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
  • C11D3/16—Organic compounds
  • C11D3/37—Polymers
  • C11D3/3746—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
  • C11D3/3757—(Co)polymerised carboxylic acids, -anhydrides, -esters in solid and liquid compositions
  • C11D3/3761—(Co)polymerised carboxylic acids, -anhydrides, -esters in solid and liquid compositions in solid 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
  • 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
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/16—Organic compounds
  • C11D3/20—Organic compounds containing oxygen
  • C11D3/22—Carbohydrates or derivatives thereof
  • C11D3/222—Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin

Definitions

• the invention relates to auxiliaries granules, composed of cellulose and optionally cellulose / starch derivatives, polymeric binders and gel-forming surfactants, which are used as disintegrating agents for tablets in u.a. Detergent and cleaning product is suitable. Furthermore, a method for producing the granules and their use is described.
• Disintegrating agents for tablets or granules are auxiliaries which positively influence the disintegration of tablets or of the granules on contact with liquids, in particular water. In this case, both the disintegration of tablets into coarse parts as well as subsequently a disintegration into smaller particles up to the dissolution / dispersion of all detergent components should be effected and accelerated.
• Tablets are made by pressing a starting granulate with certain pressures, the bulk density being e.g. for compact detergents is about 900g / l, after tableting to 1200 g / l increases.
• Such tablets with higher densities than the starting granules are naturally less soluble / divisible than the starting granules.
• the addition of decay-promoting explosives is appropriate.
• Addition to the dispenser is most convenient to the user and safest for the quality of the wash.
• very high Requirements placed on the rate of disintegration of the tablet In particular, the first step of the disintegration of the tablet in coarse parts must go very quickly, otherwise residues of the tablet remain in the dispenser and are not used for washing.
• a time of approximately 30 seconds is available for flushing in the tablets via the dispensing chamber.
• the tablets have to fulfill their function both in hot and cold rinsing water. In the washing drum are different conditions for the disintegration of the tablet, since both mechanical friction and increasing water temperatures affect the dissolution process of the tablet.
• tablet disintegrants in pharmaceutical practice. According to their mechanism of action, several models are discussed for tablet disintegrants, such as the development of gas bubbles (effervescent powder), the mutual particle repulsion, the water transport (wicking) and the swelling / expansion by water absorption.
• DE-OS 2,251,249 e.g. rapidly disintegrating drug tablets prepared by compressing drug granules and disintegrant granules.
• the use of granular starting materials results in a porous tablet structure.
• disintegrant granules based on starch with a particle size of 2.0 to 0.3 mm are used.
• Drug tablets are known from DE-OS 2 355 204, which are pressed from granular components, the granules are set for reasons of tablet stability prior to compression to a moisture content of less than 2%.
• US 3,629,393 claims sustained-release drug tablets which are pressed from granular ingredients using disintegrants of high molecular weight, water-swellable compounds such as cellulose derivatives in the form of granules.
• the granule dimensions move in the examples by 0.84 mm.
• US 4,072,535 describes the use of pre-compacted starch disintegrators for pharmaceuticals and detergents.
• the grain size of Kompaktates is 0.05 mm to 0.42 mm, the moisture content is 9-16%, preferably 11-13%.
• the disintegration times of the example tablets are several minutes.
• Detergent tablets are known from DE-OS 2 321 693, containing 1 to 25 wt.% Fibrous cellulose as disintegrant. In the examples, tablets having a strength of 15 to 19 N are prepared using compacted cellulose granules.
• EP 0170791 tablet-shaped washing additives which are pressed from granular components, wherein also 1 to 5 wt.% Granular tablet disintegrants based on crosslinked Polyvinylpyrrolidone and / or cellulose ethers are used.
• the granules should be free of dust particles.
• the tablets have breaking strengths of 50 to 120 N and have long dissolution times of several minutes.
• washing or cleaning active moldings are known, which are prepared using a disintegrant granules having a high water adsorption capacity and a particle size distribution, wherein at least 90 wt.% A particle size of at least 0.2 mm and a maximum of 3 mm to have.
