EP1349914B1 - Verfahren zur herstellung von reinigungsmitteln - Google Patents
Verfahren zur herstellung von reinigungsmitteln Download PDFInfo
- Publication number
- EP1349914B1 EP1349914B1 EP01272727A EP01272727A EP1349914B1 EP 1349914 B1 EP1349914 B1 EP 1349914B1 EP 01272727 A EP01272727 A EP 01272727A EP 01272727 A EP01272727 A EP 01272727A EP 1349914 B1 EP1349914 B1 EP 1349914B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- weight
- pellets
- zeolite
- processing aid
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
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
- C11D3/20—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
-
- 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
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
- C11D3/1246—Silicates, e.g. diatomaceous earth
- C11D3/128—Aluminium silicates, e.g. zeolites
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- 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
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/04—Carboxylic acids or salts thereof
Definitions
- This invention relates to a solid laundry cleaning agent and its manufacture.
- the invention relates in particular to a laundry cleaning agent in pressed block form (hereinafter “laundry tablet”), but is also applicable to particulate laundry cleaning agents (hereinafter “washing powder”).
- laundering powder particulate laundry cleaning agents
- a known laundry tablet comprises about 10% of a sodium (linear C 8-15 alkyl) benzene sulfonate, about 6 wt% of zeolite, about 12% of sodium carbonate, about 15% of sodium citrate dihydrate, about 20% of an amorphous silicate, present as a builder, about 10% of a cellulosic disintegrant and about 27% of additional ingredients (weight/tablet weight).
- a tablet is formed by simple dry mixing of a typical tower base powder with all the other ingredients, followed by tabletting the mixture in a standard tabletting machine, such as a Korsch rotating press.
- EP-B-486592 a process for the production of compacted granules for use in detergents.
- a homogenous premix to which a plasticizer and/or lubricant is added, is extruded through perforated dyes under high pressure to form strands which are cut into pieces.
- the premix may be of a tower powder. Zeolite is mentioned as a possible drying powder, to prevent the granules from sticking together, and as a possible premix component, albeit not in very high amounts.
- pelletisation - as distinct from extrusion - can be used as a key step in the manufacture of advantageous laundry tablets.
- Those laundry tablets can achieve the aims noted above - thus, they can be of high density; be small tablets; have high zeolite content; have low disintegrant content; fast disintegration; and have a low or no amorphous silicate content.
- the present invention offers the prospect of advantageous washing powders, with high bulk density, high zeolite content and low or no amorphous silicate content.
- a method of making a solid laundry cleaning agent comprising the steps of pelletising a flowable tower spray powder and a flowable zeolitic powder in a pellet mill to form a premix comprising pellets with a zeolite content of at least 30% (weight of zeolite/weight of pellets); and mixing (hereinafter also called post-mixing) the pellets with the other ingredient(s) of the solid laundry cleaning agent, wherein the zeolitic powder is a zeolite admixed with up to 10% of a processing aid (weight of processing aid/weight of zeolitic powder including processing aid), the processing aid being selected from a nonionic surfactant, an acrylic polymer or copolymer; starch or a derivative thereof; gelatin; polyvinyl alcohol; soap; and water
- the tower spray powder is made up of the following constituents (weight/weight of tower spray powder): 20-60% anionic surfactant; 0-15% processing aid; 0-25% further zeolite; 12-45% inorganic alkali metal, preferably sodium, salt; and. 0-20% additional constituent(s).
- the tower spray powder comprises 30-50% of one or more anionic surfactant.
- Preferred anionic surfactants for the tower spray powder include (but are not limited to) alkali metal salts, ammonium salts, amine salts, aminoalcohol salts or magnesium salts of one or more of the following compounds: alkylsulphonates, alkylamide sulphonates, alkylarylsulphonates, olefinsulphonates, alkylamide sulphonates, alkyl sulfosuccinates, alkyl ether sulfosuccinates, alkylamide sulfosuccinates, alkyl sulfosuccinamate, alkyl sulfoacetates, acyl sarconsinates, acyl isothionates and N-acyl taurates.
- the alkyl or acyl group in these various compounds comprises a carbon chain containing 8 to 22, preferably, 12 to 20, carbon atoms.
- anionic surfactants which may be used include salts (having cations as described above) of fatty acids, individually or as mixtures, including salts of oleic and stearic acids, and of acids of palm kernel oil, coconut oil and tallow; and lactylates whose acyl group contains 8 to 20 carbon atoms.
- Especially useful are solid soaps, and preferably solid alkali metal salts of C 16-18 saturated fatty acids, especially of tallow fatty acids, as these are useful also as processing aids.
- An especially preferred anionic surfactant for use in the present invention is an alkali metal, preferably sodium, salt of a (C 8-15 - preferably C 9-13 linear alkyl)benzene sulphonic acid (hereinafter 8-15 LAS and 9-13 LAS).
