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 an auxiliary granulate, composed of cellulose and optionally cellulose / starch derivatives, polymeric binders and gel-forming surfactants, which are used as disintegrants for tablets in Washing and Detergent tablets is suitable. Furthermore, a method for Preparation of the granules and their use described.
• Disintegrants for tablets or granules are auxiliary substances that disintegrate Tablets or granules in contact with liquids, especially water influence positively. It is said that both the disintegration of tablets into rough parts also a subsequent disintegration into smaller particles up to dissolution / Dispersion of all detergent components can be effected and accelerated.
• Tablets are determined by pressing a starting granulate with Press produced, the bulk density, e.g. for compact detergents approx. 900g / l, after tabletting rises to 1200 g / l.
• Such tablets with higher densities than the starting granulate are naturally less soluble / separable as the starting granulate. Since they are in use in the However, the washing machine should dissolve quickly or should disintegrate and dissolve, it is appropriate to add disintegrants that promote decay.
• the addition to the induction chamber is the most convenient for the user and for the user The safest quality of the washing process.
• the first step of disintegrating the tablet into large parts must be done very quickly go, because otherwise residues of the tablet remain in the dispenser and not can be used for washing.
• washing machines take about 30 seconds to rinse the tablets over the induction bowl available.
• the tablets must be used when hot perform their function even with cold induction water. Lie in the washing drum other conditions for the disintegration of the tablet, since both mechanical Friction as well as rising water temperatures the dissolution process of the tablet influence.
• DE-OS 2 251 249 e.g. rapidly disintegrating pharmaceutical tablets described by pressing pharmaceutical granules and Disintegrant granules are produced.
• the use of granular Starting materials lead to a porous tablet structure.
• An example is Disintegrant granules based on starch with a particle size of 2.0 to 0.3 mm used.
• No. 3,629,393 claims pharmaceutical tablets with delayed release of the active ingredient, which are pressed from granular components, disintegrants from high-molecular, water-swellable compounds, such as cellulose derivatives, being used in the form of granules.
• the granule dimensions in the examples are around 0.84 mm.
• US 4,072,535 describes the use of disintegrants made of precompacted starch for pharmaceuticals and detergents.
• the grain size of the compact is 0.05 mm to 0.42 mm, the moisture content is stated as 9-16%, preferably 11-13%.
• the disintegration times of the sample tablets are several minutes.
• Detergent tablets are known from DE-OS 2 321 693, which contain 1 to 25% by weight. contain fibrous cellulose as a disintegrant. In the examples Tablets made with a strength of 15 to 19 N, being compacted Cellulose granules can be used.
• tablet-like washing additives consist of granular constituents are pressed, 1 to 5% by weight also being granular tablet disintegrant based on cross-linked Polyvinyl pyrrolidone and / or cellulose ethers are used.
• the granules should be free of dust.
• the tablets have a breaking strength of 50 up to 120 N and have long dissolving times of several minutes.
• washing or cleaning-active moldings which can be produced using an explosive granulate that has a high Has adsorption capacity for water and a grain size distribution in which at least 90% by weight a particle size of at least 0.2 mm and a maximum of 3 mm have.
• the dust content ⁇ 0.1 mm is less than 1%.
• the explosive granules contains at least 20% by weight of disintegrants, such as starch, starch derivatives, Cellulose, cellulose derivatives. According to the teaching of this patent, this has an effect Presence of anionic or nonionic surfactants negatively affects the Tablet disintegration time.
• the granules are made in a conventional manner manufactured, such as spray drying, superheated steam drying of aqueous preparations or by granulation, pelleting, extrusion or roller compaction powder components. Detailed procedural information on Granulation process or further process steps after the granulation the explosive granules are not made.
• the example produced Detergent tablet contains a disintegrant based on compacted cellulose thermochemically treated wood pulp and has a tablet hardness of 45 N. on. Tablets of higher strength, i.e. above 50 N are not described.