• the dust content ⁇ 0.1 mm is less than 1%.
• the disintegrant granules contain at least 20% by weight of disintegrants, such as starch, starch derivatives, cellulose, cellulose derivatives. According to the teaching of this patent, the presence of anionic or nonionic surfactants adversely affects tablet disintegration time.
• the granules are prepared by conventional means, such as spray drying, hot steam drying of aqueous preparations, or by granulation, pelleting, extrusion or roll compaction of powdered ingredients. Detailed process information on the granulation process or on further process steps after the granulation of the disintegrant granules are not made.
• the detergent tablet prepared by way of example contains a disintegrant based on compacted cellulose from thermochanically treated wood pulp and has a tablet hardness of 45 N. Higher strength tablets, i. over 50 N are not described.
• WO 98/55575 describes an auxiliary granulate for washing and cleaning agent-active moldings.
• the claimed auxiliary granules contain 10 to 95% by weight of cellulose having particle sizes below 0.1 mm and 5 to 90% by weight of microcrystalline cellulose.
• the celluloses are partially combined with carboxymethyl cellulose, TAED and citric acid / bicarbonate.
• the particle sizes of Kompaktates be more than 90% by weight of 0.3 to 2.0 mm, less than 5% by weight less than 0.2 mm and have no dust content.
• roll compaction of the dry premix is preferred.
• Detailed process information for granule production are not made.
• the detergent tablets exemplified using the excipient granules have low strengths of 35 N or less. More stable, more compact tablets with higher strength from 50 N are not described.
• cellulose / cellulose derivatives or starch / starch derivatives are combined with thickening surfactants and finely divided polymers of (meth) acrylic acid in compacted granulated form as disintegrant granules for detergents and cleaners , Water softeners and stain salts in tablet form claimed.
• the granules have a non-linear source kinetics, wherein in relation to the entire swelling process in the initial phase of the swelling process, a very large increase in volume occurs. About the dissolution behavior of the tablets in the dispenser of a washing machine no information is given.
• the patent application WO 98/40462 describes a compact of powdered and / or granular ingredients, in particular detergent ingredients, which contains particles of cellulose-containing material which act as disintegrating agents and which can also be present in compacted form.
• cellulose component are thermomechanical (TMP) and chemical thermomechanical (CTMP) treated wood pulps.
• TMP thermomechanical
• CMP chemical thermomechanical
• the particle size of the compacted disintegrant may be 0.2 to 6 mm.
• Surfactant raw materials can also be fed to the compact via the cellulose component, with 0.5-5% surfactant / compact being mentioned.
• the prior art also includes sales products of the company Degussa AG with the name Elcema G250 and Elcema G 400, which consist of compacted pure cellulose and have been used since 1971 as a tablet disintegrant. These products are made by dry granulation and have a particle size of 0.03 to 0.40 mm. The moisture content is ⁇ 6%.
• the object of the invention is therefore to provide a comparison with the prior art improved disintegrant granules for tablets.
• it should swell so rapidly and strongly that tablets made using it are largely dissolved in the dispensing chamber of washing machines during the brief water scavenging time.
• the disintegrant granules should have a high Have abrasion resistance and are not limited in its effect by inevitably incurred in the course of its manufacturing process fine and dust in particular parts.
• the disintegrants in tablets with high strengths above 50 N should ensure a combination of good explosive action and good solubility and experience only minor signs of aging in the form of a weakening of the properties by storage of the tablets over several weeks.
• the object also includes the provision of a method for producing the disintegrant granules and their use in tablets for washing and cleaning processes.
• Component A is a compound having Component A:
• water-insoluble, swellable cellulose is used.
• Particularly suitable fibrils native cellulose with a maximum length of 0.30 mm proved.
• Both microcrystalline and amorphous particulate cellulose and mixtures thereof can be used.
• the finely divided cellulose preferably has apparent densities of from 40 g / l to 300 g / l, very particularly preferably from 65 g / l to 170 g / l. If already granulated types are used, their bulk density is higher and, in an advantageous embodiment, can be from 350 g / l to 550 g / l.