- an alkali metal salt of an alkylbenzene sulphonic acid for example an LAS
- an alkylbenzene sulphonic acid for example an LAS
- an alkali metal salt of an alkylbenzene sulphonic acid (for example an LAS) is not present in the zeolitic powder which is to be pelletized.
- an anionic surfactant is present in the zeolitic powder which is to be pelletized.
- an alkali metal salt of an alkylbenzene sulphonic acid for example an LAS
- an alkylbenzene sulphonic acid for example an LAS
- the pellets do not contain any anionic sulphate surfactant.
- the post-mixed ingredients include an anionic sulphate surfactant, suitably providing 2-10%, preferably 3-7%, of the final cleaning agent (weight/weight).
- Suitable anionic sulphate surfactants may include alkyl sulphates, alkyl ether sulphates, alkylamidoether sulphates, alkylaryl polyether sulphates, monoglyceride sulphates.
- alcohol sulphates are especially preferred.
- an alkyl group in these sulphate compounds is a C 8-22 , preferably C 12-20 , alkyl group.
- the processing aid improves the efficiency of a later pelletisation step and/or of a later tabletting step, where provided.
- a suitable processing aid preferably functions as a plasticizer or lubricant. These aids include a solid soap; an acrylic/ maleic anhydride copolymer.
- Suitable nonionic surfactants include alkoxylated alcohols, particularly alkoxylated fatty alcohols. These include ethoxylated and propoxylated fatty alcohols, as well as ethoxylated and propoxylated alkyl phenols, both having alkyl groups, suitably linear or secondary, of from 7 to 18, more preferably 8 to 16 carbon chains in length, and an average of 2 to 20 moles, preferably 2 to 10, most preferably 4 to 6 moles of alkylene oxide per mole of alcohol or phenol. Ethoxylated compounds are generally preferred.
- nonionic surfactants that may be used are sorbitan esters of fatty acids, typically fatty acids having from 10 to 24 carbon atoms, for example sorbitan mono oleate.
- nonionic surfactants that may be used are amine oxides and polyhydroxy fatty acid amides.
- the processing aid where provided, is present in an amount of from 1-10%, preferably 2-8%, more preferably 3-5% (weight/weight of cleaning agent).
- the tower spray powder may include further zeolite, but this is not essential.
- the further zeolite preferably provides 4-30%, more preferably 6-20%, of the cleaning agent (weight/weight).
- the further zeolite it is less than the input of zeolite from the zeolite powder added to the tower spray powder.
- Suitable inorganic sodium salts may be selected from sodium silicate, sodium carbonate and sodium sulphate.
- each of these salts is present, and each, preferably, is in the range 4-15%, most preferably 5-12% (calculated as anhydrous amount).
- Additional constituents of the tower spray powder may be selected from a stabilizer, particularly for a per compound or an enzyme.
- Suitable stabilizers are salts of polyphosphonic acids, such as 1-hydroxyethane-1,1-diphosphonic acid (HEDP), diethylenetriaminopentamethylene phosphonic acid (DETPMP), ethylenediaminotetramethylene phosphonic acid (EDTMP) and aminotrimethylene phosphonic acid (ATP).
- HEDP 1-hydroxyethane-1,1-diphosphonic acid
- DETPMP diethylenetriaminopentamethylene phosphonic acid
- ETMP ethylenediaminotetramethylene phosphonic acid
- ATP aminotrimethylene phosphonic acid
- an optical brightener for example a suitable stilbene compound, in particular diaminostilbene disulfonic acid or a derivative thereof, especially an alkali metal salt.
- An optical brightener may conveniently be delivered via the tower spray powder.
- a soil redeposition inhibitor for example one or more of polyvinyl pyrollidone, carboxymethyl-cellulose-sodium salt (CMC) or methylcellulose (MC).
- a soil redeposition inhibitor may conveniently be delivered via the tower spray powder.
- the additional constituents of the tower spray powder do not comprise in total more than 10% of the tower spray powder (weight/weight).
- each individual additional constituent will not comprise more than 2% of the tower spray powder (weight/weight).
- the flowable zeolitic powder comprises at least 80 wt% zeolite, and preferably at least 90 wt% zeolite.
- references to “zeolite” are to substantially virgin zeolite, including bound water of crystallisation and any atmospherically absorbed unbound water that may be present, but not including deliberately added materials.
- “Zeolitic powder” denotes zeolite (as just defined) and also such a material containing deliberately added.material(s).
- both the tower spray powder and the flowable zeolitic powder are preferably macroscopically dry when delivered to the pellet mill. Preferably, both are free-flowing.
- the amount of liquid components present (if any) must not be such that the respective powders become damp, or sticky, or prone to form lumps.
- Zeolite for use in the present invention is desirably stored in conditions which discourage water take-up from the atmosphere; for example it can be stored in closed or sealed plastic sacks.
- zeolite MAP zeolite MAP
- zeolite X zeolite X
- zeolite P zeolite P
- suitable types are the natural materials analcite, chabazite, heulandite, stilbite, faujasite, natrolite and thomsite.
