EP0871698B1 - Procede de production de detergents sous forme de comprimes resistant a la rupture - Google Patents

Procede de production de detergents sous forme de comprimes resistant a la rupture Download PDF

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Publication number
EP0871698B1
EP0871698B1 EP96901299A EP96901299A EP0871698B1 EP 0871698 B1 EP0871698 B1 EP 0871698B1 EP 96901299 A EP96901299 A EP 96901299A EP 96901299 A EP96901299 A EP 96901299A EP 0871698 B1 EP0871698 B1 EP 0871698B1
Authority
EP
European Patent Office
Prior art keywords
weight
tablets
alkali metal
optionally
water
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
Application number
EP96901299A
Other languages
German (de)
English (en)
Other versions
EP0871698A1 (fr
Inventor
Hans Kruse
Volker Bauer
Horst Prühs
Hans Janke
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Henkel AG and Co KGaA
Original Assignee
Henkel AG and Co KGaA
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Henkel AG and Co KGaA filed Critical Henkel AG and Co KGaA
Publication of EP0871698A1 publication Critical patent/EP0871698A1/fr
Application granted granted Critical
Publication of EP0871698B1 publication Critical patent/EP0871698B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C11D3/06—Phosphates, including polyphosphates
    • 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
    • C11D17/0091—Dishwashing tablets
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C11D3/08—Silicates