• the bulk densities of the cellulose derivatives are typically in the range of 50 g / l to 1000 g / l, preferably in the range of 100 g / l and 800 g / l.
• the particle size of the finely divided cellulose is preferably between 0.030 mm and 0.20 mm, in the case of granulated types, the preferred average particle size is between 0.350 mm and 0.800 mm.
• the particle size of the finely divided cellulose derivatives is preferably 0.030 mm to 3.0 mm.
• the proportion of cellulose in disintegrant granules is between 60 to 99% by weight, preferably between 60 to 95% by weight.
• regenerated celluloses such as viscose are also used.
• regenerated celluloses in powder form are characterized by a very good water absorption.
• the viscose powder can be produced from cut viscose fiber or by precipitation of the dissolved viscose.
• Low molecular weight cellulose degraded by electron beam is also suitable, for example, for producing the disintegrant granulate.
• plasticized regenerated fibers are used.
• a typical plasticizer for such products may be mentioned here, for example, glycerol.
• the granules according to the invention may comprise water-swellable cellulose derivatives such as cellulose ethers and cellulose esters and starch or starch derivatives and other swellable polysaccharides and polygalactomannans, for example ionically modified celluloses and starches such as carboxymethyl-modified cellulose and starch, nonionically modified celluloses and starches such as alkoxylated celluloses and starches such as hydroxypropyl and hydroxyethyl starch or hydroxypropyl and hydroxyethyl cellulose and alkyletherified products such as methylcellulose, as well as mixed modified celluloses and starches from the aforementioned modifications, optionally combined with a modification to Networking leads.
• water-swellable cellulose derivatives such as cellulose ethers and cellulose esters and starch or starch derivatives and other swellable polysaccharides and polygalactomannans
• ionically modified celluloses and starches such as carboxymethyl-mod
• Suitable starches are also cold-swelling starches which are formed by mechanical or degrading reactions on the starch grain. These include, above all, swelling powders from extruder and drum dryer processes as well as enzymatically, oxidatively or acid-degrading modified products. Chemically derivatized starches preferably contain substituents attached to the polysaccharide chains in sufficient numbers by ester and ether groups
• Starches modified with ionic substituents such as carboxylate, hydroxyalkyl or phosphate groups have been found to be particularly advantageous and are therefore preferred. To improve the swelling behavior, the use of easily cross-linked starches has proven itself. Also alkaline treated starches can be used because of their good cold water swellability.
• the combination of cellulose with cellulose derivatives and / or starch and / or starch derivatives has been proven.
• the proportions can vary within wide limits, based on the combination, the proportion of cellulose derivatives and / or starch and / or starch derivatives preferably 0.1 to 85 wt.%, Particularly preferably 5 to 50 wt.%.
• Component B is a compound having Component B:
• Binders used are polymers or copolymers of (meth) acrylic acid or mixtures of such polymers or copolymers in the granules.
• the polymers are selected from the group of homopolymers of (meth) acrylic acid, from the group of copolymers with the following monomer components of ethylenically unsaturated dicarboxylic acids and / or their anhydrides and / or ethylenically unsaturated sulfonic acids and / or acrylic esters and / or vinyl esters and / or vinyl ethers or their saponification products and / or crosslinkers and / or graft bases based on polyhydroxy compounds.
• Non-crosslinked polymers or copolymers of (meth) acrylic acid having weight-average molecular weights of 5,000 to 70,000 have proved to be particularly suitable.
• the copolymers are preferably copolymers of (meth) acrylic acid and ethylenically unsaturated dicarboxylic acids or their anhydrides, such as maleic acid or maleic anhydride, which contain, for example, 40 to 90% by weight of (meth) acrylic acid and 60 to 10% by weight of maleic acid or Maleic anhydride whose relative molecular weight, based on free Acids, between 3,000 and 100,000, preferably 3,000 to 70,000 and most preferably 5,000 to 50,000.