- Preferred zeolite for use in the present invention is zeolite A.
- the tower spray powder and the zeolitic powder are preferably mixed upstream of the pellet mill in a separate unit, for example a vertical mixer/granulator, a horizontal mixer/granulator or a tumbler unit, all of which are conventional. Preferably, no heating is provided during this step.
- the zeolite content of the pellets is at least 35%, more preferably at least 40%. Most preferably, it is at least 45% and, especially, at least 50%.
- the zeolite content of the pellets does not exceed 80%, more preferably 70%, most preferably the zeolite content of the pellets does not exceed 65%.
- pelletisation in a standard pellet mill e.g. a Kahl mill or a UMT mill, is efficient and unproblematic. This was unexpected given the failure we encountered in trying to extrude such materials.
- pellet mills Further information on pellet mills is readily available. Examples of patents concerning rotary pellet mills include DE 3813081 , DE 3806945 and DE 3432780 .
- Preferably external heat is not provided in the pelletising step.
- the temperature of the material being pelletised rises moderately, typically to temperatures in the range 30-55°C, without detriment.
- the tower spray powder and the flowable zeolitic powder, as defined above, are preferably mixed together without any further material.
- pellets which are products of the pellet mill are chopped strands, "shaved" from the outer wall of the pellet mill as pelletisation proceeds. Based on our work to date it does not seem necessary from a technical standpoint to treat the pellets in any way before mixing them with post-mixed ingredients, to form the end laundry cleaning agent. However, they could if wished, primarily for aesthetic reasons, be given a simple mechanical treatment in a "ploughshare" shovel mixer, to reduce their mean aspect ratio, to be as close as possible, what may be considered to be the aesthetic ideal, 1:1 (pellet length:maximum diameter). We have found it easy to reduce the mean aspect ratio of the as-formed pellets, by feeding them straight from the pellet mill into the shovel mixer, preferably when the pellets are still warm.
- pellets may be spheronized. Preferably, however, the pellets are not spheronized.
- pellets may be dusted with a powder to aid flowability.
- the pellets are not dusted.
- the mean aspect ratio of the pellets used in the post-mixing is in the range 0.5-5:1, more preferably 0.8-3:1 (pellet length:maximum diameter).
- the pellets are circularly cylindrical and so the aspect ratio denotes length:diameter.
- the pellets from the pellet mill are given a mechanical treatment to reduce their mean aspect ratio, to be within this range.
- the pellets are intended as a universal base material to which the post-mixing ingredient(s) can be added, for example to make a heavy duty laundry detergent product, or a color care laundry detergent product.
- the pellets themselves preferably do not contain any of the "specialist" ingredients which are characteristic of such products.
- the pellets preferably do not contain any enzymes, bleaching compounds or bleach activators.
- the post-mixing ingredient(s) will depend on the target use for the laundry cleaning agent - for example for general purpose laundry; for heavy duty/white clothes; or for colored clothes.
- the ratio of the pellets to the post-mixing ingredient(s) is in the range of 20-80 : 80-20 (weight/weight).
- the ratio is in the range of 40-70 : 60-30.
- the ratio is in the range 50-60 : 50-40.
- the post-mixing ingredient(s) suitably include one or more of the following: a surfactant, for example an anionic and/or nonionic surfactant; sodium bicarbonate; sodium carbonate; sodium citrate; an anti-foaming agent; an enzyme; a bleaching agent; a bleach activator; a stabilizer, for example of the phosphonate type as defined above; a soil release polymer; a soil redeposition inhibitor; an optical brightener; a fabric softener; a colorant; and a fragrance.
- a surfactant for example an anionic and/or nonionic surfactant
- the surfactant component of the post-mixing ingredient(s) is relatively small, suitably making up not more than 10% of the total weight of post-mixing ingredient(s).
- the post-mixing ingredients may include an alcohol sulphate and this is preferably the only anionic surfactant component, and preferably the only surfactant component, in the post-mixing ingredient(s).
- the major complement of post-mixing ingredient(s) is a bleaching agent, for example sodium percarbonate, and a bleach activator, for example TAED; together preferably constituting at least 50% of the weight of post-mixing ingredient(s).
- one or more enzymes for example, protease, amylase and cellulase, may comprise at least 2% of the weight of post-mixing ingredient(s). At least 40% of the weight of post-mixing ingredient(s) may be made up of sodium bicarbonate and/or sodium carbonate and/or sodium citrate.
- a particulate laundry cleaning agent may be made by simple mixing of the pellets and the post-mixing ingredient(s), for example in a tumbler unit.
- the bulk density of the resulting particulate material is typically high, suitably at least 750g/l, preferably at least 800 g/l.
- preferred laundry cleaning agents of the present invention are laundry tablets. Therefore, the invention preferably includes the step, after the step of mixing the pellets with the other ingredients, of pressing the particulate material to form a tablet.
