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
  • C11D17/06—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
  • C11D17/0047—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
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/04—Water-soluble compounds
  • C11D3/10—Carbonates ; Bicarbonates
• • 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
  • C11D3/2075—Carboxylic acids-salts thereof
  • C11D3/2082—Polycarboxylic acids-salts 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
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/16—Organic compounds
  • C11D3/20—Organic compounds containing oxygen
  • C11D3/2075—Carboxylic acids-salts thereof
  • C11D3/2086—Hydroxy carboxylic acids-salts 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
  • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
  • C11D7/02—Inorganic compounds
  • C11D7/04—Water-soluble compounds
  • C11D7/10—Salts
  • C11D7/12—Carbonates bicarbonates
• • 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
  • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
  • C11D7/22—Organic compounds
  • C11D7/26—Organic compounds containing oxygen
  • C11D7/265—Carboxylic acids or salts thereof

Definitions

• the invention relates to a method for producing a cobuilder-containing additive, which in particular in compressed washing or cleaning agents, for example in extruded agents, granules or tablets can be used.
• EP-A-0 737 738 (Cleantabs) described a percarbonate-containing tablet, which additionally 5 to 35 wt .-% citric acid and optionally also up to 25% by weight of bicarbonate and up to 8% by weight of polyethylene glycols may contain.
• German patent application DE-A-42 03 169 (BASF) describes a bleach activator granulate, containing benzoxazinone derivatives and 2 to 70% by weight of other conventional ingredients, to which, for example, surfactants, but also polymers, polysaccharides, polyalkylene glycols, neutral, alkaline or acidic salts of inorganic acids as well organic carboxylic acids are counted.
• Japanese patent application JP-A-02/255800 also discloses bleach activator granules with bleach activator contents of 10 to 85% by weight.
• As further ingredients are called nonionic surfactants, polyethylene glycol, citric acid and bicarbonate.
• Japanese patent application JP-A-58/213714 are active in washing or cleaning Tablets, also known as bathroom cleaners, which contain bicarbonate, polyethylene glycols a molecular weight between 2000 and 10000 and polycarboxylic acids.
• the bicarbonate is first mixed with the polyethylene glycol at temperatures melted between 60 and 100 ° C, then cooled, pulverized, with the polycarboxylic acid, especially citric acid, mixed, and then pressed.
• German patent application DE-A-38 25 317 (Lab. Hausmann), however, describes Powders or tablets, which are used as contact lens cleaners and which besides Hydrogen peroxide and manganese EDTA, especially alkali metal bicarbonate, citric acid and contain polyethylene glycol with a molecular weight of 6000.
• Roll compacting of detergents or cleaning agents or individual components of detergents or cleaning agents is a reliable state of the art. It is already known from European patent application EP-A-0 253 323 that builders such as zeolite and / or phosphate by roller compaction in granules with high Bulk weight and very good application properties are transferred can. Conditions are described in detail in this printed state of the art described under which a roller compaction is usually carried out. Here is carried out that the pressure in the nip and the residence time of the material in the area of the baling pressure are to be adjusted so that a well-formed band of cuffs is generated with high density.
• the high degree of compaction is not only in the With regard to modern washing or cleaning agents with high bulk density, but also desirable with regard to increased abrasion stability of the granules.
• excessive pressures impair the process reliability, because when used, the material is plasticized on the rollers and leads to sticking can lead. This undesirable effect occurs when there is an increase in pressure no further compression of the material and the now additionally entered Pressing force mainly the heating and plasticizing of the material, for example caused by partial melting of water-containing components. This is also the reason that roller compacting is usually not additional externally elevated temperatures, but at ambient temperature / room temperature be performed.
• the unpublished German patent application P 197 04 229.5 describes the use a powdery to granular additive for use in washing or Detergents for water softening of the washing or cleaning liquor and at the same time Promotion of foam formation in the liquor, with the additive bicarbonate and organic Contains polycarboxylic acids and a water-soluble binder, which is among the Processing conditions as a melt is present.
• the content of the additives is Bicarbonate, organic polycarboxylic acids and binders at least 60% by weight while the additive can contain surfactants in amounts of 0 to below 5% by weight.
• Such Additives have an excellent dissolving behavior in water and therefore contribute Improvement of the induction behavior, but also the dissolving behavior of detergents or cleaning agents for machine use.
• additives are manufactured in a mixer which is suitable for melt granulation or a coating process with a Melt is suitable, or by granulation in a fluidized bed.
