EP1418224B1 - Procédé de fabrication d'une tablette détergente - Google Patents

Procédé de fabrication d'une tablette détergente Download PDF

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Publication number
EP1418224B1
EP1418224B1 EP02079186A EP02079186A EP1418224B1 EP 1418224 B1 EP1418224 B1 EP 1418224B1 EP 02079186 A EP02079186 A EP 02079186A EP 02079186 A EP02079186 A EP 02079186A EP 1418224 B1 EP1418224 B1 EP 1418224B1
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EP
European Patent Office
Prior art keywords
tablet
smooth
preferred
cutting
region
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
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EP02079186A
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German (de)
English (en)
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EP1418224A1 (fr
Inventor
Peter William Unilever R & D Vlaardingen APPEL
Clive E. Unilever R & D Vlaardingen MARSHMAN
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Unilever PLC
Unilever NV
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Unilever PLC
Unilever NV
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Priority to DE60208493T priority Critical patent/DE60208493T2/de
Priority to AT02079186T priority patent/ATE315077T1/de
Priority to EP02079186A priority patent/EP1418224B1/fr
Priority to ES02079186T priority patent/ES2254602T3/es
Publication of EP1418224A1 publication Critical patent/EP1418224A1/fr
Application granted granted Critical
Publication of EP1418224B1 publication Critical patent/EP1418224B1/fr
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    • 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