- the tablet may be formed with two or more layers of different composition, thereby keeping apart any materials which it would be undesirable to mix prior to use - for example a bleach and a bleach activator; or bleach and enzymes.
- one of the post-mixing ingredient(s) is a disintegrant, for example a rapidly water-swellable material, especially a water-swellable cellulosic material.
- a disintegrant for example a rapidly water-swellable material, especially a water-swellable cellulosic material.
- the disintegrant provides less than 10% of the total weight of the tablets of the present invention and preferably not more than 8%.
- tablets of very high density may be produced. This is significant because, for a given cleaning power, the tablets are smaller than prior tablets, and this brings about several significant advantages. For example, they may fit in washing machine drawers whereas larger tablets do not.
- the tablets produced in accordance with the present invention have a density of at least 1 kg/l. More preferably, the tablets have a density of at least 1.1 kg/l and most preferably at least 1.15 kg/l.
- the tablets have a hardness of at least 50 N, preferably at least 80 N, as measured by a dynamometer as the maximum force required to break the upper surface of the tablet when a perpendicular force is applied to the centre of it, by a vertically orientated cylinder of diameter 0.5cm.
- the tablets have a disintegration time of not more than 30 seconds, more preferably not more than 25 seconds, most preferably not more than 20 seconds, as measured by a standard method in which a laundry tablet is placed in a stainless steel mesh ladle, with mesh holes approximately 5mm x 5mm, and then successively lowered into and raised from a transparent tank containing 800 ml water at 20°C at a frequency of 60 immersions per minute. When no solid residue of the tablet can be seen within the ladle, the time is recorded ("disintegration time").
- the pellets, and the other ingredients of the washing powder or of the particulate material to be tabletted are of size such that at least 90 wt% thereof are in the size range 150-1200 ⁇ m, more preferably in the size range 250-1000 ⁇ m (as determined by standard mesh test, employing ASTM sieves and a Retsch vibrator with predetermined amplitude and working time).
- pellets and/or the particulate material resulting from the post-mixing may be graded, and overly large or small particles removed, for example for recycling.
- the laundry tablets may have an exceptional combination of beneficial properties, namely high density, high zeolite content and a low amount of disintegrant (all of which would normally lead to long disintegration time); and yet, unexpectedly, exhibit a short disintegration time.
- Prior tablets have contained large amounts of silicates as builders. Solid laundry cleaning agents made using the present invention, whether washing powders or laundry tablets, do not require such high amounts of such silicates.
- the content of silicon-containing compounds (not including zeolite) in the laundry cleaning agent is less than 10%, more preferably less than 5%.
- the solid laundry cleaning agents of the present invention contain no phosphate detergents.
- the amount of surfactants in the cleaning agent is at least 10% by weight. Preferably it does not exceed 30%, more preferably 25%, by weight.
- the zeolite content of the cleaning agent is at least 15% by weight, more preferably at least 20%, most preferably at least 25%, and, especially at least 30%.
- a solid laundry cleaning agent comprising: a premix of a flowable tower spray and a flowable zeolitic powder formed into pellets in a pellet mill, the resulting pellets having a zeolite content of at least 30% (weight of zeolite/weight of pellets); and other ingredients mixed with the premix to form the cleaning agent, the zeolite content of the cleaning agent being at least 15% (weight of zeolite/weight of cleaning agent), wherein the zeolitic powder is a zeolite admixed with up to 10% of a processing aid (weight or processing aid/weight of zeolitic powder including processing aid), the processing aid being selected from a nonionic surfactant; an acrylic polymer or copolymer; starch or a derivative thereof; gelatin; polyvinyl alcohol; soap; and water.
- a processing aid weight or processing aid/weight of zeolitic powder including processing aid
- a tower spray powder having the following ingredients was prepared in the conventional manner, in a vertical tower, from an aqueous slurry.
- CMC 1.01
- Sodium sulphate 10.54 Water & minors 3.43 TOTAL 100.0
- the tower spray powder was produced in standard manner.
- the soap was in the form of powder waste from soap production.
- the tower spray powder was mixed in equal weight with dry, virgin zeolite A powder (MICOLAN 1), in a tumbler mixer.
- the zeolite had been stored in sealed plastic sacks and nothing was added to it before the mixing.
- the mixed material was fed into a Kahl pellet mill operated at 100 rpm to yield circularly cylindrical pellets, 1.3mm in diameter and approximately 8-10mm in mean length.
- the temperature of the pellets as they issued from the pellet mill was about 30-40°C. They were passed directly to a Lödige batch mixer, in which a short treatment with rotating ploughshare shovels reduced the mean length of the pellets to approximately 2-4mm. At this point they were graded using a sieve, to remove powder for recycling.
- zeolite A made up 64.1% of the weight of Pellets A.
- zeolitic powder was used, made up of 90% of the dry, virgin zeolite A and 10% soap as described above (weight:weight). This zeolitic powder was mixed in equal weight with the tower spray powder.
- zeolite A made up 59.1% of the weight of Pellets B.