• the one described here Granulation process has some disadvantages, for example, it is convenient Applicable amount of binder in a relatively narrow recipe window. Become too If small quantities are used, complete granulation cannot be achieved; in to High proportions of the binder become too much due to the heat capacity of the melt Energy entered into the system so that paste formation occurs.
• a relatively large amount of coarse grain is also formed in amounts of around 30% by weight. Usually coarse grain can be ground; but because the additive is meltable Binder can become sticky quickly when there is energy input, there is a risk of a technical Failure of the mill.
• the object of the invention was to provide an alternative method of manufacture to provide a cobuilder-containing additive which contains bicarbonate and one or more contains organic polycarboxylic acids. The above mentioned occurring in the manufacture Disadvantages should be avoided.
• the invention accordingly relates to a method for producing a powder to granular additives for use in detergents or cleaning agents, being a mixture containing at least 60% by weight of bicarbonate and one or more organic polycarboxylic acids, but contains no free water, a roller compaction is subjected.
• the roller compaction carried out according to customary methods has become as the procedure that best solves the tasks. So significantly less mixing energy is introduced into the system in roller compacting, which is why the recipe degrees of freedom are increased. Coarse grain fractions are also not formed, since the slug that forms in the roller compactor is usually direct is ground in a crusher. In this grinding step, the upper grain size can the choice of an appropriate sieve can be set directly. Besides, it is not required that a melt be present during the processing operation. binder can and must preferably be contained in the mixture to be compacted but can no longer be converted into a melt under the processing conditions be. Because therefore at lower temperatures, for example at room temperature to temperatures of a maximum of 40 ° C and thus heat energy can be saved, the method according to the invention is also less expensive.
• Both sodium bicarbonate and potassium bicarbonate can be used as bicarbonate in the additive be included, but sodium bicarbonate is preferred.
• the content of the additives of bicarbonate is preferably more than 25% by weight and is particularly advantageous Embodiments above 30 wt .-%.
• Organic polycarboxylic acids which can be used are those or their Salts usually as organic builders or cobuilders in detergents or cleaning agents are included. These include, for example, 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. Citric acid, succinic acid, Glutaric acid, adipic acid, gluconic acid and any mixtures of these, in particular but citric acid and optionally mixtures of citric acid with other polycarboxylic acids to call.
• polymeric polycarboxylic acids such as polyacrylic acid, Polymaleic acid or copolymers of acrylic acid, maleic anhydride and optionally vinyl acetate under this definition.
• polyacrylic acid Polymaleic acid or copolymers of acrylic acid, maleic anhydride and optionally vinyl acetate
• the use of these (co) polymeric polycarboxylic acids is clearly less preferred from today's perspective.
• the organic polycarboxylic acids in the additives are preferably in amounts of 20 Contain up to 60 wt .-% and in particular from 20 to 50 wt .-%. While it's due that described in the unpublished German patent application P 197 04 229.5 performed melt granulation was preferred over bicarbonate to use organic polycarboxylic acid, especially with respect to citric acid, plays the ratio of these two essential components in the invention Procedure doesn't matter. The recipe variability has increased. In particularly preferred process is now even the polycarboxylic acid, especially the Citric acid, used in excess over bicarbonate.
• a preferred embodiment of the invention provides that the content of the to be compacted Mixture of bicarbonate and organic polycarboxylic acids above 65 % By weight.
• Additives which are particularly preferred by the process according to the invention thus contain more than 30% by weight and up to 45% by weight of bicarbonate, in particular sodium bicarbonate, and advantageously 35 to 60% by weight, preferably up to 50% by weight anhydrous organic polycarboxylic acid, especially anhydrous citric acid or a coated anhydrous citric acid, especially one anhydrous coated with glucose syrup Citric acid.
• bicarbonate in particular sodium bicarbonate
• anhydrous organic polycarboxylic acid especially anhydrous citric acid or a coated anhydrous citric acid, especially one anhydrous coated with glucose syrup Citric acid.
• Another essential process parameter is that the process is carried out essentially anhydrous.
• Free water i.e. water that is not bound to a solid in any form and therefore is in liquid form "should not be contained in the mixture to be compacted.
• the constituents used in the process according to the invention are either solids both at room temperature and under the process conditions and, above all, no water is removed under the process conditions, or they are present Room temperature or non-aqueous liquids under the process conditions.
• the mixture to be compacted can also contain one or more binders.
• these binders do not represent any essential constituents of the mixture to be compacted.