• WO 98/55575 describes an auxiliary granulate for washing and detergent active moldings.
• the claimed auxiliary granules contain 10 to 95% by weight cellulose with particle sizes below 0.1 mm and 5 to 90% by weight microcrystalline cellulose.
• the celluloses partially with carboxymethyl cellulose, TAED and citric acid / bicarbonate combined.
• the grain sizes of the compact are more than 90% by weight from 0.3 to 2.0 mm, less than 5% by weight less than 0.2 mm and have no dust content.
• the Roll compacting of the dry premix is preferred. Detailed Process details for the production of granules are not given.
• the below Use of the auxiliary granules produced by way of example Detergent tablets have low strengths of 35 N or less. More stable, more compact tablets with higher strength from 50N not described.
• Patent application WO 98/40462 describes a compact made of powdered and / or granular ingredients, in particular detergent ingredients, which contains particles of cellulose-containing material acting as disintegrant, the can also be in a compact form.
• Particularly preferred as Cellulose components become thermomechanical (TMP) and chemical thermomechanical (CTMP) treated wood pulps.
• TMP thermomechanical
• CMP chemical thermomechanical
• the particle size of the compacted explosives can range from 0.2 to 6 mm.
• About the Cellulose components can also add tenside raw materials to the compact be mentioned, with 0.5 - 5% surfactant / compact. That corresponds to one Surfactant content of approx.
• the state of the art also includes sales products from Degussa AG with the designation Elcema G250 and Elcema G 400, which consists of compact Pure cellulose exist and have been used as a tablet disintegrant since 1971 become. 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 one compared to the prior art to provide improved disintegrant granules for tablets. It should in particular so swell so quickly and strongly that tablets made therewith in the induction chamber of washing machines during the short water induction period largely resolved. Furthermore, the explosive granules are said to be high Have abrasion stability and its effect not through in the course of its Manufacturing process inevitably occurring fine and in particular Dust levels can be restricted. Furthermore, the explosives are said to be in tablets with high strength over 50 N a combination of good explosive effect and ensure good solubility and by storing the tablets over several Weeks only slight signs of aging in the form of a weakening of the Experience properties.
• the task also includes the provision of a method for Production of the explosive granules and their use in tablets for Washing and cleaning processes.
• the disintegrant compactates are more effective if they have a certain water content. According to the Teaching of the state of the art and practical experience was to be expected that the lowest possible water content in the finished granulate is the best would cause swelling.
• Component A is a compound having Component A:
• water-insoluble, swellable cellulose is used.
• fibrils of native cellulose with a maximum length of 0.30 mm proven.
• microcrystalline and amorphous fine particles can be used Cellulose and mixtures thereof are used.
• the finely divided cellulose preferably has bulk densities of 40 g / l to 300 g / l, very particularly preferably from 65 g / l to 170 g / l.
• bulk densities 40 g / l to 300 g / l, very particularly preferably from 65 g / l to 170 g / l.
• They bulk density is higher and can be beneficial Execution range from 350 g / l to 550 g / l.
• the bulk weights of the cellulose derivatives are typically in the range from 50 g / l to 1000 g / l, preferably in the range from 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 medium one Particle size 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 the disintegrant granulate is between 60 to 99% by weight, preferably between 60 to 95% by weight.
• regenerated ones are also used Celluloses such as viscose are used. Particularly regenerated celluloses in Powder form are characterized by very good water absorption.
• the Viscose powder can be made from cut viscose fiber or by precipitation dissolved viscose. Also degraded by electron beam low molecular weight cellulose is for example for the production of Disintegrant granules suitable.
• softened regenerated fibers are used.
• a typical plasticizer for such products may be mentioned here, for example, glycerol.