- Pellets A as described above were post-mixed with the following ingredients in a standard tumbler mixer in the proportions stated to yield a high density washing powder intended for washing colored fabrics.
- Ingredients % Pellets A 60.00 Fatty alcohol sulphate needles 4.5 C 13-15 Aliphatic alcohol, ethoxylated (7 EO) 5.0 Sodium carbonate 12.97 Sodium citrate dihydrate 10.0
- Antifoam powder polysiloxane supported on starch
- Enzymes protease, amylase, cellulase
- Soil release polymer polyethylene glycol/polyester compound 1.5 HEDP 0.8 Perfume 0.5 TOTAL 100.00
- This tablet was composed of two layers, produced in standard manner in a Korsch press. The two layers are made up as follows. Blue Phase White Phase Finished tablet (30% blue + 70% white) Pellets B 55.0 55.0 55.0 Fatty alcohol sulphate needles 4.00 4.00 4.00 Nonionic surfactant (C 13-15 alkyl, 5 EO) 3.5 1.00 1.75 Silicate builder 9.64 1.53 3.96 Sodium percarbonate - 28.57 20.00 Bleach activator (TAED) 15.0 - 4.50 Enzymes (protease, amylase, cellulase) 2.66 - 0.80 Granular disintegrant 7.00 7.00 7.00 Antifoam (as above) 0.27 0.27 0.27 Blue dye 0.013 - 0.004 Perfume - 0.29 0.2 Water & minors to 100.00 to 100.00 to 100.00 (weight percentages stated)
- the silicate builder had a ratio of SiO 2 :Na 2 O of 2.85:1 (weight:weight).
- the resulting two layer disc-shaped tablet had the following characteristics.
- Pellets B as described above were mixed together with further ingredients in a standard tumbler mixer in the proportions stated below to yield a high density washing powder intended for washing heavily soiled white fabrics.
- Pellets B 60.0 Alcohol sulphate granules 4.32 Nonionic surfactant (C 13-15 alkyl, 5 EO) 3.00 Silicate builder 4.00 Sodium percarbonate 20.00 Bleach activator (TAED) 4.50 Enzymes (protease, amylase) 0.80 Antifoam powder 4256 0.27 Perfume 0.5 Water & minors to 100.00 (weight percentages stated)
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Molecular Biology (AREA)
- Inorganic Chemistry (AREA)
- Detergent Compositions (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Claims (18)
- Verfahren zur Herstellung eines festen Waschmittels, umfassend die Schritte, ein fließfähiges Turmsprühpulver und ein fließfähiges zeolithisches Pulver in einer Pelletieranlage zu pelletieren, um ein Vorgemisch zu bilden, das Pellets mit einem Zeolithgehalt von wenigstens 30% (Gewicht des Zeoliths / Gewicht der Pellets) umfasst; und die Pellets mit dem bzw. den anderen Inhaltsstoff(en) des festen Waschmittels zu vermischen, wobei das zeolithische Pulver ein Zeolith ist, dem bis zu 10% eines Verarbeitungshilfsstoffes (Gewicht des Verarbeitungshilfsstoffes / Gewicht des zeolithischen Pulvers einschließlich Verarbeitungshilfsstoff) beigemischt sind, wobei der Verarbeitungshilfsstoff aus einem nichtionischen Tensid, einem Acrylpolymer oder -copolymer, Stärke oder einem Derivat daraus, Gelatine, Polyvinylalkohol, Seife und Wasser ausgewählt ist.
- Verfahren gemäß Anspruch 1, wobei die Pellets einen Zeolithgehalt von wenigstens 40% haben.
- Verfahren gemäß Anspruch 1 oder 2, wobei der Zeolithgehalt der Pellets 80% nicht überschreitet.
- Verfahren gemäß Anspruch 1, 2 oder 3, wobei der Verarbeitungshilfsstoff Festform hat.
- Verfahren gemäß Anspruch 4, wobei der Verarbeitungshilfsstoff eine Natrium- und/oder Kaliumseife aus einer Fettsäure ist, die aus einer Talgfettsäure, Kokosölfettsäure, Palmkernölfettsäure, Oleinsäure und Stearinsäure ausgewählt ist, wobei die Seife partikuläre Form hat.
- Verfahren gemäß einem der vorhergehenden Ansprüche, wobei das zeolithische Pulver Zeolith A umfasst.
- Verfahren gemäß einem der vorhergehenden Ansprüche, wobei das Turmsprühprodukt aus den folgenden Bestandteilen besteht (Gewicht der Bestandteile / Gewicht des Turmsprühpulvers):20 - 60% anionische(s) Tensid(e)0-15% Verarbeitungshilfsstoff(e)0 - 25% weitere(s) Zeolith(e)12 - 45% anorganische(s) Alkalimetallsalz(e)0 - 20% zusätzliche(r) Bestandteil(e)
- Verfahren gemäß einem der vorhergehenden Ansprüche, nach der Pelletierung den Schritt umfassend, die Pellets mechanisch zu bearbeiten, um ihr Aspektverhältnis zu reduzieren.