• These are preferably water-soluble binders which are solid at temperatures below 30 ° C. and a pressure of 1 bar. which are used in a preferred embodiment in amounts of 2 to 20% by weight, in particular in amounts of 5 to 15% by weight.
• Preferred binders which can be used alone or in a mixture with other binders are polyethylene glycols, 1,2-polypropylene glycols and modified polyethylene glycols and polypropylene glycols.
• the modified polyalkylene glycols include in particular the sulfates and / or the disulfates of polyethylene glycols or polypropylene glycols with a relative molecular weight between 600 and 12000 and in particular between 1000 and 4000.
• Another group consists of mono- and / or disuccinates of the polyalkylene glycols, which in turn have relative molecular weights have between 600 and 6000, preferably between 1000 and 4000.
• polyethylene glycols include those polymers which, in addition to ethylene glycol, also use C 3 -C 5 glycols and glycerol and mixtures of these as starting molecules. Also included are ethoxylated derivatives such as trimethylol propane with 5 to 30 EO.
• the preferred polyethylene glycols can be linear or branched Have structure, with linear polyethylene glycols being preferred in particular.
• the particularly preferred polyethylene glycols include those with relative molecular weights up to 12,000, advantageously around 4,000, polyethylene glycols with relative Molecular masses below 3500 and above 5000 especially in combination with Polyethylene glycols with a molecular weight around 4000 can be used and such combinations advantageously to more than 50 wt .-%, based on the total amount of polyethylene glycols, polyethylene glycols with a relative molecular weight have between 3500 and 5000.
• polyethylene glycols can also be used as binders are used, which at room temperature and a pressure of 1 cash in liquid form; here is mostly of polyethylene glycol with a relative Molecular mass of 200, 400 and 600.
• binders are used, which at room temperature and a pressure of 1 cash in liquid form; here is mostly of polyethylene glycol with a relative Molecular mass of 200, 400 and 600.
• at room temperature and 1 bar as the solids present polyethylene glycols preferred, since one Use of liquid feedstocks at room temperature or moderately elevated temperatures
• Low molecular weight polyvinylpyrrolidones and derivatives are also suitable as binders of these with relative molecular masses up to a maximum of 30,000. Relative are preferred here Molecular mass ranges between 3000 and 30,000, for example around 10,000. Polyvinylpyrrolidones are preferably not used as the sole binder, but in combination with others, especially in combination with polyethylene glycols.
• nonionic surfactants which are either liquid or solid at room temperature or at temperatures up to 40 ° C. at a pressure of 1 bar.
• the preferred nonionic surfactants include alkoxylated fatty or oxo alcohols, in particular C 12 -C 18 alcohols. Degrees of alkoxylation, in particular degrees of ethoxylation, of on average 2 to 80 AO, in particular EO per mole of alcohol and mixtures thereof have proven to be particularly advantageous.
• customary fatty alcohols or methyl-branched alcohols with essentially 12 to 18 carbon atoms and 2 to 14 EO are preferably used in the mixture to be compacted.
• liquid nonionic surfactants at room temperature or at temperatures up to 40 ° C and at a pressure of 1 bar only if other solids are present which have a corresponding suction power.
• absorbent substances include, for example, (tripoly) phosphates, zeolites, silicas or sulfates, but not the bicarbonates, citric acid or solid polyethylene glycols with relative molecular weights of 4000 or above used in the process.
• alkyl glycosides of the general formula RO (G) x should also be used, in which R denotes a primary straight-chain or methyl-branched, in particular methyl-branched aliphatic radical having 8 to 22, preferably 12 to 18, carbon atoms and G is the symbol which stands for a glycose unit with 5 or 6 carbon atoms, preferably for glucose.
• the degree of oligomerization x which indicates the distribution of monoglycosides and oligoglycosides, is any number between 1 and 10; x is preferably 1.2 to 1.4, which can be used alone or in combination with other binders.
• binders in particular in combination with polyethylene glycols and / or alkyl glycosides, are polyhydroxy fatty acid amides of the formula (I) in which R 1 CO is an aliphatic acyl radical having 6 to 22 carbon atoms, R 2 is hydrogen, an alkyl or hydroxyalkyl radical having 1 up to 4 carbon atoms and [Z] represents a linear or branched polyhydroxyalkyl radical having 3 to 10 carbon atoms and 3 to 10 hydroxyl groups.