• the granules according to the invention can be advantageous Embodiment water-swellable cellulose derivatives, such as cellulose ether and Cellulose esters and starch or starch derivatives and other swellable ones Contain polysaccharides and polygalactomannans, for example ionic modified celluloses and starches such as carboxymethyl modified cellulose and Starch, nonionically modified celluloses and starches such as alkoxylated celluloses and starches such as hydroxpropyl and hydroxyethyl starch or hydroxpropyl and hydroxyethyl cellulose and alkyl etherified products such as methyl cellulose as well as mixed modified celluloses and starches from the aforementioned Modifications, possibly combined with a modification to Networking leads.
• ionic modified celluloses and starches such as carboxymethyl modified cellulose and Starch
• nonionically modified celluloses and starches such as alkoxylated celluloses and starches
• Suitable starches are also cold swelling starches that are caused by mechanical or degrading reactions are formed on the starch grain. For this count primarily swelling starches from extruder and drum dryer processes as well products modified enzymatically, oxidizing or acid-degrading.
• Chemically Derivatized starches preferably contain substituents which are substituted by ester and A sufficient number of ether groups are attached to the polysaccharide chains
• Starches with ionic substituents such as carboxylate, hydroxyalkyl or Phosphate groups have proven to be particularly advantageous and are therefore preferred.
• To improve the swelling behavior has also proven the use of slightly cross-linked starches.
• alkaline Treated starches can be used because of their good cold water swellability become.
• the combination of cellulose with Cellulose derivatives and / or starch and / or starch derivatives have proven successful.
• the Quantities can fluctuate within wide limits, based on the Combination is the proportion of cellulose derivatives and / or starch and / or Starch derivatives preferably 0.1 to 85% by weight, particularly preferably 5 to 50% by weight.
• Component B is a compound having Component B:
• Polymers or copolymers of (meth) acrylic acid or Mixtures of such polymers or copolymers are used in the granulate.
• the polymers are selected from the group of homopolymers (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.
• Uncrosslinked polymers or copolymers of (Meth) acrylic acid with weight average molecular weights of 5,000 to 70,000 proven.
• the copolymers are preferably copolymers of (Meth) acrylic acid and ethylenically unsaturated dicarboxylic acids or their Anhydrides, such as maleic acid or maleic anhydride, for example 40 to 90% by weight of (meth) acrylic acid and 60 to 10% by weight of maleic acid or Contain maleic anhydride, their relative molar mass, based on free Acids, between 3,000 and 100,000, preferably 3,000 to 70,000 and whole is particularly preferably 5,000 to 50,000.
• binder ter- and quattropolymeric polycarboxylates have also proven to be built up from (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 from (meth) acrylic acid, maleic acid, vinyl alcohol derivatives and monomers containing sulfonic acid groups.
• suitable polymers are in the patents DE 43 00 772, DE 42 21 371 and WO 95/17444.
• the polymeric binders are preferred in the form of their preparation aqueous solutions used, but can also be in the form of finely divided powders be applied.
• the binder polymers are preferably in part or fully neutralized form, the salt formation preferably 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, particularly preferably between 5 and 15% by weight. Polymer contents above 15% in the disintegrant lead to harder ones Disintegrant granules, while polymer contents below 1% softer to form Granules tend to be less resistant to abrasion.
• Suitable polymer binders are also crosslinked polymers made from (meth) acrylic acid. They are preferably used as finely divided powders and are preferred average particle sizes from 0.045 mm to 0.150 mm and are preferred with 0.1 to 10 wt.% Used. Particles with average particle sizes over 0.150 mm also produce good disintegrant granules, but lead to the Dissolving the tablets made with the granules visually as particles visible swelling bodies, for example in the case of textile washes deposit clearly visible on the textile in a disturbing manner.
• a special embodiment of the invention is the combination of soluble poly (meth) acrylate homo- and copolymers and the aforementioned finely divided crosslinked polymer particles.
• the explosive granules contain one or more further constituents liquid, gel-forming surfactants selected from the group of nonionic, anionic or amphoteric surfactants, which are used in amounts up to 7 % By weight, preferably up to 3.5% by weight are present. If the surfactant content in the explosive is too high, in addition to increased abrasion manufactured tablets also have poor swelling properties.
