 parts by weight of CMC. This mixing took place in a Patterson-Kelley-Cron-Flow blender. A coated granulate with a bulk density of 535 g per liter was obtained.
• PVP polyvinylpyrrolidone
• CMC sodium carboxymethyl cellulose
• the tablets obtained dissolved within 6 minutes in a wash cycle with a 30 ° C wash program (Miele washing machine, type 430) without residue.
• the soiled laundry washed with it was significantly cleaner than without the addition of a detergent booster tablet despite the 2/3 nominal dosage of a cheap detergent.

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• 1984
  • 1984-05-14 DE DE19843417820 patent/DE3417820A1/de not_active Withdrawn
• 1985
  • 1985-05-06 AT AT85105496T patent/ATE36347T1/de not_active IP Right Cessation
  • 1985-05-06 DE DE8585105496T patent/DE3564286D1/de not_active Expired
  • 1985-05-06 EP EP85105496A patent/EP0170791B1/fr not_active Expired
  • 1985-05-13 ES ES543071A patent/ES8607382A1/es not_active Expired
  • 1985-05-13 US US06/733,669 patent/US4642197A/en not_active Expired - Fee Related
  • 1985-05-14 JP JP60103614A patent/JPS60252699A/ja active Pending

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