• R 1 CO is an aliphatic acyl radical having 6 to 22 carbon atoms
• R 2 is hydrogen, an alkyl or hydroxyalkyl radical having 1 up to 4 carbon atoms
• [Z] represents a linear or branched polyhydroxyalkyl radical having 3 to 10 carbon atoms and 3 to 10 hydroxyl groups.
• the polyhydroxy fatty acid amides are preferably derived from reducing sugars with 5 or 6 carbon atoms, especially from glucose.
• the group of polyhydroxy fatty acid amides also includes compounds of the formula (II) in which R 3 represents a linear or branched alkyl or alkenyl radical having 7 to 12 carbon atoms, R 4 represents a linear, branched or cyclic alkyl radical or an aryl radical having 2 to 8 carbon atoms and R 5 represents a linear, branched or cyclic alkyl radical or Aryl radical or an oxy-alkyl radical having 1 to 8 carbon atoms, C 1 -C 4 -alkyl or phenyl radicals being preferred, and [Z] for a linear polyhydroxyalkyl radical whose alkyl chain is substituted by at least two hydroxyl groups, or alkoxylated, preferably ethoxylated or propoxylated derivatives of this radical.
• R 3 represents a linear or branched alkyl or alkenyl radical having 7 to 12 carbon atoms
• R 4 represents a linear, branched or cyclic alkyl radical or an
• [Z] is also preferably obtained here by reductive amination of a sugar such as glucose, fructose, maltose, lactose, galactose, mannose or xylose.
• a sugar such as 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 patent 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 content is at room temperature or at temperatures up to 40 ° C and at a pressure of 1 bar solid binder or solid binders in the mixture to be compacted, as already mentioned 2 to 20 wt .-% and in particular 5 to 15 wt .-%.
• Preferred binders are Polyalkylene glycols, especially polyethylene glycols with a relative molecular weight above 2000, especially with a molecular weight of 4000 or 6000.
• inorganic components can be used in the mixture to be compacted Builders, which are usually in detergents or cleaning agents are included. These include, for example, aluminosilicates such as the zeolites of the type A, X, Y and / or P. However, water-soluble inorganic builders are preferably used. These include in particular the conventional phosphates such as orthophosphate, Pyrophosphate and especially tripolyphosphate, but also alkali metal carbonates and amorphous and / or crystalline layered silicates. In individual embodiments it may be preferred to use tripolyphosphates in the mixture to be compacted. The content of the mixture to be compacted or of the cobuilder-containing mixture produced Additives to these additional inorganic builders can be up to 35% by weight.
• Additives can be common ingredients of washing or cleaning agents, preferably bleach activators and / or bleach catalysts, as well as dyes and or fragrances.
• 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.
• Substances containing O and / or N-acyl groups of the number of carbon atoms mentioned are suitable and / or optionally substituted benzoyl groups.
• acylated alkylenediamines especially tetraacetylethylenediamine (TAED), acylated triazine derivatives, in particular 1,5-diacetyl-2,4-dioxohexahydro-1,3,5-triazine (DADHT), acylated Glycolurils, especially tetraacetylglycoluril (TAGU), N-acylimides, especially N-nonanoylsuccinimide (NOSI), acylated phenol sulfonates, especially n-nonanoyl or Isononanoyloxybenzenesulfonat (n- or iso-NOBS), carboxylic anhydrides, in particular Phthalic anhydride, acylated polyhydric alcohols, especially triacetin, ethylene glycol diacetate, 2,5-diacetoxy-2,5-dihydrofuran and those from the German patent applications DE-A-196 16
• German patent application DE-A-196 16 769 known hydrophilically substituted acylacetals and those in the German patent application DE-A-196 16 770 and the international patent application Acyl lactams described in WO-A-95/14075 are also preferably used. Also the conventional combinations known from German patent application DE-A-44 43 177 Bleach activators can be used.
• the bleach activator can be coated with coating substances in a known manner or, if necessary using auxiliaries, in particular methyl celluloses and / or carboxymethyl celluloses, granulated or extruded / pelleted and if desired contain further additives, for example dye. Preferably contains a such granules over 70 wt .-%, in particular from 90 to 99 wt .-% bleach activator.
• a bleach activator is preferably used, the peracetic acid under washing conditions forms.