Definitions

  • This invention relates to cleaning compositions in the form of tablets for example, for use in fabric washing or machine dishwashing.
  • Detergent compositions in tablet form have advantages over powdered products in that they do not require measuring and are thus easier to handle and dispense into the washload.
  • Tablets of a cleaning composition are generally made by compressing or compacting a quantity of the composition in particulate form.
  • WO 01/42416 describes the production of multi-phase moulded bodies comprising a combination of core moulded bodies and a particulate premix.
  • WO 00/61717 describes a detergent tablet which is characterised in that at least part of its outer surface is smooth.
  • WO 00/04129 describes a multi-phase detergent tablet comprising a first phase in the form of a shaped body having at least one mould therein and a second phase in the form of a particulate solid compressed within said mould.
  • a further objective of the present invention is to.provide a method to produce a smooth tablet or phase thereof wherein the choice of materials and the manufacturing method allows the low cost production of tablets of good performance and of good consistency and texture.
  • a cleaning tablet which has a plurality of discrete regions with differing compositions, characterised in that at least one first region of the tablet is a smooth region and at least one second region of the tablet is a solid region of compacted particulate material.
  • One method of producing smooth phases which can be used in cleaning tablets is first to produce a large quantity e.g. an extruded strand or a log of the material, followed by partitioning this quantity into smaller quantities for example by cutting.
  • the smooth composition can advantageously be divided into smooth parts for use in cleaning tablets by using a high frequency or jet cutting process.
  • the invention relates to a method of producing a cleaning tablet comprising a smooth phase wherein the preparation of the smooth phase comprises the step of high-frequency cutting or jet cutting of a cleaning material.
  • the cleaning material comprises from 10 to 90 wt% of non-soap surfactants and from 0 to 20 wt% of water.
  • tablets (and the smooth phases) of the invention are of cylindrical shape wherein the two main surfaces (upper side and bottom side) are substantially flat.
  • the smooth phases are slices of cleaning material, for example having a diameter of from 1 to 10 cm (preferably 2 to 6 cm) and a height of from 0.1 to 5 cm (preferably 0.3 to 1.5 cm).
  • tablets of the invention can be single phase tablets, which are predominantly constituted by the smooth phase as described above.
  • a preferred embodiment of the invention relates to a multiphase tablet wherein the smooth phase is present and additionally one or more other phases are present.
  • these additional phases can be smooth or solid.
  • Particularly suitable are solid phases composed of compacted particulate solids.
  • the regions of a multi-phase tablet are possibly separate layers within a tablet. However, a discrete region of a tablet could also have other forms for example one or more core(s) or insert(s).
  • the first region is a smooth layer and the second region is a layer of compacted particulate material.
  • the first region is a core or insert of smooth material embedded in the second region which is a layer of compacted particulate material.
  • the weight of this tablet will be from 5 to 200 g, more preferably from 10 to 100 g, most preferably from 15 to 50 g.
  • the smooth phase is present as a distinctive region preferably having a weight of from 2 to 20 grammes, more preferred from 3 to 10 grammes.
  • the other phases together have a weight of 10 to 50 grammes, more preferred 15 to 40 grammes.
  • smooth phase refers to compositions which are on the one hand solid enough to retain their shape at ambient temperature and on the other hand smooth in appearance. Smooth textures are generally of low or no porosity and have -at normal viewing distance- the appearance of a continuous phase for example as opposed to porous and particulate appearance of a compacted particulate material.
  • the smooth phase is transparent or translucent.
  • this means that the composition has an optical transmissivity of at least 10%, most preferably 20%, still more preferably 30%, through a path length of 0.5 cm at 25° C.
  • These measurements may be obtained using a Perkin Elmer UV/VIS Spectrometer Lambda 12 or a Brinkman PC801 Colorimeter at a wavelength of 520nm, using water as the 100% standard.
  • compositions according to the invention does not preclude the composition being coloured, e.g. by addition of a dye, provided that it does not detract substantially from clarity.
  • the smooth phase comprises from 20-80 wt% of non-soap surfactants (based on the total weight of said smooth phase), more preferred from 25 to 75 wt%, most preferred 30 to 70 wt%. It has been found that the combination of a separate smooth first region and these high surfactant levels provide very good dispersing and cleaning properties to the tablet.
  • the non-soap surfactants in the first region comprise a combination of anionic surfactants and non-ionic surfactants in a weight ratio of from 5 : 1 to 1 : 5, more preferred 3 : 1 to 1 : 3, more preferred 2 : 1 to 1: 2.
  • Further surfactants for example cationic surfactants may equally be present for example at a level of 0.1 to 10 wt% based on the weight of the smooth part.
  • the smooth region may comprise additional solid materials such as mineral salts, sugar or structuring soaps for example at a level of 2 to 90 wt% based on the weight of the smooth part, more preferred from 3 to 70 wt%, most preferred 5 to 40 wt%.
  • suitable salts are for example soluble salts such as acetate, citrate, urea. The use of these materials can advantageously lead to improved structuring and/or improved dissolution properties of the smooth phase.
