EP3318622B1 - Gefärbte partikel für waschmittel und herstellungsverfahren dafür - Google Patents

Gefärbte partikel für waschmittel und herstellungsverfahren dafür Download PDF

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Publication number
EP3318622B1
EP3318622B1 EP16020434.3A EP16020434A EP3318622B1 EP 3318622 B1 EP3318622 B1 EP 3318622B1 EP 16020434 A EP16020434 A EP 16020434A EP 3318622 B1 EP3318622 B1 EP 3318622B1
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EP
European Patent Office
Prior art keywords
sodium sulfate
detergents
bentonite
coloured particles
phase
Prior art date
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EP16020434.3A
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English (en)
French (fr)
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EP3318622A1 (de
Inventor
Miguel Ángel CABALLERO
Ainhoa BILBAO
Jorge BERENGUER
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.)
Minera Catalano Aragonesa SA
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Minera Catalano Aragonesa SA
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Priority to ES16020434T priority Critical patent/ES2953916T3/es
Priority to EP16020434.3A priority patent/EP3318622B1/de
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Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/06Powder; Flakes; Free-flowing mixtures; Sheets
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00Special methods for preparing compositions containing mixtures of detergents
    • C11D11/0082Special 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
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02Inorganic compounds ; Elemental compounds
    • C11D3/04Water-soluble compounds
    • C11D3/046Salts
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/40Dyes ; Pigments