Definitions

  • the present invention relates to a method for producing break-resistant Detergent tablets, in particular for use in mechanical Dishwashing, both in the commercial and household sectors.
  • Powder, granule or tablet detergents for dishes in dishwashers consist essentially of sodium tripolyphosphate, Alkali silicate, usually alkali metasilicate, and possibly from a low-foaming, nonionic surfactant and bleaching agents, namely active chlorine releasing compounds, but preferably those in aqueous solution Release active oxygen. Above all, they serve to facilitate the Removal of stains from tea, coffee or fruit juices.
  • the known agents are generally prepared by customary methods Manufacturing processes such as mixing or granulating and / or others Pressing.
  • disk-like tablets have been produced from simple mixtures of the known detergent constituents with the addition of a tabletting aid, not specified, and using a compression pressure of about 70 to 1000 kg / cm 2 (7 to 100 MPa).
  • Tablets of the type mentioned above are also described in German Offenlegungsschrift 28 57 001. They are also produced by pressing the mere mixtures of the components using appropriate pressures.
  • Lubricants, lubricants and disintegrants such as insoluble stearate salts, fatty acids, fatty alcohols, starch, polyethylene glycol, Aerosil (R) , colloidal silica, alginates, Veegum (R) , sugar, gelatin and zeolites are mentioned as tableting aids.
  • the present invention therefore relates to a process for the preparation of unbreakable, alkaline detergent tablets suitable for use in dishwashers from pentaalkali metal triphosphate, alkali silicates, which may optionally contain water of crystallization, and, if appropriate, alkali metal carbonates, bleaching agents, foam inhibitors and / or enzymes and nonionic surfactants, which is characterized in that that 15-60, preferably 25-50% by weight of pentaalkali metal phosphate in a proportion of 20-100% by weight, preferably 35-80% by weight, and in particular 40-60% by weight of phase I, 35-80, preferably 40-55% by weight of alkali metal silicate, optionally containing water of crystallization, calculated as Na 2 SiO 3 , and optionally up to 20% by weight of sodium carbonate, up to 18, preferably 1-10% by weight of a bleaching agent, up to 3, preferably 1 to 2% by weight of paraffin oil and / or up to 3% by weight of a low-foaming
  • phase 1 tripolyphosphates can be used successfully in tabletting processes in the detergent and cleaning agent sector.
  • Detergent tablets are known from US Pat. No. 3,417,024 (1968), which depending on the desired degree of decay tripolyphosphate of phase I or May contain phase II.
  • Alkali metasilicate is used in amounts of 35-80, preferably 40-55% by weight, calculated as Na 2 SiO 3 , predominantly in crystalline-free, slightly granulated form with residual water contents of up to 5% by weight, preferably 3 ⁇ 1% by weight. -% used. About 3 - 15, preferably 4 - 12 wt .-%, calculated as an anhydrous compound, can be used in the form of its penta- and / or nonahydrate. The solubility of the tablets can thus be controlled as desired. Sodium metasilicate pentahydrate is preferred because of its higher alkalinity. Metasilicates containing water of crystallization alone would dilute the active substance content of the tablets too much.
  • sodium carbonate because of the better decay properties the tablets are preferably in compacted form, as is commercially available is used.
  • the amount of the optional addition of cleaning-enhancing nonionic, preferably low-foaming surfactants is up to 3% by weight, preferably 0.5 - 2.5 wt .-%, otherwise when using the tablets in the dishwashers in connection with the soiling of the dishes unwanted foaming can occur by adding a foam inhibitor would require.
  • the known low-foaming nonionic surfactants are suitable Ethoxylation products of long chain alcohols and alkylphenols, where To reduce the tendency to foam, the free hydroxyl group of the polyethylene glycol ether residue by ether or acetal groups or by polypropylene glycol ether residues are substituted.
  • the free hydroxyl groups with a n-alkyl radicals e.g. methyl, ethyl, propyl, butyl, pentyl
  • the block polymers are also suitable of ethylene oxide with polypropylene oxide.
  • the biological ones are preferred easily degradable surfactants.
  • bleaching agents preferably 1-10, preferably come as bleaching agents %
  • bleach activators such as Tetraacetylethylenediamine (TAED) or tetraacetylglycoluril (TAGU) or peracids or their salts, e.g. the magnesium salt of monoperphthalic acid in Consideration.
  • TAED Tetraacetylethylenediamine
  • TAGU tetraacetylglycoluril
  • peracids or their salts e.g. the magnesium salt of monoperphthalic acid in Consideration.
  • compounds that release active chlorine such as the salts of chlorine-substituted isocyanuric acids, especially pure trichloroisocyanuric acid themselves, can be used. You may be in Amounts of 0.5 to 3, preferably 1 to 2 wt .-%, based on the pressing mixture, admixed.
  • active chlorine bleach Unless active chlorine bleach is added, it can be improved the cleaning performance additional enzymes, preferably commercially available Amylases and / or proteases and / or lipases and / or cutinases in quantities from 0.2 to 5, preferably 0.5 to 3,% by weight are used.
  • additional enzymes preferably commercially available Amylases and / or proteases and / or lipases and / or cutinases in quantities from 0.2 to 5, preferably 0.5 to 3,% by weight are used.
  • a dust-binding additive of up to 3, preferably 1 to, is expedient 2% by weight paraffin oil, alone or together with nonionic surfactants.
  • some of the bleach-free granules can be bleach-stable Dyes or color pigments such as Phthalocyanine, stain and then mix in together with the bleaching agents.
  • fragrances, known bactericidal and dirt-suspending agents, foam inhibitors and corrosion inhibitors can be added.
  • the cleaning agent components are mixed in known mixing devices such as a Lödige mixer.
  • Pressing tools are preferably used for pressing, the stamp surfaces of which are coated with a plastic. Caking on the pressing tools does not occur.
  • the tablets obtained disintegrate perfectly even after prolonged storage.
  • Essentially all known eccentric and rotary presses are suitable for pressing the mixture, which can be used for the production of tablets with diameters of approximately 1.0 cm and more.
  • the compression pressure must be so high that break-stable tablets are formed immediately after manufacture, which are not damaged during tableting, packaging and transport and, despite these high demands on fracture stability, disintegrate quickly during use. This optimum is usually determined by the person skilled in the art by routine testing.
  • the density of the tablets is then - for a given mixture - a consequence of the pressure applied.
  • a compression pressure of 10 to 80, preferably 20 to 65 MPa has proven to be optimal.
  • the tablets obtained by this process have an average density of 1.3-1.9 g / cm 3 and, in addition to high breaking strength, have a uniform porous structure with a large inner surface. They therefore disintegrate particularly quickly when used in the dishwasher.
  • Phase I became 7.0% by weight of compact anhydrous sodium carbonate with 1.0% by weight of defoamer (DEA- WAX (R) -DLW 5419), 7.0% by weight sodium perborate monohydrate, 16.0% by weight sodium metasilicate pentahydrate and 1.0% by weight Plurafac (R) LF 403 (linear fatty alcohol alkoxylate from BASF) in a Lödige mixer mixed.
  • the liter weight of the mixture was 1000 g.
  • the breaking strength of the tablets after preparation was 208 N, after one day> 485 N.
  • the dissolution time was 2.3 minutes after 1 day and 3.2 minutes after 7 days.
  • the tablets were of a uniform structure and of great stability. To determine their dissolution rate, the tablets were placed in one sieve-shaped basket in 1 liter of tap water of 16 ° d at 50 ° C as long moved up and down until they were dissolved (diving test).
  • the tablets When the tablets are used in commercial dishwashers they can come to the tank water by hand or by an automatic Cleaning dosing device can be added. Because the cleaning solution was used directly, especially for this was a quick resolution of the tablets required. The cleaning solution was for several Rinse cycles are used, with constant dilution by fresh water was carried out and accordingly from time to time with new, quickly soluble tablets must be made.
  • the dosage was in one Another trial in a commercial dishwasher (box-type machine) carried out via a rinsing meter, in which 2 kg of this easily soluble tablets from the storage container in the form of a sieve were deposited.
  • a rinsing meter in which 2 kg of this easily soluble tablets from the storage container in the form of a sieve were deposited.
  • the dosage amount was regulated via the conductivity.
  • Examples 1 and 2 which represent compositions according to the invention, the clear advantage of these tablets compared to those according to Examples 1a and 2a, which represent comparative experiments in which with pentasodium triphosphate not defined in more detail with about 20% by weight of phase I -Share was worked.
  • the solubility of the tablets with a high proportion of Phase I increased as expected, but the unusual improvement in the breaking strength of the tablets, which was already noticeable after one day of storage, was not to be expected.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Detergent Compositions (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
  • Glanulating (AREA)