• ter- and quattropolymere polycarboxylates composed of (meth) acrylic acid, maleic acid and optionally fully or partially saponified vinyl alcohol derivatives, or those of (meth) acrylic acid, ethylenically unsaturated sulfonic acids and polyhydroxy units, such as sugar derivatives, or such from (meth) acrylic acid, maleic acid, vinyl alcohol derivatives and monomers containing sulfonic acid groups.
• suitable polymers can be found in the patents DE 43 00 772, DE 42 21 371 and WO 95/17444.
• the polymeric binders are preferably used in the preparation in the form of their aqueous solutions, but can also be used in the form of finely divided powders.
• the binder polymers are preferably in part or fully neutralized form, the salt formation is preferably carried out with cations of alkali metals, ammonia and amines, or mixtures thereof.
• the proportion of polymers / copolymers in the disintegrant is between 1 and 40% by weight, preferably between 1 and 20% by weight, more preferably between 5 and 15% by weight. Polymer contents above 15% in the disintegrant result in harder disintegrant granules, while polymer contents below 1% tend to form soft granules that are less resistant to abrasion.
• Suitable polymer binders are also crosslinked polymers of (meth) acrylic acid. They are preferably used as finely divided powders and preferably have average particle sizes of 0.045 mm to 0.150 mm and are preferably used with 0.1 to 10 wt.%. Although particles having an average particle size of more than 0.150 mm also give good disintegrant granules, but after dissolution of the pellets produced with the granules visually visible as particles swelling bodies, which are clearly visible, for example, in the case of textile washes deposited on the textile material in a disturbing manner.
• a particular embodiment of the invention is the combination of soluble poly (meth) acrylate homo- and copolymers and the aforementioned finely divided crosslinked polymer particles.
• the disintegrant granules contain one or more liquid, water-gelling surfactants selected from the group of nonionic, anionic or amphoteric surfactants which are present in amounts of up to 7% by weight, preferably up to 3.5% by weight. If the surfactant content in the disintegrant is too high, in addition to an increased abrasion of the tablets produced therewith, also worse swelling properties result.
• the nonionic surfactants may include, for example, alkyl polyglucosides, fatty acid alkylolamides, fatty acid polyethylene glycol esters, fatty amine oxethylates, Fatty alcohol ethoxylates with 3-15 moles of ethylene oxide or propylene oxide, fatty acid glycerides, sorbitan esters, sucrose esters, for example sucrose palmitate, pentaerythritol partial esters, which may also be ethoxylated, and alkylphenol-polyethylene glycol ethers or phenol-poly-ethylene glycol ethers.
• the anionic surfactants may be, for example, alkyl sulfates, linear and branched alkyl benzene sulfonates, alkyl glycerol ethers, fatty alcohol polyethylene glycol ether sulfates, paraffin sulfonates, alpha-olefin sulfonates, sulfosuccinates, phosphoric acid esters or fatty alcohol ether carboxylates.
• amphoteric surfactants may, for example, be cocofatty acid amidopropyl betaine, modified imidazolines or fatty acid amide derivatives having betaine structure.
• mixtures of surfactants are used; in a further preferred embodiment, only nonionic surfactants are used.
• the compacted granules according to the invention are characterized by a special swelling kinetics, the extent does not change linearly as a function of time but reaches a very high level after a very short time.
• the swelling behavior in the first 10 seconds after contact with water In the range of the water content of 2 to 8 wt.%
• This combination of properties has a positive influence on the tablets produced with the disintegrating agents and leads there to short tablet disintegration times and a very good dispensing behavior in the dosing chambers of the washing machines.
• the superior effect of the agents according to the invention is shown by the fact that almost all tablets disintegrate and are washed away.
• the specific water absorption capacity of the granules according to the invention is very high and can be determined gravimetrically.
• the water absorption determined in this way is preferably 500 to 2000%
• the liquid uptake (also referred to as specific porosity) of the disintegrants according to the invention is markedly increased in comparison with products of the prior art and is in a range of more than 750 ml / kg, preferably in the range of 800 to 1000 ml / kg.
• This high fluid intake has a significant influence on the swelling effect and water transport in the disintegrant.
• Products of the prior art have an average liquid intake of about 600 ml / kg.
