EP0636168A1 - Procede de fabrication d'un agent de lavage se presentant sous forme de granules et contenant du perborate - Google Patents

Procede de fabrication d'un agent de lavage se presentant sous forme de granules et contenant du perborate

Info

Publication number
EP0636168A1
EP0636168A1 EP93908873A EP93908873A EP0636168A1 EP 0636168 A1 EP0636168 A1 EP 0636168A1 EP 93908873 A EP93908873 A EP 93908873A EP 93908873 A EP93908873 A EP 93908873A EP 0636168 A1 EP0636168 A1 EP 0636168A1
Authority
EP
European Patent Office
Prior art keywords
weight
parts
water
granulation
sodium
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.)
Withdrawn
Application number
EP93908873A
Other languages
German (de)
English (en)
Inventor
Juan Carlos Wuhrmann
Jürgen Härer
Jochen Jacobs
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 EP0636168A1 publication Critical patent/EP0636168A1/fr
Withdrawn legal-status Critical Current

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
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C11D3/08—Silicates
    • 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
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
    • C11D11/0088—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads the liquefied ingredients being sprayed or adsorbed onto solid particles
    • 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
    • C11D3/10—Carbonates ; Bicarbonates
    • 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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/39—Organic or inorganic per-compounds
    • C11D3/3942—Inorganic per-compounds