Claims (3)

  1. Procédé de production de comprimés d'agents nettoyants alcalins résistant à la rupture, appropriés à l'utilisation dans des lave-vaisselle, constitués de pentatriphosphate de métal alcalin, de silicates de métaux alcalins qui peuvent contenir éventuellement de l'eau de cristallisation, ainsi que le cas échéant, de carbonates de métaux alcalins, d'agents de blanchiment, d'inhibiteurs de mousse et/ou d'enzymes, et de tensioactifs non ioniques, qui est caractérisé en ce que l'on mélange, d'une manière connue en soi, 15 à 60, de préférence 25 à 50 % en poids de pentatriphosphate de métal alcalin avec une proportion de 20 à 100 % en poids, de préférence de 35 à 80 % en poids et en particulier, de 40 à 60 % en poids de phase I, 35 à 80, de préférence 40 à 55 % en poids de silicate de métal alcalin renfermant éventuellement de l'eau de cristallisation, calculé comme Na2 SiO3 , et le cas échéant, jusqu'à 20 % en poids de carbonate de sodium, jusqu'à 18, de préférence 1 à 10 % en poids d'un agent de blanchiment, jusqu'à 3, de préférence 1 à 2 % en poids d'huile de paraffine et/ou jusqu'à 3 % en poids d'un tensioactif non ionique à mousse freinée, et que l'on presse le mélange en appliquant des pressions de compression supérieures à 7 MPa.
  2. Procédé selon la revendication 1, caractérisé en ce que l'on ajoute lors du mélangeage des ingrédients, la quantité requise d'activateurs de blanchiment, en cas d'utilisation d'agents de blanchiment à base d'oxygène actif.
  3. Procédé selon la revendication 1, caractérisé en ce que l'on remplace environ 3 à 15, de préférence 4 à 12 % en poids de la fraction de métasilicate de sodium anhydre par son penta- et/ou par son nonahydrate.
EP96901299A 1995-01-27 1996-01-18 Procede de production de detergents sous forme de comprimes resistant a la rupture Expired - Lifetime EP0871698B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19502774A DE19502774A1 (de) 1995-01-27 1995-01-27 Verfahren zur Herstellung von bruchstabilen Reinigungstabletten
DE19502774 1995-01-27
PCT/EP1996/000200 WO1996023053A1 (fr) 1995-01-27 1996-01-18 Procede de production de detergents sous forme de comprimes resistant a la rupture