  • the smooth region of the tablet may also contain diluent materials for example polyethyleneglycol, dipropyleneglycol, isopropanol or (mono-)propyleneglycol.
  • diluent materials for example polyethyleneglycol, dipropyleneglycol, isopropanol or (mono-)propyleneglycol.
  • the level of these diluents is from 0 to 40 wt%, more preferred 1 to 20, most preferred from 4 to 15 wt% based on the weight of the smooth phase.
  • the smooth phase comprises no or only low levels of water.
  • the level of water is less than 20 wt % based on the weight of the smooth phase, more preferred less than 15 wt%, most preferred from 5 to 12 wt%.
  • the smooth phases are substantially free from water, which means that apart from low levels of moisture (e.g. for neutralisation or as crystal water) no additional added water is present.
  • the total weight of surfactants in the smooth phase is from 2 to 20 grammes, more preferred from 3 to 10 grammes.
  • the smooth phase comprises no or only low levels of ingredients such as builders, bleach activators and bleach materials.
  • the level of these ingredients in the smooth phase is less than 5 wt%.
  • the tablet may be a multi-phase tablet wherein the phases other than the smooth phase as described above comprise no or only low levels of surfactants.
  • the level of surfactants in the other phases is less than 10 wt%(based on the total weight of said phases), more preferred from 0 to 9 wt%, most preferred from 1 to 8 wt%.
  • the cleaning tablets comprise a first smooth region (as described above) in combination with a second region of the tablet which is a solid region, for example prepared by compression of a particulate composition.
  • the second region may comprise surfactant materials
  • this region preferably comprises ingredients of the tablet other than surfactants.
  • these ingredients are for example builders, bleach system, enzymes etc.
  • the builders in the tablet are predominantly present in the second region.
  • the bleach system is predominantly present in the second region.
  • the enzymes are predominantly present in the second region.
  • the term "predominantly present” refers to a situation wherein at least 90 wt% of an ingredient is present in the second region, more preferred more than 98 wt%, most preferred substantially 100 wt%.
  • each of the regions may be composed of a limited number of discrete regions.
  • the first smooth region may be a single discrete part of the tablet but may also be a limited number (say 1-5) discrete smooth parts.
  • each of these smooth parts are at least 1 gramme, also preferably each of these smooth parts is substantially of the same composition. If reference is made to the composition or weight of the first region it is understood that this concerns the total weight and composition of these smooth parts.
  • the solid second region may be composed of a limited number (say 1-5) of solid parts e.g. separate layers in the tablet.
  • each of these parts has a weight of at least 10 grammes, also preferably each of the solid parts is substantially of the same composition. If reference is made to the composition or weight of the second region it is understood that this concerns the total weight and composition of these solid parts.
  • the cleaning tablets of the invention may optionally comprise further regions, for example the tablet may be partly or wholly coated.
  • Cleaning tablets according to the invention are preferably manufactured by firstly preparing a smooth part.
  • the preparation of the smooth phase may include the heating of the cleaning material followed by cooling.
  • the preparation of the cleaning material may involve extrusion.
  • Extrusion processes for washing articles are known, for example WO 01/02532 describes the extrusion of washing articles with a pressure of less than 10 bar.
  • extrusion processes will involve the forming of an extrudable mass which is then subsequently extruded from an extrusion device and optionally then partitioned into parts of the desired size and weight.
  • the smooth parts may then be hardened.
  • the partitioning involves a high frequency cutting or jet cutting process.
  • high frequency cutting processes are ultrasonic cutting and focused energy cutting for example by using focused laser light or ultrasound.
  • jet cutting are air or water jet cutting.
  • Ultrasonic cutting devices are for example described in EP 783 399 and US 6070509 and generally involve an oscillating cutting device e.g. a vibrating knife. Ultrasonic cutting machines may for example operate at oscillating frequencies of between 10 and 50 kHz, more preferred 20 to 40 kHz.
  • Focused energy cutting generally uses focussed beams of high frequency radiation such as ultrasound or light (e.g. laser light such as for example from a CO 2 laser). Examples of laser devices for cutting are described in WO 00/48764, EP1083019 and WO 01/38242.
  • Jet cutting processes involve the focused application of flows of liquid of gases for example air or other gases such as CO 2 or nitrogen or liquids such as for example water or propylene glycol.
  • the pressure of the flow will be from 6.9 ⁇ 10 4 to 6.9 ⁇ 10 5 kPa (10000 to 100000 psi), more preferred 1.38 ⁇ 10 5 to 5.52 ⁇ 10 5 kPa (20000 to 80000 psi), most preferred from 2.07 ⁇ 10 5 to 3.45 ⁇ 10 5 kPa (30000 t0 50000 psi) (1 psi corresponds to 6.9 kPa).
  • the diameter of the flow jets is from 0.025 mm to 0.25 mm, more preferred from 0.08 to 0.20 mm, most preferred from 0.1 to 0.15 mm.
  • liquid cutting devices are for example described in WO00/69290 and US4640300.
  • gas cutting devices are described in US 4471895.
  • air or steam is used as the cutting gas it is used a elevated temperature of from 50 to 500°C, more preferred from 60 to 250 °C.
  • the extrudable mass preferably has before extrusion an initial elevated temperature for example from 60 to 120°C, more preferred from 70 to 90°C.