• the nonionic surfactants can be, for example, alkyl polyglucosides, fatty acid alkylolamides, Fatty acid polyethylene glycol esters, fatty aminoxethylates, Fatty alcohol ethoxylates with 3-15 mol ethylene oxide or propylene oxide, Fatty acid glycerides, sorbitan esters, sucrose esters, e.g. Sucrose palmitate, Pentaaerythritol partial esters, which can also be ethoxylated, and alkylphenol polyethylene glycol ether or be phenol poly ethylene glycol ether.
• the anionic surfactants can be, for example, alkyl sulfates, linear and branched Alkylbenzenesulfonates, alkylglycerol ethers, fatty alcohol polyethylene glycol ether sulfates, Paraffin sulfonates, alpha olefin sulfonates, sulfosuccinates, phosphoric acid esters or Be fatty alcohol ether carboxylates.
• amphoteric surfactants can, for example, coconut fatty acid amidopropyl betaine, modified imidazolines or fatty acid amide derivatives with betaine structure.
• mixtures of Surfactants are used, in a further preferred embodiment only non-ionic surfactants used.
• the compacted granulate according to the invention is distinguished by a special one Swelling kinetics, the expansion does not change depending on the time linear but reaches a very high level after a very short time.
• the swelling behavior in the first 10 seconds is of particular interest after contact with water.
• This The combination of properties has a positive influence on those with the explosives tablets produced and leads to short tablet disintegration times and one very good flushing behavior in the dosing chambers of the washing machines. Both Wash-in tests show the superior effect of the agents according to the invention in 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. That way determinable water absorption is preferably 500 to 2000%
• the fluid intake (also called specific porosity) of the Disintegrant according to the invention is compared to products of the prior art Technology significantly increased and is in a range of over 750 ml / kg, preferably in the range 800 to 1000 ml / kg.
• This high fluid intake has a significant influence on the swelling effect and water transport in the Explosives.
• State of the art products have average Liquid absorption values of approx. 600 ml / kg.
• the disintegrant granules according to the invention are first produced by mixing the granulate components according to the invention with conventional mixing methods. For example, mixers from Vomm, Lödige, Schugi, Eirich, Henschel or Fukae can be used. In this first step of Mixing and granulating are precompounds Agglomeration process produced. These precompounds form a free-flowing Goods with a water content between 10 and 80% by weight.
• the required Water content in the premix depends on the one used Compression device. A water content of at least 10%, preferably 20% is required to achieve good compaction and high To guarantee liquid absorption in the later dry granulate.
• these pre-compounds are mechanically compressed.
• the swelling and water absorption behavior of the granules according to the invention is final compaction essential.
• Compacting using Printing can be done in different ways.
• the products can be between two Printing areas in roller compressors, e.g. B. smooth or profiled.
• the compactate is ejected as a strand.
• Compression methods in Matrices with stamps or pillow rollers produce compact forms such as tablets or briquettes.
• Roll compactors, extruders, Roller or cube presses, but also pelletizing presses are used.
• pelleting presses Compression with pelleting presses has proven to be particularly suitable, with a suitable process control granules are obtained without further size reduction can be dried.
• Suitable pelleting presses e.g. manufactured by Amandus Kahl and Fitzpatrick.
• an explosive granulate with a Bulk density 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.
• Compliance A preferred limit of the bulk density of a maximum of 400 g / l has changed the particularly good swelling properties proved to be favorable. Surprisingly, it was found that the granules also in these Bulk densities have very good abrasion resistance.
• the coarse, compacted particles are crushed, e.g. Mills, Carvers or roller mills are suitable.
• the shredding can take place before or after drying.
• the inventive Granules preferably with a particle size distribution of 0.05 to 3 mm, particularly preferably 0.1 to 1.5 mm.
• a removal of dust components below 0.1 mm can e.g. with usual Screening devices are carried out. Since dust content up to 10 wt Use of the granules according to the invention predominantly does not interfere their separation is often omitted.