• the preparation of the disintegrant granules according to the invention is carried out first by mixing the granule components according to the invention with conventional mixing methods.
• mixers from Vomm, Lödige, Schugi, Eirich, Henschel or Fukae can be used.
• precompounds are produced by agglomeration processes. These precompounds form a free-flowing product which has a water content of between 10 and 80% by weight.
• the required water content in the premix depends on the compressor used.
• a water content of at least 10%, preferably 20% is required to achieve a good compaction and to guarantee a high liquid absorption in the subsequent dry granules.
• these precompounds are mechanically compacted.
• the compression using pressure can be done in various ways.
• the products can between two pressure surfaces in roller compactors, z. B. smooth or profiled, be compacted.
• the output of the Kompaktates takes place as a strand.
• Compacting methods in dies with punches or cushion rolls result in compact forms such as tablets or briquettes.
• Roller compactors, extruders, roller or die presses, but also granulation presses can be used as compacting machines.
• Suitable pelleting presses are manufactured, for example, by the companies Amandus Kahl and Fitzpatrick.
• the compaction preferably produces a disintegrant granulate having a bulk density of from 100 g / l to 500 g / l, particularly preferably from 150 g / l to 450 g / l and very particularly preferably from 250 g / l to 400 g / l.
• the compliance with a preferred limit of the bulk density of a maximum of 400 g / l has proved to be favorable because of the particularly good swelling properties. Surprisingly, it was found that the granules also have a very good abrasion stability at these bulk densities.
• the coarse, compacted particles are comminuted, e.g. Mills, shredders or roller mills are suitable.
• the comminution can be carried out before or after drying.
• the granules according to the invention are preferably adjusted to a particle size distribution of 0.05 to 3 mm, more preferably 0.1 to 1.5 mm.
• Removal of dust levels below 0.1 mm may be achieved e.g. be carried out with conventional screening devices. Since dust fractions of up to 10 wt. In the application of the granules of the invention does not interfere predominantly, their separation can often be omitted.
• the water content according to the invention of 2 to 8% by weight, preferably 2.5 to 7% by weight and more preferably 3 to 5% by weight is set.
• conventional dryers such as drum dryers (temperatures of, for example, 95-120 ° C.) or fluidized-bed dryers (temperatures of, for example, 70-100 ° C.) are suitable.
• the invention includes the use of the compacted granules as disintegrating agents for molded articles, for example tablets, cubes, spheres and the like. Particularly preferred is the use as a disintegrant for detergent formulations, detergent formulations, stain salts, water softeners in tablet or cube form.
• the disintegrant granules according to the invention are present in the shaped bodies in amounts of 0.5% by weight to 15% by weight, preferably 3% by weight to 8% by weight and more preferably 4% by weight to 7% by weight.
• the moldings of the invention have sufficient stability and strength, and allow safe handling, packaging and storage. On contact with water, however, they should disintegrate rapidly, so that the components can develop the desired effect. A sufficient stability against mechanical effects is given for moldings from a breaking strength of 50 N.
• the granules according to the invention impart to these high-density moldings a decomposition and dissolution characteristic which is otherwise only given in the case of moldings of low strength.
• the tablets for laundry detergent formulations generally contain builders, bleaches and bleach activators, surfactants, tableting aids, disintegrants and other customary additives and auxiliaries.
• Suitable builders are polyphosphates, pyrophosphates, metaphosphates or phosphonates, sheet silicates, amorphous silicates, amorphous disilicates and zeolite.
• Other constituents of the builder system may include fillers such as alkali carbonates, bicarbonates z. For example, sodium carbonate or sodium bicarbonate, sesquiocarbonates, sodium sulfate, magnesium sulfate, or citrate, citric acid, succinic acid, tartaric acid and malic acid. Frequently used as Hilfsgerüststoff co-builders and dispersants.
• Such co-builders or dispersants may be polyacrylic acids and their sodium salts.
• Copolymers of (meth) acrylic acid and maleic acid, terpolymers and quattropolymers of (meth) acrylic acid, maleic acid, vinyl alcohol and sulfo-containing vinyl compounds can also be used.