Definitions

  • the invention relates to a method for producing a cleaning agent which can be used in dishwashers and which contains a perborate salt as an oxygen carrier.
  • German Offenlegungsschrift 29 25 137 proposes homogeneous dust-free and free-flowing detergent and cleaning agent granules which contain pentasodium triphosphate, sodium sulfate, sodium perborate, detergent substances, silicates and complexing agents.
  • the constituents are granulated in a reactor at reaction times between 0.1 to 20 seconds and at temperatures below 95 ° C., preferably below 50 ° C., with the addition of water.
  • perborate salts are sensitive to water and / or temperatures.
  • the pentasodium triphosphate can form salts containing water of crystallization and thus consume the water required for granulation to form the hexahydrate, so that it cannot damage the perborate salts.
  • German patent application DE 39 10569 it is proposed to first convert pentasodium triphosphate partially into the hexahydrate to produce a detergent granulate, then to mix it with essentially anhydrous sodium metasilicate, anhydrous sodium carbonate and sodium metasilicate hydrate, to granulate with a water glass solution and then to granulate it , ie not during or before granulation, if necessary add an active oxygen carrier. Finally, the granules obtained in this way should ripen in a moist air stream.
  • pentasodium triphosphate is also used, it is possible to granulate perborate salts directly.
  • the invention thus relates to a method for producing a cleaning agent for dishwashers with a perborate salt as an oxygen carrier, in which, for example, in a first granulation stage (A)
  • anhydrous sodium carbonate of which up to about 5 parts by weight can be replaced by sodium metasilicate hydrates (penta- or hexahydrate), mixed (B) and then in a granulation mixer in a final granulation stage (C)
  • the granulation process according to the invention provides for the water softener to be subjected to pregranulation in a first granulation stage.
  • water softeners within the meaning of the invention are preferably understood to mean water softeners or water softener combinations free of pentasodium triphosphate.
  • about 4 to 25% by weight of the sodium salt of a polycarboxylic acid can be used as the water softener in the first stage.
  • the polycarboxylic acid sodium salts in question here are well known to the person skilled in the art.
  • They are homopolymers or copolymers of unsaturated monocarboxylic acids or dicarboxylic acids, that is to say in particular one or more monomers from the following group: acrylic acid, methacrylic acid, maleic acid, itaconic acid, citraconic acid.
  • Preferred products are in the molecular weight range below 100,000, for example between 50,000 and 70,000.
  • the copolymers of acrylic acid and maleic acid in a molar ratio of about 1: 9 to 9: 1 are particularly preferred.
  • mixtures of about 10 to 30% by weight of zeolite NaA powder and about 1 to 8% by weight of the sodium salt of one of the aforementioned polycarboxylic acids can be used as the water softener.
  • the zeolite NaA powder is the water-containing form customary for use in detergents and cleaning agents, not the annealed water-free form. About 0.1 to 10 parts by weight of water are added for the purpose of granulation, ie the caking of the particles. The water can be added directly as such into the mixing kettle * . In addition to or instead of water can be used but also water-containing surfactant r Zeolithaufschlämmungen.
  • Such zeolite slurries are known from the spray drying technology of detergents. They usually consist of about 10 to 60% by weight of zeolite NaA powder, water and nonionic surfactants for stabilization. Suitable nonionic surfactants are, for example, the ethoxylates of long-chain alcohols. Such zeolite slurries are preferably used in an amount of about 2 to 5% by weight.
  • the percentage by weight refers here, as elsewhere, to the entire cleaning agent.
  • the individual constituents of the cleaning agents are to be selected from the amounts stated so that they total 100% by weight.
  • the granulation process is carried out until about 85% by weight of the powder has a grain size of more than 0.2 mm.
  • Fast-running mixers and dwell times of 0.2 to 10 seconds are required for this, and the precise setting of these values is easily possible for the cleaning agent technician on the basis of a few preliminary tests.
  • Relevant for the grain size of the product of the first stage are, in addition to the amount of water added, in particular the shear forces exerted on the material in the first mixing stage. These shear forces are determined by the number, shape and number of revolutions of the mixing tools arranged in the first mixing stage.
  • the number of revolutions of the shaft suitable for the optimal grain distribution, " _T the number of knives and their angle of inclination can easily be determined by the skilled person through experiments.
  • the material leaving the first pelletizing stage expediently enters a conveyor device, which in the simplest case consists of a conveyor belt.
  • the conveying path and the conveying speed are matched to one another such that the time from leaving the first mixing stage to entering the second stage takes about 10 to at most 60 seconds, preferably about 10 to 30 seconds. It is also advantageous if care is taken to ensure that the water does not evaporate from the material. This can be done by moving the conveyor belt in an atmosphere saturated with water vapor or by overlaying the water softener with the powdered sodium silicate (preferably metasilicate with the above-mentioned S1O2 to Na2 ⁇ ratio).
  • a crusher is expediently arranged, which breaks the so-called rollover. H. coarse grains or chunks, crushed.
  • anhydrous sodium carbonate (soda) and the sodium metasilicate hydrate which may be used are continuously fed in the intended amount onto the conveyor belt. It is preferred to add these components after the anhydrous metasilicate.
  • the anhydrous sodium carbonate to be used should predominantly have a grain size of 0.05 to 1 mm.
  • the sodium metasilicate should have an average grain size of 0.2 to 1.5 mm, the amount is 5 to 20 parts by weight or% by weight.
  • the mixture reaches a mixer in which the water softener is intimately mixed with the overlaid metasilicate, the soda and the metasilicate hydrate.
  • the dry mixing of the components takes about 20 to 120 seconds. Any further heating of the material is stopped by the mixing process. A partial evaporation of the remaining water • f and a lump formation is successfully countered. Particularly good powder properties and favorable granulation conditions are achieved when the dry mixture has a temperature of 45 to 70 ° C.
  • the powdery mixture is after the completion of the dry mixing, i.e. H. after complete homogenization, fed to the new granulation.
  • This can either be carried out in the same mixing unit if it has the facilities required for the granulation, or it can be a special one.
  • Granulator can be used.
  • the granulator consists, for example, of a drum mixer which is arranged horizontally or is slightly inclined. It can be rotatably mounted as a whole and equipped with chicanes, or it can also be stationary and equipped with mixing and conveying elements, so-called plow blades, arranged on a rotatable longitudinal shaft. A plurality of nozzles are arranged in the interior of the mixer, by means of which liquid components are sprayed uniformly onto the material whirled around or which trickles down from rotating mixing tools.
  • the powdery mixture is sprayed with the aqueous solution of about 0.5 to 5 parts by weight of water glass, dissolved in about 1 to 8 parts by weight of water.
  • the aqueous solution of about 0.5 to 5 parts by weight of water glass, dissolved in about 1 to 8 parts by weight of water.
  • about 2 to 15 parts by weight of perborate salt are added.