• the water content according to the invention is 2-8% by weight, preferably 2.5-7% by weight and particularly preferably 3-5% by weight.
• dryers such as Roller dryer (temperatures e.g. from 95 - 120 ° C) or fluid bed dryer (temperatures e.g. from 70 - 100 ° C).
• the invention includes the use of the compacted granules as Disintegrants for pressed molded articles, for example tablets, cubes, balls and the like.
• Disintegrants for pressed molded articles, for example tablets, cubes, balls and the like.
• Use as a disintegrant for is particularly preferred Detergent formulations, detergent formulations, stain salts, Water softener in tablet or cube form.
• the disintegrant granules according to the invention are in the molded articles in quantities from 0.5% by weight to 15% by weight, preferably 3% by weight to 8% by weight and particularly preferably contain 4% by weight to 7% by weight.
• the moldings according to the invention have sufficient stability and Strength, and allow safe handling, packaging and Storage. Upon contact with water, however, they should disintegrate quickly, so that the Components can have the desired effect. Adequate Stability against mechanical influences is for molded articles from one Breaking strength of 50 N is given. Lend the granules according to the invention a decay and disintegration characteristic such as these highly compressed shaped bodies it is otherwise only given in the case of moldings of low strength.
• the moldings for detergent formulations usually contain Builders, bleaching agents and bleach activators, surfactants, tableting aids, Disintegrants and other usual additives and auxiliaries.
• Other components of the builder system can include fillers such as Alkali carbonates, bicarbonates e.g. B. sodium carbonate or sodium hydrogen carbonate, Sesquiocarbonates, sodium sulfate, magnesium sulfate, or citrate, citric acid, Succinic acid, tartaric acid and malic acid. Often called Auxiliary builders cobuilders and dispersants also used. Such cobuilders or Dispersants can be polyacrylic acids and their sodium salts.
• Copolymers of (meth) acrylic acid and maleic acid, terpolymers and Quattropolymers from (meth) acrylic acid, maleic acid, vinyl alcohol and vinyl compounds containing sulfo groups can be used.
• ter- and quatropolymeric polycarboxylates made from are also preferred (Meth) acrylic acid, maleic acid and vinyl alcohol or vinyl alcohol derivatives (such as they are described in DE 43 00 772 C2) or those made from (meth) acrylic acid, 2-alkylallylsulfonic acid and sugar derivatives (as described in DE 42 21 381 C1) or from (meth) acrylic acid, maleic acid, vinyl alcohol derivatives and Monomers with sulfonic acid groups (described in DE 195 16 957 A).
• Polyethylene glycol and / or polypropylene glycol are further components used with a molecular weight of 900 to 30,000, and carboxylated Polysaccharides, polyaspartates and polyglutamate. Mixtures with various organic builders such as Citric acid is possible.
• the usual 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 peracid salts, peracids such as perbenzoates, peroxyphthalates, diperazelaic acid and diperdodecanedioic acids.
• the bleach content 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 N-acyl and O-acyl compounds forming with H 2 O 2 organic peracids, preferably N, N'-tetraacylated diamines, carboxylic acid anhydrides and esters of polyols such as glucose pentaacetate. Acetylated mixtures of sorbitol and mannitol can also be used.
• Particularly suitable bleach activators are N, N, N ', N'-tetraacetylethylene diamine (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, for example quaternary ammonium compounds with C8 - C16 N-alkyl or N-alkenyl groups and N-substituents such as methyl, hydroxyethyl or Hydroxypropyl groups.
• Tableting aids are also optionally used, for example Polyalkylene glycols and magnesium stearates.
• Examples of other common detergent additives and auxiliaries are enzymes, Magnesium silicates, aluminum aluminates, benzotriazole, glycerin, Magnesium stearate, polyalkylene glycols, hexametaphosphate, phosphonates, Bentonites, soil release polymers, carboxymethyl celluloses.