• Particular preference is also ter- and quattropolymere polycarboxylates prepared from (meth) acrylic acid, maleic acid and vinyl alcohol or vinyl alcohol derivatives (as described in DE 43 00 772 C2) or those of (meth) acrylic acid, 2-alkylallylsulfonic and sugar derivatives (as described in DE 42 21 381 C1) or those of (meth) acrylic acid, maleic acid, vinyl alcohol derivatives and monomers with sulfonic acid groups (described in DE 195 16 957 A).
• constituents used are polyethylene glycol and / or polypropylene glycol having a molecular weight of from 900 to 30,000, and carboxylated polysaccharides, polyaspartates and polyglutamate. Also mixtures with various organic builders such as e.g. Citric acid is possible.
• Typical bleaching agents to be used are sodium perborate tetrahydrate and sodium perborate monohydrate, sodium percarbonate, peroxypyrophosphates, citrate perhydrates, as well as H 2 O 2 -producing peracidic salts, peracids, such as perbenzoates, peroxyphthalates, diperazelaic acid and diperdodecanedioic acids.
• the content of bleaching agents in tablets is preferably 10-60% by weight and in particular 15-50% by weight. In order to achieve a good bleaching effect when washing below 60 ° C and below, activators can be incorporated.
• Suitable bleach activators are the H 2 O 2 organic peracids forming N-acyl and O-acyl compounds, preferably N, N'-tetraacylated diamines, carboxylic anhydrides and esters of polyols such as glucose pentaacetate. Further, acetylated mixtures of sorbitol and mannitol may be used. Particularly suitable as bleach activators are N, N, N ', N'-tetraacetylethylenediamine (TAED), 1,5-diacetyl-2,4-dioxo-hexahydro-1,2,5-triazine (DADHT) and acetylated sorbitol-mannitol. Mixtures (SORMAN).
• cationic surfactants may also be present in detergent formulations, for example quaternary ammonium compounds having C 8 -C 16 N-alkyl or N-alkenyl groups and N-substituents such as methyl, hydroxyethyl or hydroxypropyl groups.
• Tableting aids are also used if appropriate, for example polyalkylene glycols and magnesium stearates.
• Examples of further customary detergent additives and auxiliaries are enzymes, magnesium silicates, aluminum aluminates, benzotriazole, glycerol, magnesium stearate, polyalkylene glycols, hexametaphosphate, phosphonates, bentonites, soil release polymers, carboxymethylcelluloses.
• Dishwashing tablets as an embodiment of detergent formulations generally contain as builders polyphosphates, pyrophosphates, metaphosphates or phosphonates, sheet silicates, amorphous silicates, amorphous disilicates and zeolites, and fillers such as sodium carbonate, sodium sulfate, magnesium sulfate, sodium bicarbonate, citrate and citric acid, succinic acid, tartaric acid and malic acid , Frequently co-builders and dispersants are used as auxiliary builder.
• co-builders or dispersants may be polyacrylic acids or copolymers with polyacrylic acid and its sodium salts.
• Typical bleaching agents are sodium perborate tetrahydrate and sodium perborate monohydrate, sodium percarbonate, peroxypyrophosphates, citrate perhydrates, as well as H 2 O 2 -forming peracidic salts, peracids, such as perbenzoates, peroxyphthalates, diperazelaic acid and diperdodecanedioic acids.
• the content in the tablets is preferably 10-60% by weight, and more preferably 15-50% by weight.
• Low-foaming nonionic surfactants of the type polyalkylene glycol and alkyl polyglucosides are also used.
• Examples of other customary detergent additives and auxiliaries are also here enzymes, magnesium silicates, aluminum aluminates, benzotriazole, glycerol, magnesium stearate, polyalkylene glycols, hexametaphosphate and phosphonates.
• Water softening tablets generally consist of builders such as phyllosilicates, amorphous silicates, amorphous disilicates and zeolites, as well as fillers such as sodium carbonate, sodium sulfate, magnesium sulfate, sodium bicarbonate, citrate and citric acid.