- Verfahren gemäß einem der vorhergehenden Ansprüche, wobei das Verhältnis der Pellets zu dem bzw. den anderen Inhaltsstoff(en) im Bereich von 20 - 80 : 80 - 20 liegt (Gewicht der Pellets / Gewicht der anderen Inhaltsstoffe).
- Verfahren gemäß Anspruch 9, wobei das Verhältnis der Pellets zu dem bzw. den anderen Inhaltsstoff(en) im Bereich von 40 - 70 : 60 - 30 liegt.
- Verfahren gemäß einem der vorhergehenden Ansprüche, wobei der bzw.
die andere(n) Inhaltsstoff(e) einen oder mehrere der folgenden Inhaltsstoffe aufweisen:ein Tensid; Natriumbicarbonat; Natriumcarbonat; Natriumcitrat, ein Antischaummittel; ein Enzym; ein Bleichmittel; einen Bleichaktivator; einen Stabilisator; ein Schmutzlösepolymer; einen Vergrauungsinhibitor; einen Textilweichmacher; einen Farbstoff und einen Duftstoff. - Verfahren gemäß einem der vorhergehenden Ansprüche, wobei das entstehende partikuläre Material eine Schüttdichte von wenigstens 750 g/l hat.
- Verfahren gemäß einem der vorhergehenden Ansprüche, nach dem Schritt des Mischens den Schritt umfassend, das partikuläre Material zu pressen, um eine Tablette auszubilden.
- Verfahren gemäß Anspruch 13, wobei der bzw. die andere(n) Inhaltsstoff(e) ein Abbaumittel aufweisen.
- Verfahren gemäß Anspruch 13 oder 14, wobei die Tablette eine Dichte von wenigstens 1 kg/l hat.
- Verfahren gemäß Anspruch 13, wobei die Tablette eine Dichte von wenigstens 1,1 kg/l hat.
- Festes Waschmittel, das mit einem Verfahren gemäß einem der vorhergehenden Ansprüche erzeugt ist.
- Festes Waschmittel, umfassend ein Vorgemisch aus einem fließfähigen Turmsprühstoff und einem fließfähigen zeolithischen Pulver, die in einer Pelletieranlage zu Pellets ausgebildet sind, wobei die entstehenden Pellets einen Zeolithgehalt von wenigstens 30% haben (Gewicht des Zeoliths /Gewicht der Pellets); und andere Inhaltsstoffe, die mit dem Vorgemisch vermischt sind, um das Waschmittel auszubilden, wobei der Zeolithgehalt des Waschmittels wenigstens 15% (Gewicht des Zeoliths / Gewicht des Waschmittels) beträgt, wobei das zeolithische Pulver ein Zeolith ist, dem bis zu 10% eines Verarbeitungshilfsstoffes (Gewicht des Verarbeitungshilfsstoffes / Gewicht des zeolithischen Pulvers einschließlich Verarbeitungshilfsstoff) beigemischt sind, wobei der Verarbeitungshilfsstoff aus einem nichtionischen Tensid, einem Acrylpolymer oder -copolymer, Stärke oder einem Derivat daraus, Gelatine, Polyvinylalkohol, Seife und Wasser ausgewählt ist.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB0100412 | 2001-01-08 | ||
GB0100412A GB2370843A (en) | 2001-01-08 | 2001-01-08 | Laundry cleaning agents and their manufacture |
PCT/GB2001/005769 WO2002053697A1 (en) | 2001-01-08 | 2001-12-24 | A process for the production of cleaning agents |
Publications (3)
Publication Number | Publication Date |
---|---|
EP1349914A1 EP1349914A1 (de) | 2003-10-08 |
EP1349914B1 true EP1349914B1 (de) | 2009-12-16 |
EP1349914B2 EP1349914B2 (de) | 2013-09-04 |
Family
ID=9906405
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP01272727.7A Expired - Lifetime EP1349914B2 (de) | 2001-01-08 | 2001-12-24 | Verfahren zur herstellung von reinigungsmitteln |
Country Status (6)
Country | Link |
---|---|
EP (1) | EP1349914B2 (de) |
AT (1) | ATE452178T1 (de) |
DE (1) | DE60140821D1 (de) |
ES (1) | ES2337443T5 (de) |
GB (1) | GB2370843A (de) |
WO (1) | WO2002053697A1 (de) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102008060469A1 (de) * | 2008-12-05 | 2010-06-10 | Henkel Ag & Co. Kgaa | Maschinelle Geschirrspülmitteltablette |
GB2544470B (en) * | 2015-11-16 | 2019-06-05 | Reckitt Benckiser Vanish Bv | Laundry composition |
CN113136266A (zh) * | 2021-04-30 | 2021-07-20 | 东莞市合信新材料有限公司 | 一种固体洗衣去污球及其制备方法 |
Family Cites Families (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5376288A (en) † | 1989-06-21 | 1994-12-27 | Noro Nordisk A/S | Detergent additive granulate and detergent |
DE4010533A1 (de) * | 1990-04-02 | 1991-10-10 | Henkel Kgaa | Tablettierte wasch- und/oder reinigungsmittel fuer haushalt und gewerbe und verfahren zu ihrer herstellung |
DE3926253A1 (de) † | 1989-08-09 | 1991-02-14 | Henkel Kgaa | Verdichtete wasch- und reinigungsmittel in granulatform, verfahren zu ihrer herstellung und anwendung des verfahrens zur gewinnung lagerstabil rieselfaehiger waschmittel-konzentrate |
DK0486592T3 (da) * | 1989-08-09 | 1994-07-18 | Henkel Kgaa | Fremstilling af kompakterede granulater til vaskemidler |
DE4034131C2 (de) † | 1990-10-26 | 1999-08-26 | Henkel Kgaa | Gerüststoff für Waschmittel |
JP2951743B2 (ja) † | 1991-05-09 | 1999-09-20 | 花王株式会社 | 高嵩密度粒状洗剤の製造方法 |
DE4125330A1 (de) † | 1991-07-31 | 1993-02-04 | Henkel Kgaa | Verfahren zur herstellung von zeolith-granulaten |