  • Sodium perborate which can be present as a monohydrate or pentahydrate, is preferred.
  • a foam inhibitor e.g. B. a liquid paraffin oil or a liquid silicone oil to be added
  • this can be injected before the aqueous silicate solution. Amounts of about 1 to 3 parts by weight are preferred. It is also advantageous to spray the nonionic, low-foaming surfactant to be added in an amount of from 0 to about 3 parts by weight (preferably about 0.5 to 3 parts by weight) in the final granulation step. This can be done together with the sodium silicate solution or separately from it via a separate spray nozzle. However, the surfactant can also be mixed in at a later point in the process, with any small amounts of dust present in the finished granulated product being bound respectively • ⁇ - be glued to the granulate.
  • the known ethoxylation products of long-chain alcohols and alkylphenols are suitable as nonionic surfactants, the free hydroxyl group of the polyethylene glycol ether residue being substituted by ether or acetal groups or by polypropylene glycol ether residues or butyl ether residues to reduce the tendency to foam.
  • the block polymers of ethylene oxide with polypropylene oxide or also the alkyl polyglycosides are also suitable.
  • the average residence time in the granulation stage is generally about 60 to 300 seconds, preferably about 90 to 200 seconds.
  • the granulation mixer can be operated continuously or in batches.
  • the material emerging from the granulation mixer generally has a temperature of about 55 to 88 ° C. and still requires a short ripening or recrystallization time of about 5 to a maximum of 15 minutes, usually of about 3 to 12 minutes, during which it is used Avoiding clump formation is kept in motion.
  • the very sensitive perboate salt can be processed under the specified conditions with no or no significant loss of activity.
  • the completely crystallized, ripened granulate can be processed further in a manner known per se after leaving the vortex channel, that is, if not yet done, cooled with flowing air and, if desired, mixed with other constituents of the detergent, such as dyes, etc.
  • the granules are largely resistant to abrasion and have a favorable grain spectrum of approximately 0.2 to 31.5 m, ie. H. their dust content is minimal. It is particularly advantageous that the method of operation according to the invention does not cause caking at any time - for example on container walls and / or mixing elements.
  • Coarse grain formed to a small extent can be mixed into the product again after sieving and grinding. Small amounts of dust, which, for example, are swept along by the circulating air when passing through the vortex trough, can be recovered in dust separators and returned to the granulation mixer.
  • the granules are easy to pour and scatter, do not tend to separate and are stable in storage. When used, they show faultless flushing behavior, even under unfavorable conditions, ie in not optimally designed flushing devices. -5 examples
  • a cleaning agent for use in a household dishwasher was produced.
  • the products according to the present invention had approximately the following composition (in% by weight):
  • sodium silicate Na2 ⁇ : S ⁇ 2
  • paraffin oils 0 to 30%, preferably 0 to 30% sodium carbonate
  • the mixer essentially consisted of a vertically arranged downpipe with nozzles arranged in the upper third, pointing downwards, and a central, rotatable shaft on which two knife rings each with 6 knives were arranged, one in the upper and the second in the lower third of the mixing tube.
  • the knife planes were inclined up to 5 ° to the horizontal in order to achieve a slight suction effect.
  • the speed of the shaft was 2000 to 3000 rpm in the examples.
  • the powder fell into an inclined towards the horizontal, from a fixed ⁇ o - tube equipped with rotating agitator and conveying elements mixer (II).
  • the average residence time in the mixing zone (B) was approximately 30 seconds at a temperature of approximately 65 ° C.
  • the product entered the granulation zone (C), where it was mixed with an aqueous solution of 0.2 part by weight of perfume, 1.5 parts by weight of paraffin oil and 1.3 parts by weight of water glass 3. 0 was sprayed continuously. Then 7.0 parts by weight of sodium perborate monohydrate were added.
  • the product was discharged and reached one. vortex channel arranged in a closed chamber. In this vortex channel, air heated to 95 ° C. with a relative humidity of 70 to 80% was circulated.
  • the average residence time of the granules in the vortex channel was 10 minutes.
  • the product had better bleaching properties compared to tea and coffee stains like comparable composite commercial powder cleaning agents, which may have been due to a lack of homogeneity in powder compositions.
  • Example 2 The procedure was the same as in Example 1.
  • the zeolite powder was added in step A together with the metasilicate to the moist pentasodium triphosphate.
  • the temperature of the material emerging from the granulation mixer was lower than in Example 1 and was approximately 60-70 ° C.
  • stage A the hydration phase
  • stage B the components for the replacement of phosphate are added to stage B, whereby the material naturally does not heat up in this stage due to the absence of the heat of hydration.
  • the sodium perborate monohydrate is then added in the granulation stage (C).
  • the temperature of the material emerging from the granulation mixer does not exceed approx. 50 ° C. in the case of the phosphate-free mixtures.
  • A2 Sodium orthosilate pentahydrate in the weight ratio of agglomerate to silicate such as about 9: 1 can also be mixed into the agglomerate.
  • a phosphate and zeolite-free cleaning agent could also be produced by the process according to the invention. It had the following composition:
  • Sodium orthosilicate pentahydrate and nonionic surfactant can also be added to the agglomerate obtained according to the following recipe.
  • a raw material mixture consisting of
  • sodium perborate monohydrate -3 was granulated with a total of 19.08% by weight of water.
  • Sodium perborate monohydrate was added to the wet granules and the mixture was dried in a fluidized bed.
  • the temperature of the supply air was 80 ° C in test 1 and 100 ° C in test 2.
  • the dried product was with
  • Ci2-Ci4 fatty alcohol 1.00% by weight of Ci2-Ci4 fatty alcohol. 4 E0 x 5 PO and 15.00 wt .-% sodium orthosilicate pentahydrate mixed. The final water content of the blended products is 2.98%.
  • the cleaning performance was determined with standard soiling. Grade 0 receives the original soiled dishes. A grade of 10 is given with optimal cleaning.
  • the standard product is a commercially available cleaner of the following composition:
  • This cleaning agent was produced from the individual raw materials by mixing.
  • Table 1 Cleaning performance immediately after production of the dishwasher: Miele G 590 program: 55 ° C universal
  • Dishwasher Miele G 590 program: 55 ° C universal
  • the products with granulated perborate monohydrate were examined under various conditions: room temperature conditions (20 ° C / 50% relative air humidity, 30 ° C / 80% relative air humidity, 40 ° C).
  • the most important parameters for the products with granulated perborate monohydrate are the active oxygen content and the cleaning performance in the case of tea stains.
  • the bleaching performance of tea stains correlates with the active oxygen content of the product.
  • the cleaning performance was confirmed under hard water conditions (16 ° d) in order to clearly work out differences in performance in tea bleaching.
  • a bleaching performance of notes 3 - 4 under hard water conditions (16 ° d) corresponds to notes 7 - 9 under soft water conditions (softened water).
  • Water softening is state of the art in dishwashers.
  • the bleaching performance of the products with granulated perborate monohydrate is sufficient for good bleaching performance even after storage under the conditions mentioned above.