• builders such as phyllosilicates, amorphous silicates, amorphous disilicates and zeolites
• fillers such as sodium carbonate, sodium sulfate, magnesium sulfate, sodium bicarbonate, citrate and citric acid.
• co-builders and dispersants are used as auxiliary builder.
• Such co-builders or dispersants may be polyacrylic acids or copolymers with polyacrylic acid and its sodium salts.
• Low-foaming nonionic surfactants of the type polyalkylene glycol and alkyl polyglucosides are also used.
• Examples of further customary detergent additives and auxiliaries are magnesium silicates, polyalkylene glycols and phosphonates.
• disintegrant granules according to the invention it is possible with the disintegrant granules according to the invention to produce detergent tablets having disintegration times of up to 15 seconds with a tablet breaking strength of up to 80 N.
• the specific water absorption capacity of the granules according to the invention can be determined gravimetrically as follows: A defined amount of granules (eg 2.00 g) is sealed in a thin paper bag, such as a tea bag, and dipped in a vessel with an excess of water. After 3 minutes of immersion, the bag is removed from the water and hung for 10 minutes to drip. The bag is weighed and determined from the difference in weight of a wet bag with and without granules, the water absorption. Distilled water is used for the determination.
• the specific porosity of the disintegrant granules is determined by means of a known standard method for determining the degree of porosity of solids. Principle of the method:
• the solid is completely impregnated with di-n-butyl phthalate (DBP) and then the liquid absorbed in the pores is removed after a defined time under defined conditions by centrifuging.
• the amount of absorbed DBP is considered to be the measure of the porosity of the solid.
• Execution: 3 g of the sample are weighed into a commercially available tared glass filter crucible G3 and mixed with 10 ml of DBP. These crucibles are placed in a beaker, the bottom of which is laid out with filter paper. After exactly 5 minutes, the glass filter crucibles are weighed, then placed in Teflon inserts and centrifuged for 5 minutes at 1800 rev / min.
• a washing and cleaning tablet containing 5% disintegrant is used for the test.
• 500 ml of soft water at a temperature of 23 ° C are added.
• a metal sieve with a mesh size of 4 mm is applied.
• a magnetic stir bar is set in motion at about 200 rpm and a tablet is placed on top of the sieve from above.
• the time from the beginning of the tablet addition to the disintegration of the tablet is measured with a stopwatch. Disintegration is achieved when all tablet parts have fallen through the sieve.
• the washing machine are set 3 tablets in succession.
• the washing machine is connected to a pressure line with 5 bar city water and started in the 60 ° C normal program.
• the flushing time is while 30 sec, the machine takes only once water.
• the experiment is carried out a total of four times, so that 12 tablets are used. After each flush, the remaining tablets are counted. The total amount of non-flushed tablets is given.
• the TB30 / TBH30MD tablet breakage resistance tester from Erweka is used for the determination of the tablet breakage strength.
• the breaking strength is determined by means of a strain gauge with a load cell. The measuring accuracy is +/- 1N. After appropriate programming, the tablet is inserted into the measuring device and started the measuring process. The device displays the value of the breaking strength.
• the disintegrants used in the examples were prepared by wet compaction on a pelleting press made by Amandus Kahl. The degree of compaction was set to 1: 3. The water content of the mixtures before compression is shown in Table 1. After compaction, the granules were dried on a drum dryer from Babcok to the specified moisture contents.
• the comparative example V5 was produced on a roll press WP 150 of the Alexanderwerke without additional water. The pressing pressure was set to 1.1 t / cm. The granules were crushed on a Reibschnitzler. The drying also took place on a belt dryer. The granules have particle sizes between 0.3 and 2 mm, the dust content below 0.1 mm is given in the table.
• Table 1 Formulations for preparing disintegrants in% by weight and properties of the granules explosives V1 V3 V4 V5 M1 M2 M3 M4 M5 M6 M7 cellulose * 50 50 50 80 50 50 45 50 47 40 50 Linear PAA ** 12.5 12.5 12.5 20 12.5 12.5 10 10 12.5 10 - Core PAA *** 2 - CMC ### 15 5 10 20 - Nio surfactant ## 0.5 0.5 0.5 0 0.5 0.5 0.5 0.5 0 0.5 - Polymeric surfactant # 12.5 Water to the compact.