  • the extrudable mass is during the production of the smooth mass cooled e.g. to a final temperature of 20°C and then extruded. If extrusion is used this low temperature may for example be the temperature at the extrusion die for example from 10 to 40, preferably from 15 to 25, most preferred at ambient temperature (20°C).
  • step (a) takes place before step (b).
  • the particulate composition is pre-compressed at a force of 0.1 to 20 kN/cm 2 between steps (a) and (b) In another preferred embodiment the particulate composition is flattened between steps (a) and (b).
  • the (co-)compression of the combination of the smooth and the solid region(s) takes place at a force of from 0.05 to 20 kN/cm 2 .
  • the co-compression in step (c) can advantageously be at a force of 0.1- 10 kN/cm 2 , more preferred 0.5 to 5 kN/cm 2 .
  • the co-compression preferably takes place at a force of 1- 100 kN/cm 2 , more preferred 2-50 kN/cm 2 ., most preferred 2-10 kN/cm 2 .
  • One advantage of the method of the present invention is that the co-compression step of (c) leads to good adherence of the first region to the second region and avoids the need of applying an adhesive material between the smooth and solid region.
  • Another advantage of the method of the invention is that it can be carried out in a normal tablet press without the need of adaptation of the shape of the pressing surfaces.
  • a tablet of this invention may be intended for use in machine dishwashing.
  • Such a tablet is likely to contain surfactant in a low concentration such as 0.5 to 2 wt% based on the whole tablet, although higher concentrations ranging up to 10 wt% may be used.
  • Such will typically contain salts, such as over 60 wt%, often over 85 wt% of the tablet.
  • Water soluble salts typically used in machine dishwashing compositions are phosphates (including condensed phosphates) carbonates and silicates, generally as alkali metal salts.
  • Water soluble alkali metal salts selected from phosphates, carbonates and silicates may provide 60 wt% or more of a dishwashing composition.
  • a tablet of this invention will be intended for fabric washing.
  • the tablet will be likely to contain at least 2 wt%, probably at least 5 wt%, up to 40 or 50 wt% non-soap surfactant based on the whole tablet, and from 5 to 80 wt% detergency builder, based on the whole tablet.
  • compositions which are used in tablets of the invention will contain one or more detergent surfactants.
  • these preferably provide from 5 to 50% by weight of the overall tablet composition, more preferably from 8 or 9% by weight of the overall composition up to 40% or 50% by weight.
  • Surfactant may be anionic (soap or non-soap), cationic, zwitterionic, amphoteric, nonionic or a combination of these.
  • Anionic surfactant may be present in an amount from 0.5 to 50% by weight, preferably from 2% or 4% up to 30% or 40% by weight of the tablet composition.
  • Synthetic (i.e. non-soap) anionic surfactants are well known to those skilled in the art.
  • alkylbenzene sulphonates particularly sodium linear alkylbenzene sulphonates having an alkyl chain length of C 8 -C 15 ; olefin sulphonates; alkane sulphonates; dialkyl sulphosuccinates; and fatty acid ester sulphonates.
  • Primary alkyl sulphate having the formula ROSO 3 - M + in which R is an alkyl or alkenyl chain of 8 to 18 carbon atoms especially 10 to 14 carbon atoms and M + is a solubilising cation, is commercially significant as an anionic surfactant.
  • Linear alkyl benzene sulphonate of the formula where R is linear alkyl of 8 to 15 carbon atoms and M + is a solubilising cation, especially sodium, is also a commercially significant anionic surfactant.
  • such linear alkyl benzene sulphonate or primary alkyl sulphate of the formula above, or a mixture thereof will be the desired anionic surfactant and may provide 75 to 100 wt% of any anionic non-soap surfactant in the composition.
  • the amount of non-soap anionic surfactant lies in a range from 5 to 20 wt% of the tablet composition.
  • Soaps for use in accordance to the invention are preferably sodium soaps derived from naturally occurring fatty acids, for example, the fatty acids from beef tallow.
  • Suitable nonionic surfactant compounds which may be used include in particular the reaction products of compounds having a hydrophobic group and a reactive hydrogen atom, for example, aliphatic alcohols, acids, amides or alkyl phenols with alkylene oxides, especially ethylene oxide.
  • Nonionic surfactant compounds are alkyl (C 8-22 ) phenol-ethylene oxide condensates, the condensation products of linear or branched aliphatic C 8-20 primary or secondary alcohols with ethylene oxide, and products made by condensation of ethylene oxide with the reaction products of propylene oxide and ethylene-diamine.
  • the primary and secondary alcohol ethoxylates especially the C 9-11 and C 12-15 primary and secondary alcohols ethoxylated with an average of from 5 to 20 moles of ethylene oxide per mole of alcohol.
  • the amount of nonionic surfactant lies in a range from 4 to 40%, better 4 or 5 to 30% by weight of the whole tablet.
  • nonionic surfactants are liquids. These may be absorbed onto particles of the composition.
  • the surfactant may be wholly nonionic, in an amount below 5 wt% of the whole tablet although it is known to include some anionic surfactant and to use up to 10 wt% surfactant in total.
  • a composition which is used in tablets of the invention will usually contain from 5 to 80%, more usually 15 to 60% by weight of detergency builder. This may be provided wholly by water soluble materials, or may be provided in large part or even entirely by water-insoluble material with water-softening properties. Water-insoluble detergency builder may be present as 5 to 80 wt%, better 5 to 60 wt% of the composition.
  • Alkali metal aluminosilicates are strongly favoured as environmentally acceptable water-insoluble builders for fabric washing.
  • Alkali metal (preferably sodium) aluminosilicates may be either crystalline or amorphous or mixtures thereof, having the general formula: 0.8 - 1.5 Na 2 O.Al 2 O 3 . 0.8 - 6 SiO 2 . xH 2 O