DE4414338A1 (de) † | 1994-04-25 | 1995-10-26 | Henkel Kgaa | Verfahren zur Herstellung von Builder-Granulaten |
DE19808757B4 (de) † | 1998-03-02 | 2007-09-20 | Henkel Kgaa | Duftperlen in Wasch- und Reinigungsmittelformkörpern |
DE19948671A1 (de) * | 1999-10-08 | 2001-04-19 | Cognis Deutschland Gmbh | Waschmittel |
DE19953503A1 (de) * | 1999-11-06 | 2001-05-10 | Henkel Kgaa | Verfahren zur Herstellung von Duftperlen |
-
2001
- 2001-01-08 GB GB0100412A patent/GB2370843A/en not_active Withdrawn
- 2001-12-24 DE DE60140821T patent/DE60140821D1/de not_active Expired - Lifetime
- 2001-12-24 WO PCT/GB2001/005769 patent/WO2002053697A1/en not_active Application Discontinuation
- 2001-12-24 EP EP01272727.7A patent/EP1349914B2/de not_active Expired - Lifetime
- 2001-12-24 ES ES01272727T patent/ES2337443T5/es not_active Expired - Lifetime
- 2001-12-24 AT AT01272727T patent/ATE452178T1/de not_active IP Right Cessation
Also Published As
Publication number | Publication date |
---|---|
EP1349914B2 (de) | 2013-09-04 |
ES2337443T3 (es) | 2010-04-26 |
EP1349914A1 (de) | 2003-10-08 |
DE60140821D1 (de) | 2010-01-28 |
ATE452178T1 (de) | 2010-01-15 |
GB2370843A (en) | 2002-07-10 |
GB0100412D0 (en) | 2001-02-21 |
ES2337443T5 (es) | 2013-11-18 |
WO2002053697A1 (en) | 2002-07-11 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CA2290504C (en) | Tablets, and process for making tablets | |
EP0523099B1 (de) | Verfahren zur herstellung von wasch- und reinigungsmitteln | |
CZ20012719A3 (cs) | Prací prostředek ve formě tablety | |
JPH05186800A (ja) | 洗剤組成物 | |
CA2350467A1 (en) | Detergent compositions | |
EP1349914B1 (de) | Verfahren zur herstellung von reinigungsmitteln | |
EA001705B1 (ru) | Способ получения композиций моющих средств с высокой насыпной плотностью | |
EP0877791B1 (de) | Verfahren zur herstellung von wasch- oder reinigungsmittelformkörpern | |
US7033988B2 (en) | Detergent tablets comprising solubility aids | |
JPS63112697A (ja) | 石鹸ヌードルを含む洗剤組成物 | |
CZ20011248A3 (cs) | Prací prostředek | |
MXPA01007832A (es) | Tableta detergente revestida. | |
WO2000046339A1 (en) | Coated detergent tablet | |
GB2376692A (en) | Fabric softening laundry tablet | |
CZ20004657A3 (cs) | Tableta vytvořená slisováním částicového materiálu a způsob její přípravy | |
EP1489160B1 (de) | Wasch- oder reinigungsaktive Formkörper für den Gebrauch im Haushalt | |
CN1375002A (zh) | 洗涤组合物 | |
EP1568762A1 (de) | Waschmitteltabletten und deren Herstellung | |
WO2003014286A1 (en) | Detergent compositions | |
EP1832648A1 (de) | Wäschewaschmittel und Verfahren | |
JP2002538269A (ja) | 洗剤錠剤の製造方法 | |
GB2342098A (en) | Detergent composition | |
MXPA01000373A (en) | Detergent tablet with high mechanical and dissolution characteristics | |
MXPA00008244A (en) | Process for preparing granular detergent compositions | |
JP2002520480A (ja) | 錠剤から粉末を生産するための方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
17P | Request for examination filed |
Effective date: 20030514 |
|
AK | Designated contracting states |
Kind code of ref document: A1 Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE TR |
|
AX | Request for extension of the european patent |
Extension state: AL LT LV MK RO SI |
|
17Q | First examination report despatched |
Effective date: 20050701 |
|
17Q | First examination report despatched |
Effective date: 20050701 |
|
RAP1 | Party data changed (applicant data changed or rights of an application transferred) |
Owner name: RECKITT BENCKISER N.V. |
|
GRAP | Despatch of communication of intention to grant a patent |
Free format text: ORIGINAL CODE: EPIDOSNIGR1 |
|
GRAS | Grant fee paid |
Free format text: ORIGINAL CODE: EPIDOSNIGR3 |
|
GRAA | (expected) grant |
Free format text: ORIGINAL CODE: 0009210 |
|
AK | Designated contracting states |
Kind code of ref document: B1 Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE TR |
|
REG | Reference to a national code |
Ref country code: GB Ref legal event code: FG4D |
|
REG | Reference to a national code |
Ref country code: CH Ref legal event code: EP |
|
REG | Reference to a national code |
Ref country code: IE Ref legal event code: FG4D |
|
REF | Corresponds to: |
Ref document number: 60140821 Country of ref document: DE Date of ref document: 20100128 Kind code of ref document: P |
|
REG | Reference to a national code |
Ref country code: NL Ref legal event code: VDEP Effective date: 20091216 |
|
REG | Reference to a national code |