• Example M2 of the invention When comparing Example M2 of the invention with Example V2, there were significant differences in the liquid absorption, which are due to compacting and the moisture content during compaction.
• M2 moisture content of the compacting and drying
• V2 dry-compacted pattern
• Table 3 shows the strength and results of the rinse test of the individual detergent tablets using the different disintegrants: Table 3: Explosive means according to example Humidity (%) Rinse test (do not rupture tabl.) Strength [N] Decay time [sec] V1 18 10 61 50 V2 5 10 58 52 V3 10 6 60 40 M1 6 1 62 12 M2 4 0 65 9 V4 1 3 58 25 M3 3 0 57 8th M4 3 1 63 10 M5 4 1 58 9 M6 5 0 59 7 M7 3 0 58 9
• Table 3 shows that both the composition and the same composition of the moisture content of the disintegrant granules have a significant influence on the tablet disintegration time.
• Disintegrants with the preferred level of 3-5 wt% water as in M2 also show the best disintegration times of the tablets. If, in addition, suitable swellable substances are incorporated as disintegrant component, the disintegration properties can be further increased.
• Table 4 shows the influence of storage time (4 weeks at 40 ° C / 60% relative humidity in a closed container) on the flushing behavior of tablets with disintegrants.
• Table 4 Phosphate-containing detergent tablet according to Table 2 example Moisture of the explosive [%] Rinse test (tablet) Swelling kinetics after 3 sec [mm] immediately n. 4 weeks V4 1 3 3 0.85 M1 6 1 1 0.90 M2 4 0 1 0.97 V3 10 6 7 0.80 V1 18 10 11 0.45 V2 6 10 11 0.47 M3 3 0 - 2.0 M4 3 1 - 1.7 M5 4 1 - 1.6 M6 5 0 - 2.2
• Table 4 shows that the moisture content of the disintegration granules according to the invention leads to superior properties of the tablets produced therewith in the important rinsing test or that the swellability with values of 0.9 and higher is superior to the comparison products.
• Tablets with inventive disintegrant show good storage stability.
• Tablets with In addition to cellulose, M3-M6 also contains cellulose derivatives and thus has a further improved swelling kinetics.
• the tablet disintegration time of highly compressed tablets with inventive disintegrant is superior to the comparison products.

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• Chemical & Material Sciences (AREA)
• Life Sciences & Earth Sciences (AREA)
• Engineering & Computer Science (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Oil, Petroleum & Natural Gas (AREA)
• Wood Science & Technology (AREA)
• Organic Chemistry (AREA)
• Health & Medical Sciences (AREA)
• Molecular Biology (AREA)
• Emergency Medicine (AREA)
• Detergent Compositions (AREA)
• Medicinal Preparation (AREA)
• Glanulating (AREA)
• Casting Or Compression Moulding Of Plastics Or The Like (AREA)
• Sewing Machines And Sewing (AREA)
• Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

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• 1999
  • 1999-03-29 DE DE59913705T patent/DE59913705D1/de not_active Expired - Lifetime
  • 1999-03-29 ES ES99106370T patent/ES2270547T3/es not_active Expired - Lifetime
  • 1999-03-29 AT AT99106370T patent/ATE334187T1/de active
  • 1999-03-29 EP EP99106370A patent/EP1043391B1/de not_active Expired - Lifetime
  • 1999-03-29 PT PT99106370T patent/PT1043391E/pt unknown
• 2000
  • 2000-03-27 US US09/534,455 patent/US6303560B1/en not_active Expired - Lifetime
  • 2000-03-28 PL PL339271A patent/PL196418B1/pl unknown
  • 2000-03-28 CZ CZ20001116A patent/CZ293387B6/cs not_active IP Right Cessation
  • 2000-03-29 TR TR2000/00832A patent/TR200000832A2/xx unknown
  • 2000-03-29 HU HU0001329A patent/HU228596B1/hu not_active IP Right Cessation

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