  • xH2O xH2O
  • xH2O calcium ion exchange capacity
  • the preferred sodium aluminosilicates contain 1.5-3.5 SiO 2 units (in the formula above). Both the amorphous and the crystalline materials can be prepared readily by reaction between sodium silicate and sodium aluminate, as amply described in the literature.
  • Suitable crystalline sodium aluminosilicate ion-exchange detergency builders are described, for example, in GB 1429143 (Procter & Gamble).
  • the preferred sodium aluminosilicates of this type are the well known commercially available zeolites A and X, the novel zeolite P described and claimed in EP 384070 (Unilever) and mixtures thereof.
  • a water-insoluble detergency builder could be a layered sodium silicate as described in US 4664839.
  • NaSKS-6 is the trademark for a crystalline layered silicate marketed by Hoechst (commonly abbreviated as "SKS-6").
  • KSKS-6 has the delta-Na 2 SiO 5 morphology form of layered silicate. It can be prepared by methods such as described in DE-A-3,417,649 and DE-A-3,742,043.
  • layered silicates such as those having the general formula NaMSi x O 2x+1 .yH 2 O wherein M is sodium or hydrogen, x is a number from 1.9 to 4, preferably 2, and y is a number from 0 to 20, preferably 0 can be used.
  • Water-soluble phosphorous-containing inorganic detergency builders include the alkali-metal orthophosphates, metaphosphates, pyrophosphates and polyphosphates.
  • Specific examples of inorganic phosphate builders include sodium and potassium tripolyphosphates, orthophosphates and hexametaphosphates.
  • Non-phosphorous water-soluble builders may be organic or inorganic.
  • Inorganic builders that may be present include alkali metal (generally sodium) carbonate; while organic builders include polycarboxylate polymers, such as polyacrylates, acrylic/maleic copolymers, and acrylic phosphonates, monomeric polycarboxylates such as citrates, gluconates, oxydisuccinates, glycerol mono- di- and trisuccinates, carboxymethyloxysuccinates, carboxymethyloxymalonates, dipicolinates and hydroxyethyliminodiacetates.
  • alkali metal generally sodium
  • organic builders include polycarboxylate polymers, such as polyacrylates, acrylic/maleic copolymers, and acrylic phosphonates, monomeric polycarboxylates such as citrates, gluconates, oxydisuccinates, glycerol mono- di- and trisuccinates, carboxymethyloxysuccinates, carboxymethyloxymalonates, dip
  • At least one region (preferably the second region) of a fabric washing tablet preferably include polycarboxylate polymers, more especially polyacrylates and acrylic/maleic copolymers which can function as builders and also inhibit unwanted deposition onto fabric from the wash liquor.
  • Tablets according to the invention may contain a bleach system in at least one region of a tablet, preferably in the second region.
  • This preferably comprises one or more peroxy bleach compounds, for example, inorganic persalts or organic peroxyacids, which may be employed in conjunction with activators to improve bleaching action at low wash temperatures. If any peroxygen compound is present, the amount is likely to lie in a range from 10 to 25% by weight of the composition.
  • Preferred inorganic persalts are sodium perborate monohydrate and tetrahydrate, and sodium percarbonate, advantageously employed together with an activator.
  • Bleach activators also referred to as bleach precursors
  • Preferred examples include peracetic acid precursors, for example, tetraacetylethylene diamine (TAED), now in widespread commercial use in conjunction with sodium perborate; and perbenzoic acid precursors.
  • TAED tetraacetylethylene diamine
  • perbenzoic acid precursors perbenzoic acid precursors.
  • the quaternary ammonium and phosphonium bleach activators disclosed in US 4751015 and US 4818426 are also of interest.
  • bleach activator which may be used, but which is not a bleach precursor, is a transition metal catalyst as disclosed in EP-A-458397, EP-A-458398 and EP-A-549272.
  • a bleach system may also include a bleach stabiliser (heavy metal sequestrant) such as ethylenediamine tetramethylene phosphonate and diethylenetriamine pentamethylene phosphonate.
  • a bleach is present and is a water-soluble inorganic peroxygen bleach, the amount may well be from 10% to 25% by weight of the composition.
  • the detergent tablets of the invention may also contain (preferably in the second region) one of the detergency enzymes well known in the art for their ability to degrade and aid in the removal of various soils and stains.
  • Suitable enzymes include the various proteases, cellulases, lipases, amylases, and mixtures thereof, which are designed to remove a variety of soils and stains from fabrics.
  • suitable proteases are Maxatase (Trade Mark), as supplied by Gist-Brocades N.V., Delft, Holland, and Alcalase (Trade Mark), and Savinase (Trade Mark), as supplied by Novo Industri A/S, Copenhagen, Denmark.
  • Detergency enzymes are commonly employed in the form of granules or marumes, optionally with a protective coating, in amount of from about 0.1% to about 3.0% by weight of the composition; and these granules or marumes present no problems with respect to compaction to form a tablet.
  • the detergent tablets of the invention may also contain (preferably in the second region) a fluorescer (optical brightener), for example, Tinopal (Trade Mark) DMS or Tinopal CBS available from Ciba-Geigy AG, Basel, Switzerland.
  • a fluorescer optical brightener
  • Tinopal DMS is disodium 4,4'bis-(2-morpholino-4-anilino-s-triazin-6-ylamino) stilbene disulphonate
  • Tinopal CBS is disodium 2,2'-bis-(phenyl-styryl) disulphonate.
  • An antifoam material is advantageously included (preferably in the second region), especially if a detergent tablet is primarily intended for use in front-loading drum-type automatic washing machines.
  • Suitable antifoam materials are usually in granular form, such as those described in EP 266863A (Unilever).