Definitions

  • This description refers, as its title indicates, to new, improved coloured particles for detergents and their production process.
  • These particles essentially contain a mixture of sodium sulfate and bentonite which are characterised by being fast-dissolving and having a low apparent density, in the range of 0.8 to 1.1 kg/l.
  • These coloured particles are obtained using a production process that hitherto has not been described.
  • the invention is applicable as a distinguishing element in the manufacture of powdered detergents.
  • coloured particles also known as "speckles”
  • spekles are well known in the market, as a component of a commercial nature in powdered detergent formulations.
  • the said particles are used to give the powdered detergent a visually distinguishing element that is associated with the improved efficacy of the powdered detergent.
  • the particles are solely based on sodium sulfate and a colouring agent although there are also other options that use exclusively carbonates or bentonites together with colouring agents.
  • the said coloured particles that exist in the market present one or more of the following drawbacks and problems for use:
  • the said patent describes the possibility of dividing one of the solids into 2 parts, including a 4th step in which the 2nd part of the solid is added. As can be seen, it is a process of 3 or 4 steps of adding and mixing two solids in which not even a pigment/dye is added for colouring.
  • CN 102 504 977 A describes a color particle composition that is used for powdery, sheet or granular fabric detergent.
  • EP 2 216 389 A1 describes a detergent builder granule.
  • EP 2 009 086 A1 discloses a procedure for colouring non-adsorbent minerals and the product thus obtained.
  • US 2011/053823 A1 discloses colored speckles.
  • the present description refers to coloured particles for detergents having the features of claim 1 and the process to obtain them having the features of claim 5, which resolves the problems that currently exist with the production of coloured particles.
  • Bentonite is the name given to a clay with a high content (typically more than 60-70%) of montmorillonite.
  • Montmorillonite belongs to the group of smectites, a group that includes other clays.
  • bentonite that are characterised by a high content of other clays from the smectite group (beidellite, hectorite, nontronite, saponite, sauconite and stevensite, amongst others).
  • Bentonite is used as a binding agent as it endows the mixture with the necessary plastic properties to allow it to be granulated.
  • clays such as kaolin, sepiolite, attapulgite, illite or other smectites etc. can be used as binders.
  • bentonite is preferred due to its greater effectiveness and because it is accepted in the detergent industry.
  • the characteristic production process comprises a phase of mixing the solids, a phase of metering the water and/or additives, and a granulating phase.
  • the coloured particles for detergents that are presented are new since, prior to the present invention a product of this type that contains a mix of sodium sulfate and bentonite in the same particle has not been proposed. The process of obtaining the new coloured particles for detergents has not been described previously either.
  • the coloured particles for detergents that are presented overcome the drawbacks of the coloured particles for detergents described to date and/or present in the market.
  • the coloured particles for detergents described herein are much faster-dissolving than other commercial products, even in cold water.
  • the process described in this invention simplifies the process with respect to known particle manufacturing processes, as it reduces it to just two phases of adding materials even when more ingredients are added, such as pigment/dye and other additives to improve the physical or mechanical characteristics of the product obtained.
  • the coloured particles for detergents that are the subject matter of the invention consist of a mixture of sodium sulfate and bentonite. Both elements are well known and commonly used for other functions in the field of detergents.
  • the bentonite used is of a light colour, preferably white, to foster a greater intensity of the final colour of the new coloured particles.
  • Bentonite is provided in a proportion of between 15% and 25% by weight in relation to the total weight of solids used (bentonite and sodium sulfate).
  • the sodium sulfate used has a grain size of between 70 and 450 ⁇ m, preferably between 70 and 250 ⁇ m, and it is provided in a proportion of between 75% and 85% by weight in relation to the total weight of solids used (bentonite and sodium sulfate).
  • Water is used as the binder of the mixture of sodium sulfate and bentonite, as it is more economical and the desired results are achieved with the process employed. It is added in a proportion of 5% to 15% by weight in relation to the total weight of the solids used (bentonite and sodium sulfate).
  • Liquid dyes and pigments are added to the mixture of sodium sulfate and bentonite as colouring agents. With the process described herein they are added at the same time as the water, thus simplifying the process and making it quicker.
  • the percentage of pigment or ink added is between 0.3% and 5% in relation to the total weight of the solids used (bentonite and sodium sulfate), preferably between 0.7% and 1.5%.
  • PVA polyvinyl alcohol
  • CMC carboxymethylcellulose
  • sodium silicate materials that are well known by any person skilled in the art and accepted in the detergent industry. They can be added without increasing the steps in the production process, both in solid and liquid state. When they are solids they are added in the initial mixing of solids. When they are liquids they are added together with the granulating water.
  • the percentage of these additives used is between 0% and 3% in relation to the total weight of the solids used (bentonite and sodium sulfate)
  • the apparent density of the coloured particles obtained is between 0.8 and 1.1 kg/l, preferably between 0.9 and 1.1 kg/l.
  • the grain size of the coloured particles is between 600 and 1.200 ⁇ m
  • an intensive type mixer such as an EIRICH type mixer is used, although there are other industrial mixers such as LODIGE, BÜHLER, etc. It comprises two main elements: the pan where granulating is carried out and a granulating tool.
  • the pan rotates on its axis to help granulation and to shorten the total duration of process.
  • the granulating tool consists of rotating blades which produce a vortex that granulates the product.
  • the production process comprises 3 distinct sequential phases. These 3 phases take place consecutively in the same intensive type mixer with granulating tool.
  • Phase 1 the solids (sodium sulfate, bentonite and other solid additives, where appropriate) are added to the granulating pan and are mixed for between 20 and 90 seconds to obtain a good dispersion of the bentonite in the sodium sulfate and ensure a homogeneous mix.
  • This step is critical, since if an adequate mix is not obtained, a certain number of sodium sulfate particles will not be capable of subsequent granulation in phase 3, due to not being in contact with the water and bentonite at the same time, since they do not have plastic properties to form granules by themselves.
  • phase 2 commences, in which the mix of liquids that contains water and pigment is added.
  • liquids such as binders and bulking agents are added, they are added together with the water.
  • a constant addition flow is maintained, although adding the amount of liquids required takes between 45 and 80 seconds.
  • the granulating agent is water which, when added to the solid mixture transforms the material, endowing it with a larger particle size and, at the same time, a lower apparent density than would be obtained if the bentonite and sodium sulfate were combined in dry conditions.
  • Phase 3 the pan's granulating tool is used for a period of 1 to 15 minutes, preferably 3 minutes.
  • This phase is characterised by the growth of the grain when it comes into contact with the water and the plastic material in optimized operating conditions.
  • the phase is considered to have ended when a certain time has elapsed, which will correspond to the most suitable granulometric distribution for the type of product to be then processed. If the operating time in this phase is less then there will be a significant amount of particles that will not reach a sufficient particle size. Likewise, increasing time beyond the optimum period will result in a higher rejected or even broken fraction due to excessive granulating.
  • the product After granulation is achieved in phase 3 the product undergoes screening to the required particle size range. Following this, it goes to the dryer where excess moisture is eliminated, preventing the formation of clumps of the finished product, since it is a hygroscopic material. Rejected fractions of the product are reutilised and returned to the start of the process where the material is reused, avoiding waste management costs.
  • Example 1 the procedure described in patent EP 2009086B1 is followed to produce a coloured sodium sulfate.
  • Granular sodium sulfate is placed in a reactor and sodium silicate and pigment are added under stirring. It is then dried. Particles with a diameter of 900 ⁇ m and an apparent density of 1.5 kg/1 are obtained. This density is higher than that of powdered detergents.
  • Example 2 in the granulator, a mixture of sodium sulfate and bentonite is added in a percentage of 85% sodium sulfate and 15% bentonite (% by weight in relation to the total weight of the mixture). It is mixed for 30 seconds to homogenise it and the mixture of water and colouring agent is added. It is mixed for 2 minutes and a granulated product of a homogeneous appearance is obtained, with a mean particle size of 800 ⁇ m and density of 0.9 kg/l. It is a product that is apt for the powdered detergent market since it has suitable particle size, colouring and apparent density.
  • Example 3 to a commercial detergent with a density of 0.8 kg/l, the granulate that is the subject matter of this invention (example 2) and another commercial coloured product (example 1) are added.
  • the product is shaken, simulating transportation conditions, a percentage of the coloured sulfate particles of example 1 (apparent density 1.5 kg/l), falls to the bottom of the package and the desired effect upon opening the box of detergent is not achieved.
  • the apparent density is much lower (0.9 kg/l compared to 1.5 kg/l)
  • transportation conditions are simulated the new coloured particles remain evenly distributed in the detergent.
  • Example 4 in this example the dissolution of different colour particles (example 2 and example 1) is studied and compared using methods that are known and accepted in the detergent industry.