• Dishwashing tablets as a form of training Detergent formulations usually contain builders Polyphosphates, pyrophosphates, metaphosphates or phosphonates, Layered silicates, amorphous silicates, amorphous disilicates and zeolites, as well as fillers such as sodium carbonate, sodium sulfate, magnesium sulfate, sodium hydrogen carbonate, Citrate as well as citric acid, succinic acid, tartaric acid and malic acid.
• Cobuilders and dispersants are often used as auxiliary builders. Such cobuilders or dispersants can be polyacrylic acids or copolymers with polyacrylic acid and its sodium salts.
• Customary bleaching agents 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 in the tablets is preferably 10-60% by weight and in particular 15-50% by weight.
• Low-foaming non-ionic surfactants of the type polyalkylene glycol and Alkyl polyglucosides are also used.
• Examples of other common detergent additives and auxiliaries are also here Enzymes, magnesium silicates, aluminum aluminates, benzotriazole, glycerin, Magnesium stearate, polyalkylene glycols, hexametaphosphate and phosphonates.
• Water softening tablets usually consist of builders such as Layered silicates, amorphous silicates, amorphous disilicates and zeolites, as well Fillers such as sodium carbonate, sodium sulfate, magnesium sulfate, Sodium bicarbonate, citrate and citric acid. Often called Auxiliary builders cobuilders and dispersants also used. Such cobuilders or Dispersants can be polyacrylic acids or copolymers with polyacrylic acid and their sodium salts.
• Low-foaming non-ionic surfactants of the type polyalkylene glycol and Alkyl polyglucosides are also used.
• Examples of other common detergent additives and auxiliaries are Magnesium silicates, polyalkylene glycols and phosphonates.
• Disintegrant granules possible detergent tablets with disintegration times of up to 15 sec 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 immersed 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 drain. The bag is weighed and the water absorption is determined from the weight difference of a wet bag with and without granules. Distilled water is used for the determination.
• the specific porosity of the disintegrant granules is determined using 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 centrifugation. The amount of DBP absorbed is taken as a measure of the porosity of the solid.
• DBP di-n-butyl phthalate
• a washing and cleaning tablet containing 5% disintegrant is used for used the test.
• a magnetic stir bar is placed in the beaker set in motion at approx. 200 rpm and a tablet on top of the sieve hung up.
• the time from the start of tablet addition until the tablet disintegrates is measured with a stopwatch. The disintegration is achieved when all tablet parts fell through the sieve.
• the Tablet breaking strength tester type TB30 / TBH30MD from Erweka used for the determination of the tablet breaking strength.
• the tensile strength is measured using a strain gauge a load cell.
• the measuring accuracy is +/- 1N.
• the tablet is placed in the measuring device inserted and the measuring process started.
• the device shows the value of the Breaking strength.
• the disintegrants used in the examples were produced by wet compaction on a pellet mill from 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 the compacting, the granules were dried to the specified moisture contents on a Babcok drum dryer. Comparative example V5 was produced on a WP 150 roller press from Alexanderwerke without additional water. The pressing pressure was set at 1.1 t / cm. The granules were crushed on a grater. Drying was also carried out 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.
• a roller-compacted cellulose from Degussa AG with the trade name Elcema G 250 was used as comparative example V2 . (5% moisture, bulk density 400 g / l
• example M2 When comparing example M2 according to the invention with example V2 there are significant differences in fluid intake caused by Compacting process and the moisture content when compacting are justified.
• moisture content according to the invention when compacting and drying (M2) result in 950 ml / kg intake of DBP
• the dry compact and thus compressed pattern (V2) in the capillary structure resulted in a Consumption of only 600 ml / kg DBP.