  • Such antifoam granules typically comprise a mixture of silicone oil, petroleum jelly, hydrophobic silica and alkyl phosphate as antifoam active material, absorbed onto a porous absorbed water-soluble carbonate-based inorganic carrier material.
  • Antifoam granules may be present in an amount up to 5% by weight of the composition.
  • a detergent tablet of the invention includes an amount of an alkali metal silicate, particularly sodium ortho-, meta- or disilicate.
  • an alkali metal silicate particularly sodium ortho-, meta- or disilicate.
  • the presence of such alkali metal silicates at levels, for example, of 0.1 to 10 wt%, may be advantageous in providing protection against the corrosion of metal parts in washing machines, besides providing some measure of building and giving processing benefits in manufacture of the particulate material which is compacted into tablets.
  • a tablet for fabric washing will generally not contain more than 15 wt% silicate.
  • a tablet for machine dishwashing will often contain more than 20 wt% silicate.
  • the silicate is present in the second region of the tablet.
  • ingredients which can optionally be employed in a region of a fabric washing detergent of the invention tablet include anti-redeposition agents such as sodium carboxymethylcellulose, straight-chain polyvinyl pyrrolidone and the cellulose ethers such as methyl cellulose and ethyl hydroxyethyl cellulose, fabric-softening agents; heavy metal sequestrants such as EDTA; perfumes; and colorants or coloured speckles.
  • anti-redeposition agents such as sodium carboxymethylcellulose, straight-chain polyvinyl pyrrolidone and the cellulose ethers such as methyl cellulose and ethyl hydroxyethyl cellulose, fabric-softening agents
  • heavy metal sequestrants such as EDTA
  • perfumes and colorants or coloured speckles.
  • dispersing aids are water-swellable polymers (e.g. SCMC) highly soluble materials (e.g. sodium citrate, potassium carbonate or sodium acetate) or sodium tripolyphospate with preferably at least 40% of the anhydrous phase I form.
  • SCMC water-swellable polymers
  • highly soluble materials e.g. sodium citrate, potassium carbonate or sodium acetate
  • sodium tripolyphospate preferably at least 40% of the anhydrous phase I form.
  • the second region of a detergent tablet of this invention is a preferably a matrix of compacted particles.
  • the particulate composition has an average particle size in the range from 200 to 2000 ⁇ m, more preferably from 250 to 1400 ⁇ m. Fine particles, smaller than 180 ⁇ m or 200 ⁇ m may be eliminated by sieving before tableting, if desired, although we have observed that this is not always essential.
  • the starting particulate composition may in principle have any bulk density
  • the present invention is especially relevant to tablets made by compacting powders of relatively high bulk density, because of their greater tendency to exhibit disintegration and dispersion problems.
  • Such tablets have the advantage that, as compared with a tablet derived from a low bulk density powder, a given dose of composition can be presented as a smaller tablet.
  • the starting particulate composition may suitably have a bulk density of at least 400 g/l, preferably at least 500 g/l, and perhaps at least 600 g/l.
  • Tableting machinery able to carry out the manufacture of tablets of the invention is known, for example suitable tablet presses are available from Fette and from Korch.
  • Tableting may be carried out at ambient temperature or at a temperature above ambient which may allow adequate strength to be achieved with less applied pressure during compaction.
  • the particulate composition is preferably supplied to the tableting machinery at an elevated temperature. This will of course supply heat to the tableting machinery, but the machinery may be heated in some other way also.
  • the size of a tablet will suitably range from 10 to 160 grams, preferably from 15 to 60 g, depending on the conditions of intended use, and whether it represents a dose for an average load in a fabric washing or dishwashing machine or a fractional part of such a dose.
  • the tablets may be of any shape. However, for ease of packaging they are preferably blocks of substantially uniform cross-section, such as cylinders or cuboids.
  • the overall density of a tablet preferably lies in a range from 1040 or 1050g/l up to 1600g/l.
  • the mixture was pumped into a sequence of 2 stainless steel tubes by a Maag Sinox P7 pump or a piston pump, type SIBa HK 05016SST4000M000 ex Prominent, Vleuten (NL). Both tubes were double jacketed.
  • the first tube was 2.5m long and had an inner diameter of 73mm.
  • the second tube was 1.5m long and had an inner diameter of 45mm.
  • the tubes were connected by a 10cm long pipe.
  • the mixture was pumped into the tubes at a temperature of 85°C at a throughput of 4 kg/hr.
  • the first tube was cooled using a water bath at 40°C.
  • the second tube was cooled using a 50:50 weight mixture of ethylene glycol and water.
  • the coolant temperature was -15°C.
  • the material coming out of the second tube had a temperature of about 20°C and was collected and divided into bars of around 0.5m.
  • the bars can for example be cut into slices of 5 grammes each by using a laser cutting device (CO 2 laser) an acoustic knife (oscillating at 25kHz) a water jet (operating at 25000 psi and with a diameter of 0.1 mm).
  • a laser cutting device CO 2 laser
  • an acoustic knife oscillating at 25kHz
  • a water jet operating at 25000 psi and with a diameter of 0.1 mm.
  • a detergent powder was made of the following composition by pregranulating the granule ingredients, followed by post-dosing the rest of the ingredients Ingredient Parts by weight Granules Na-las 1.1 Nonionic 7EO 0.5 C12 soap 0.1 NaAc.3aq 0.3 Zeolite A24 2.4 Light soda ash 0.4 Moisture/minors 0.4 Post-dose EAG (17% silicone) 3.0 Fluorescer (15%) 2.2 STP 62.4 Na-disilicate (80%) 3.8 TAED (83%) 4.3 Percarbonate 16.9 Dequest 2047 1.9 Minors/ enzymes/colour to 100
  • the tablets were made in 2 different ways:

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  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Detergent Compositions (AREA)

Claims (10)

  1. Procédé de production d'une pastille détergente comprenant une phase lisse, dans lequel la préparation de la phase lisse comprend l'étape de découpe à haute fréquence ou de découpe au jet d'un matériau détergent.
  2. Procédé selon la revendication 1, dans lequel le matériau détergent comprend de 10 à 90 % en poids de tensioactifs non savonneux et de 0 à 20 % en poids d'eau.
  3. Procédé selon la revendication 1, dans lequel la pastille détergente est une pastille lisse monophase ayant un poids de 5 à 200 grammes, de préférence de 10 à 100 grammes, mieux encore de 15 à 35 grammes.
  4. Procédé selon la revendication 1, dans lequel la pastille détergente est une pastille multiphases comprenant la phase lisse en tant qu'une région distincte ayant un poids de 2 à 20 grammes, mieux de 3 à 10 grammes.
  5. Procédé selon la revendication 1, dans lequel les processus de découpe à haute fréquence sont sélectionnés parmi la découpe aux ultrasons et la découpe par énergie focalisée.
  6. Procédé selon la revendication 5, dans lequel l'appareil de découpe aux ultrasons fonctionne à des fréquences entre 10 et 50 kHz, mieux de 20 à 40 kHz.
  7. Procédé selon la revendication 5, dans lequel la découpe par énergie focalisée utilise des faisceaux focalisés d'ultrasons ou de lumière, de préférence de lumière laser.
  8. Procédé selon la revendication 1, dans lequel la découpe au jet met en oeuvre l'application focalisée de flux de liquides, tels que par exemple de l'eau ou du propylène glycol.
  9. Procédé selon la revendication 1, dans lequel la découpe au jet met en oeuvre l'application focalisée de flux de gaz, tels que par exemple de l'air, de la vapeur ou de l'azote.
  10. Procédé selon la revendication 8 ou 9, dans lequel la pression du flux est de 6,9 . 104 à 6,9 . 105 kPa (10000 à 100000 psi), de préférence de 1,38 . 105 à 5,52 . 105 kPa (20000 à 80000 psi), mieux encore de 2,07 . 105 à 3,45 . 105 kPa (30000 à 50000 psi), et le diamètre des flux est de 0,025 mm à 0,25 mm, de préférence de 0,08 à 0,20 mm, mieux encore de 0,1 à 0,15 mm.
EP02079186A 2002-10-09 2002-10-09 Procédé de fabrication d'une tablette détergente Expired - Lifetime EP1418224B1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
DE60208493T DE60208493T2 (de) 2002-10-09 2002-10-09 Verfahren zur Herstellung einer Reinigungsmitteltablette
AT02079186T ATE315077T1 (de) 2002-10-09 2002-10-09 Verfahren zur herstellung einer reinigungsmitteltablette
EP02079186A EP1418224B1 (fr) 2002-10-09 2002-10-09 Procédé de fabrication d'une tablette détergente
ES02079186T ES2254602T3 (es) 2002-10-09 2002-10-09 Procedimiento de produccion de una pastilla de limpieza.