Publications (2)

Publication Number Publication Date
EP0871698A1 EP0871698A1 (fr) 1998-10-21
EP0871698B1 true EP0871698B1 (fr) 2000-04-12

Family

ID=7752604

Family Applications (1)

Application Number Title Priority Date Filing Date
EP96901299A Expired - Lifetime EP0871698B1 (fr) 1995-01-27 1996-01-18 Procede de production de detergents sous forme de comprimes resistant a la rupture

Country Status (7)

Country Link
EP (1) EP0871698B1 (fr)
AT (1) ATE191745T1 (fr)
DE (2) DE19502774A1 (fr)
ES (1) ES2146382T3 (fr)
FI (1) FI973114A0 (fr)
PT (1) PT871698E (fr)
WO (1) WO1996023053A1 (fr)

Families Citing this family (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4408718A1 (de) * 1994-03-15 1995-09-21 Henkel Kgaa Bruch- und lagerstabile, polyfunktionelle Reinigungstabletten, Verfahren zu ihrer Herstellung und ihre Verwendung
GB2318800A (en) * 1996-11-01 1998-05-06 Unilever Plc Detergent composition
GB9706083D0 (en) * 1997-03-24 1997-05-14 Unilever Plc Detergent compositions
ZA984570B (en) 1997-06-06 1999-11-29 Unilever Plc Cleaning compositions.
GB9711829D0 (en) 1997-06-06 1997-08-06 Unilever Plc Detergent compositions
US6534473B1 (en) * 1998-02-10 2003-03-18 Unilever Patent Holdings Bv Process for the manufacture of tablet detergent compositions
DE19843773A1 (de) * 1998-09-24 2000-03-30 Henkel Kgaa Wasch- und Reinigungsmittelformkörper mit feinteiligen Aufbereitungskomponenten
FR2784392B1 (fr) * 1998-10-09 2000-11-17 Rhodia Chimie Sa Tablettes de composition detergente ou anticalcaire et leur mise en oeuvre en lave-vaisselle ou lave-linge
GB9826097D0 (en) * 1998-11-27 1999-01-20 Unilever Plc Detergent compositions
DE19859807A1 (de) * 1998-12-23 2000-06-29 Henkel Kgaa Phosphat-Compounds
BR0012037A (pt) * 1999-06-29 2002-03-19 Unilever Nv Tablete para lavar pratos à máquina
GB2390853A (en) * 2002-07-16 2004-01-21 Reckitt Benckiser Nv Cleaning composition containing hydrophobic component
DE102011106092B4 (de) * 2011-06-09 2024-01-11 Budich International Gmbh Mehrphasige Reinigertablette mit integriertem Entschäumer und ihre Verwendung

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3315950A1 (de) * 1983-05-02 1984-11-15 Henkel KGaA, 4000 Düsseldorf Verfahren zur herstellung von reinigungsmitteltabletten
DE3541146A1 (de) * 1985-11-21 1987-05-27 Henkel Kgaa Mehrschichtige reinigungsmitteltabletten fuer das maschinelle geschirrspuelen
DE3634813A1 (de) * 1986-10-13 1988-04-14 Henkel Kgaa Reinigungsmitteltabletten fuer das maschinelle geschirrspuelen
DE4229650C1 (de) * 1992-09-04 1994-01-05 Henkel Kgaa Verfahren zur Herstellung von Reinigungstabletten

Also Published As

Publication number Publication date
DE19502774A1 (de) 1996-08-01
ES2146382T3 (es) 2000-08-01
FI973114A (fi) 1997-07-25
FI973114A0 (fi) 1997-07-25
EP0871698A1 (fr) 1998-10-21
DE59604972D1 (de) 2000-05-18
WO1996023053A1 (fr) 1996-08-01
ATE191745T1 (de) 2000-04-15
PT871698E (pt) 2000-10-31

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