• Table 3 shows the strength and the results of the induction test of the individual detergent tablets when using the different disintegrants: Explosives according to example Humidity (%) Wash-in test (not disassembled tabl.) Strength [N] Disintegration time [sec] V1 18th 10th 61 50 V2 5 10th 58 52 V3 10th 6 60 40 M1 6 1 62 12th M2 4th 0 65 9 V4 1 3rd 58 25th M3 3rd 0 57 8th M4 3rd 1 63 10th M5 4th 1 58 9 M6 5 0 59 7 M7 3rd 0 58 9
• Table 3 shows that both the composition and the same Composition the moisture content of the explosive granules one have a significant influence on the tablet disintegration time. Explosives with the preferred content of 3-5 wt% water as in M2 also show the best Disintegration times of the tablets. Are also suitable swellable Substances incorporated as a disintegrant component can Disintegration properties can be further increased.
• Table 4 shows the influence of the storage time (4 weeks at 40 ° C / 60% relative humidity in the closed container) on the induction behavior of tablets with disintegrants.
• Detergent tablet containing phosphate according to Table 2 example Disintegrant moisture [%] Wash-in test immediately (Tablet) n. 4 weeks Swelling kinetics after 3 seconds [mm] V4 1 3rd 3rd 0.85 M1 6 1 1 0.90 M2 4th 0 1 0.97 V3 10th 6 7 0.80 V1 18th 10th 11 0.45 V2 6 10th 11 0.47 M3 3rd 0 - 2.0 M4 3rd 1 - 1.7 M5 4th 1 - 1.6 M6 5 0 - 2.2
• Table 4 shows that the moisture content according to the invention in Disintegrant granules to superior properties of the manufactured Tablets in the important wash-in test leads or that the swellability with values of 0.9 and higher is superior to the comparison products.
• Tablets with Disintegrants according to the invention show good storage stability.
• Tablets with In addition to cellulose, M3-M6 also contain cellulose derivatives and show thereby further improved swelling kinetics.
• the comparative granules V1 and V2 show significantly less activity than the product according to the invention from example M6 / M7.
• Commercial tablets show different dissolving behavior.
• Low strength tablets dissolve faster than high strength tablets.
• Granules from Example M3 in disilicate-based detergent formulations Raw material quantity in% by weight Recipe a) b) Amorphous disilicate 36 30th Fatty alcohol ethoxylate 2nd 7 Fatty alcohol sulfate 11 15 Linear alkyl benzene sulphonate 4th 2nd Sodium percarbonate 16 16 TAED 4th 4th Acrylate-maleate copolymer - 3rd soda 7 4th Sodium citrate 5 5
• Example M3 The granules from Example M3 led to very good disintegration times for disilicate tablets.
• Water softener with the following composition: Raw material quantity in% by weight Zeolite 15 Sodium bicarbonate 32 citric acid 20th Polycarboxylate 17th Layered silicate 8th Process aids 5 Disintegrant preparation according to Example M2 or V2 3rd
• Machine dishwashing detergent of the following composition: Raw material quantity in% by weight Soda-silicate cogranulate 20th Tripolyphosphate 35 soda 20th Sodium perborate 12th TAED 4th Enzyme mix 2nd Process aids 3rd Perfume, dyes 2nd Explosives preparation according to example M2 or V2 2nd
• the tablet disintegration time of highly compressed tablets with the inventive Disintegrant is superior to the comparison products.

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• Chemical & Material Sciences (AREA)
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• Chemical Kinetics & Catalysis (AREA)
• Oil, Petroleum & Natural Gas (AREA)
• Wood Science & Technology (AREA)
• Organic Chemistry (AREA)
• Health & Medical Sciences (AREA)
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• Emergency Medicine (AREA)
• Detergent Compositions (AREA)
• Medicinal Preparation (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 PT PT99106370T patent/PT1043391E/pt unknown
  • 1999-03-29 AT AT99106370T patent/ATE334187T1/de active
  • 1999-03-29 EP EP99106370A patent/EP1043391B1/fr not_active Expired - Lifetime
• 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 HU HU0001329A patent/HU228596B1/hu not_active IP Right Cessation
  • 2000-03-29 TR TR2000/00832A patent/TR200000832A2/xx unknown

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