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP02079186A EP1418224B1 (fr) 2002-10-09 2002-10-09 Procédé de fabrication d'une tablette détergente

Publications (2)

Publication Number Publication Date
EP1418224A1 EP1418224A1 (fr) 2004-05-12
EP1418224B1 true EP1418224B1 (fr) 2006-01-04

Family

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EP02079186A Expired - Lifetime EP1418224B1 (fr) 2002-10-09 2002-10-09 Procédé de fabrication d'une tablette détergente

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EP (1) EP1418224B1 (fr)
AT (1) ATE315077T1 (fr)
DE (1) DE60208493T2 (fr)
ES (1) ES2254602T3 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014079690A1 (fr) * 2012-11-23 2014-05-30 Unilever N.V. Procédé de découpe d'articles cosmétiques à l'aide d'un fluide sous pression

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1669438B1 (fr) 2004-12-08 2007-10-17 Unilever N.V. Comprimé détergent
DE602005014328D1 (de) 2005-01-04 2009-06-18 Unilever Nv Wasch- und Reinigungsmittelformkörper
EP1705240A1 (fr) 2005-03-23 2006-09-27 Unilever N.V. Tablettes détergentes
DE602006002151D1 (de) 2005-03-23 2008-09-25 Unilever Nv Körperförmige Wasch- oder Reinigungsmittelzusammensetzungen
EP1746152A1 (fr) 2005-07-20 2007-01-24 Unilever N.V. Compositions détergentes
EP1746151A1 (fr) 2005-07-20 2007-01-24 Unilever N.V. Pastilles de composition détergente
DE102010051226A1 (de) 2010-11-12 2012-05-31 Dental Care Innovation Gmbh Ausspültablete mit abrasiven Bestandteilen
US10626350B2 (en) 2015-12-08 2020-04-21 Ecolab Usa Inc. Pressed manual dish detergent
JP2020505431A (ja) 2017-02-02 2020-02-20 ウォーター ピック インコーポレイテッド 歯牙清掃用研磨剤を含む錠剤

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Publication number Priority date Publication date Assignee Title
US4011170A (en) * 1974-07-10 1977-03-08 John Harlan Pickin Marbled detergent bars
GB9124762D0 (en) * 1991-11-21 1992-01-15 Unilever Plc Food cutting process
US5225098A (en) * 1992-03-20 1993-07-06 The Procter & Gamble Company Neutral pH freezer bar and process
DE69830334T2 (de) * 1997-11-26 2006-02-02 The Procter & Gamble Company, Cincinnati Waschmitteltablette
ES2227900T3 (es) * 1997-11-26 2005-04-01 THE PROCTER & GAMBLE COMPANY Procedimiento para fabricar una pastilla detergente.

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014079690A1 (fr) * 2012-11-23 2014-05-30 Unilever N.V. Procédé de découpe d'articles cosmétiques à l'aide d'un fluide sous pression

Also Published As

Publication number Publication date
DE60208493T2 (de) 2006-07-06
ATE315077T1 (de) 2006-02-15
ES2254602T3 (es) 2006-06-16
EP1418224A1 (fr) 2004-05-12
DE60208493D1 (de) 2006-03-30

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