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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)

Abstract

L'invention concerne un procédé de fabrication d'un agent de lavage pour lave-vaisselle selon lequel on peut utiliser du perborate. Selon ledit procédé, l'on granule le perborate dans une seconde phase de granulation conjointement avec les autres constituants prégranulés et mélangés avec ledit perborate.
EP93908873A 1992-04-10 1993-04-01 Procede de fabrication d'un agent de lavage se presentant sous forme de granules et contenant du perborate Withdrawn EP0636168A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19924212166 DE4212166A1 (de) 1992-04-10 1992-04-10 Verfahren zur Herstellung perborathaltiger Reinigergranulate
DE4212166 1992-04-10
PCT/EP1993/000795 WO1993021297A1 (fr) 1992-04-10 1993-04-01 Procede de fabrication d'un agent de lavage se presentant sous forme de granules et contenant du perborate

Publications (1)

Publication Number Publication Date
EP0636168A1 true EP0636168A1 (fr) 1995-02-01

Family

ID=6456607

Family Applications (1)

Application Number Title Priority Date Filing Date
EP93908873A Withdrawn EP0636168A1 (fr) 1992-04-10 1993-04-01 Procede de fabrication d'un agent de lavage se presentant sous forme de granules et contenant du perborate

Country Status (3)

Country Link
EP (1) EP0636168A1 (fr)
DE (1) DE4212166A1 (fr)
WO (1) WO1993021297A1 (fr)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB9504442D0 (en) * 1995-03-06 1995-04-26 Brunner Mond & Co Ltd Granular bleach/builder product
GB9526097D0 (en) * 1995-12-20 1996-02-21 Unilever Plc Process
BRPI0808513A2 (pt) 2007-03-09 2014-08-19 Danisco Us Inc Genencor Div Variantes de alfa-amilase de espécies de bacillus alcalifílico, composições compreendendo variantes de alfa-amilase e métodos de uso
US9040279B2 (en) 2008-06-06 2015-05-26 Danisco Us Inc. Saccharification enzyme composition and method of saccharification thereof
CA2726803A1 (fr) 2008-06-06 2009-12-10 Danisco Us Inc. Alpha amylases variantes de bacillus subtilis et leurs procedes d'utilisation
EP2698434A1 (fr) 2008-06-06 2014-02-19 Danisco US Inc. Utilisations d'une alpha-amylase de Bacillus subtilis
CA2778471A1 (fr) 2009-10-23 2011-04-28 Danisco Us Inc. Procedes destines a reduire le saccharide donnant une couleur bleue

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1071874B (fr) * 1959-12-24
DE2925137A1 (de) * 1979-06-22 1981-01-08 Keri Dipl Ing Karoly Homogene, staubfreie und rieselfaehige wasch- und reinigungsmittelgranulate, sowie verfahren zu deren herstellung
IT1187668B (it) * 1985-05-16 1987-12-23 Montefluos Spa Procedimento per ottenere perborato di sodio moncidrato granulare dotato di una buona resistenza meccanica
DE3910569A1 (de) * 1989-04-01 1990-10-04 Henkel Kgaa Verfahren zur herstellung eines maschinengeschirrspuelmittel-granulates
KR920703439A (ko) * 1989-08-19 1992-12-17 원본미기재 과 붕산염 일수화물의 과립화 방법

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO9321297A1 *

Also Published As

Publication number Publication date
WO1993021297A1 (fr) 1993-10-28
DE4212166A1 (de) 1993-10-14

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