• the transition metal compounds in question include in particular known from the German patent application DE-A-195 29 905 manganese, iron, Cobalt, ruthenium or molybdenum salt complexes and those from the German patent application DE-A-196 20 267 known N-analog compounds, which from the German Patent application DE-A-195 36 082 known manganese, iron, cobalt, ruthenium or Molybdenum-carbonyl complexes, which are described in German patent application DE-A-196 05 688 manganese, iron, cobalt, ruthenium, molybdenum, titanium, vanadium and Copper complexes with nitrogenous tripod ligands resulting from the German patent application DE-A-196 20 411 known cobalt, iron, copper and ruthenium amine complexes, the manganese described in German patent application DE-A-44 16 438, Copper and cobalt complexes described in European patent application EP-A-0 272 030 described cobalt complexes resulting from the
• Bleach activators and / or bleach catalysts are preferably used in amounts of 5 to 35% by weight, in particular up to a maximum of 30% by weight, because of the bleach activators and catalysts, the dissolving behavior of the additives is adversely affected.
• additives containing cobuilders in which only minor or contain no amounts of bleach activators and / or bleach catalysts are.
• These additives produced according to the invention preferably consist of at least 70% by weight of bicarbonate and organic polycarboxylic acid.
• a mixture is roller compacted, which are 80 to 100 wt .-% of bicarbonate, organic polycarboxylic acid and a or more binders or of bicarbonate, organic polycarboxylic acid and tripolyphosphate consists.
• An advantageous embodiment of the invention provides that the invention manufactured additives or the solid dyes to be compacted in Have amounts below 1 wt .-%. Fragrances, on the other hand, are only found in the compacting mixtures used if absorbent components are included.
• the fragrance content of the additives produced according to the invention can be 2 to a maximum about 10% by weight, but in particular 3 to 5% by weight.
• the bulk density of the cobuilder-containing additives produced according to the invention is usually between 600 and 1000 g / l.
• washing or Detergent or a component claimed for this which or which 3 to 10% by weight of the additives according to the invention described above contains or contain.
• Such agents are particularly suitable as hand washing agents for textiles foaming all-purpose cleaners or bathroom cleaners as well as machine detergents for delicates, Wool and the like.
• These additives are used in the manufacture of washing or Detergents preferably added later.
• the invention provides that the washing or cleaning agent or the component for this is produced by tableting, the according to the invention manufactured Cobuilder-containing additives used in the premix to be tabletted become.
• the detergents or cleaning agents produced according to the invention can contain customary ingredients such as anionic, nonionic, cationic, zwitterionic and / or amphoteric surfactants in conventional amounts, preferably between 5 and 40% by weight, inorganic water-soluble Builder substances, for example phosphates, crystalline layered silicates, amorphous Silicates and / or alkali carbonate, but also inorganic water-insoluble builder substances, for example zeolite A, X, Y and / or P, further organic builder substances, in particular (co) polymeric salts of acrylic acid and / or maleic acid, bleaching agents, preferably perborate and / or percarbonate, bleach activators and / or bleach catalysts as described above, graying inhibitors, phosphonates, dye transfer inhibitors and / or ingredients that prevent the dirt from re-opening, Enzymes, in particular proteases, amylases, lipases, cellulases and / or (per) oxidases, Cont
• Additives A, B and C of the compositions given below were prepared.
• the solids were mixed with one another in a mixer, for example from Lödige, and any liquids which were present were added in the customary manner.
• the binder polyethylene glycol with a molecular weight of 4000 was added in solid form.
• the mixture to be compacted was then subjected to roller compaction (roller mill from Alexanderwerke) with subsequent breaking and sieving of the strands that had been extruded.
• the screened fines with particle sizes below 0.4 mm were screened and subjected to a further roller compaction.
• the coarse fractions with particle sizes above 1.6 mm (the upper grain limit can be set by a suitable sieve insert on the crusher) in the additives A, B and C produced according to the invention were each below 5% by weight! Composition in% by weight:
• a B C Sodium bicarbonate 39.0 39.0 32.0 Citric acid (anhydrous) 46.0 ----- 38.0 Citric acid (anhydrous, coated with glucose) syrup) ----- 46.0 ----- Polyethylene glycol (molecular weight 4000) 15.0 15.0 ----- Sodium tripolyphosphate ----- ----- 30.0 Bulk density in g / l 830 790 740
• recipes A, B and C were also those in the unpublished version German patent application P 197 04 229.5 subjected to the method described. While the recipes A and B coarse-grained fractions (particle sizes> 1.6 mm) above of 30% by weight was formulation C due to the lack of a melt binder not produceable.

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Citations (6)

• 1997
  • 1997-11-20 DE DE1997151398 patent/DE19751398A1/de not_active Withdrawn
• 1998
  • 1998-11-11 EP EP98121451A patent/EP0918087A1/fr not_active Withdrawn

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