Ref country code: ES Ref legal event code: FG2A Ref document number: 2337443 Country of ref document: ES Kind code of ref document: T3 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: SE Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20091216 Ref country code: FI Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20091216 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: AT Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20091216 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: MC Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20100701 Ref country code: PT Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20100416 Ref country code: NL Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20091216 |
|
REG | Reference to a national code |
Ref country code: CH Ref legal event code: PL |
|
PLBI | Opposition filed |
Free format text: ORIGINAL CODE: 0009260 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: BE Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20091216 |
|
26 | Opposition filed |
Opponent name: HENKEL AG & CO. KGAA Effective date: 20100809 |
|
PLAX | Notice of opposition and request to file observation + time limit sent |
Free format text: ORIGINAL CODE: EPIDOSNOBS2 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: CY Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20091216 Ref country code: GR Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20100317 Ref country code: IE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20091224 Ref country code: LI Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20091231 Ref country code: CH Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20091231 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: DK Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20091216 |
|
PLAF | Information modified related to communication of a notice of opposition and request to file observations + time limit |
Free format text: ORIGINAL CODE: EPIDOSCOBS2 |
|
PLBB | Reply of patent proprietor to notice(s) of opposition received |
Free format text: ORIGINAL CODE: EPIDOSNOBS3 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: LU Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20091224 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: TR Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20091216 |
|
PUAH | Patent maintained in amended form |
Free format text: ORIGINAL CODE: 0009272 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: PATENT MAINTAINED AS AMENDED |
|
27A | Patent maintained in amended form |
Effective date: 20130904 |
|
AK | Designated contracting states |
Kind code of ref document: B2 Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE TR |
|
REG | Reference to a national code |
Ref country code: DE Ref legal event code: R102 Ref document number: 60140821 Country of ref document: DE Effective date: 20130904 |
|
REG | Reference to a national code |
Ref country code: ES Ref legal event code: DC2A Ref document number: 2337443 Country of ref document: ES Kind code of ref document: T5 Effective date: 20131118 |
|
REG | Reference to a national code |
Ref country code: FR Ref legal event code: PLFP Year of fee payment: 15 |
|
REG | Reference to a national code |
Ref country code: FR Ref legal event code: PLFP Year of fee payment: 16 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: IT Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20151224 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: IT Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20151224 |
|
PGRI | Patent reinstated in contracting state [announced from national office to epo] |
Ref country code: IT Effective date: 20170710 |
|
REG | Reference to a national code |
Ref country code: FR Ref legal event code: PLFP Year of fee payment: 17 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: DE Payment date: 20181211 Year of fee payment: 18 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: GB Payment date: 20181227 Year of fee payment: 20 Ref country code: FR Payment date: 20181123 Year of fee payment: 18 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: IT Payment date: 20181220 Year of fee payment: 18 Ref country code: ES Payment date: 20190102 Year of fee payment: 18 |
|
REG | Reference to a national code |
Ref country code: DE Ref legal event code: R119 Ref document number: 60140821 Country of ref document: DE |
|
GBPC | Gb: european patent ceased through non-payment of renewal fee |
Effective date: 20191224 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: IT Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20191224 Ref country code: GB Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20191224 Ref country code: DE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20200701 Ref country code: FR Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20191231 |
|
REG | Reference to a national code |
Ref country code: ES Ref legal event code: FD2A Effective date: 20210524 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: ES Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20191225 |