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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)

Claims (9)

  1. Farbige Partikel für Waschmittel, von der Art, wie sie bei der Herstellung von pulverförmigen Waschmitteln als Unterscheidungsmerkmal verwendet werden, dadurch gekennzeichnet, dass sie aufweisen
    Bentonit als ein Bindemittel in einem Verhältnis von zwischen 15 und 25 Gewichtsprozent in Bezug auf das Gesamtgewicht von Bentonit und Natriumsulfat,
    Natriumsulfat in einem Verhältnis von zwischen 75 und 85 Gewichtsprozent in Bezug auf das Gesamtgewicht von Bentonit und Natriumsulfat,
    Wasser als ein Binder in einem Verhältnis von zwischen 5 und 15 Gewichtsprozent in Bezug auf das Gesamtgewicht von Bentonit und Natriumsulfat
    und Farbpigment oder Flüssigfarbstoff als ein Färbemittel in einem Verhältnis von zwischen 0,3 und 5 Gewichtsprozent in Bezug auf das Gesamtgewicht von Bentonit und Natriumsulfat,
    wobei ihre Dichte zwischen 0,8 und 1,1 kg/l liegt und
    wobei ihre Korngröße zwischen 600 und 1200 pm liegt.
  2. Farbige Partikel für Waschmittel nach Anspruch 1, wobei das Natriumsulfat eine Korngröße von zwischen 70 und 450 pm, vorzugsweise zwischen 70 und 250 pm, aufweist.
  3. Farbige Partikel für Waschmittel nach einem der vorhergehenden Ansprüche, wobei das Farbpigment oder der Flüssigfarbstoff in einem Verhältnis von zwischen 0,7 und 1,5 Gewichtsprozent in Bezug auf das Gesamtgewicht von Bentonit und Natriumsulfat vorhanden ist.
  4. Farbige Partikel für Waschmittel nach einem der vorhergehenden Ansprüche, wobei sie andere Zusätze, wie beispielsweise Binder und Füllstoffe, aufweisen, die in einem Verhältnis von zwischen 0% und 3% in Bezug auf das Gesamtgewicht von Bentonit und Natriumsulfat vorliegen und aus der Gruppe, die aus Polyvinylalkohol (PVA), Cellulosen, wie beispielsweise Carboxymethylcellulose (CMC), und Natriumsilikat gebildet wird, ausgewählt sind.
  5. Verfahren zur Herstellung von farbigen Partikeln für Waschmittel nach den vorhergehenden Ansprüchen, wobei es drei aufeinanderfolgende Phasen aufweist:
    Phase 1 des Mischens von Feststoffen, wobei die Feststoffe, Natriumsulfat, Bentonit und
    gegebenenfalls andere feste Zusätze, in den Granuliertiegel gegeben und zwischen 20 und 90 Sekunden lang gemischt werden, um eine gute Dispersion des Bentonits in dem Natriumsulfat zu erzielen und ein homogenes Gemisch zu gewährleisten;
    Phase 2 des Dosierens von Wasser und/oder Zusätzen, wobei das Farbpigment zuvor mit Wasser gemischt worden ist, und
    Phase 3 des Granulierens,
    das in einem Intensivmischer durchgeführt wird, der aus zwei Hauptelementen zusammengesetzt ist: dem Tiegel, der sich um seine Achse dreht, wo das Granulieren stattfindet, und einem Granulierwerkzeug, das aus rotierenden Klingen besteht.
  6. Verfahren zur Herstellung von farbigen Partikeln für Waschmittel nach Anspruch 5, wobei in Phase 2 das Gemisch aus Flüssigkeiten, das Wasser, Farbpigment oder Farbstoff enthält, und optional flüssige Zusätze, wie beispielsweise Binder und Füllmittel, zugesetzt wird.
  7. Verfahren zur Herstellung von farbigen Partikeln für Waschmittel nach einem der vorhergehenden Ansprüche 5 bis 6, wobei in Phase 3 das Granulierwerkzeug des Tiegels an dem vorstehend genannten Gemisch eine Zeitlang von zwischen 1 bis 15 Minuten angewendet wird.
  8. Verfahren zur Herstellung von farbigen Partikeln für Waschmittel nach einem der vorhergehenden Ansprüche 5 bis 7, wobei, sobald Phase 3 geendet hat, die erzielten farbigen Partikel einer Auswahlprüfung auf den erforderlichen Partikelgrößenbereich unterzogen werden.
  9. Verfahren zur Herstellung von farbigen Partikeln für Waschmittel nach einem der vorhergehenden Ansprüche 5 bis 8, wobei, sobald Phase 3 vollendet worden ist, die farbigen Partikel zu einem Trockner gehen, wo überschüssige Feuchtigkeit entfernt wird.
EP16020434.3A 2016-11-04 2016-11-04 Gefärbte partikel für waschmittel und herstellungsverfahren dafür Active EP3318622B1 (de)

Priority Applications (2)

Application Number Priority Date Filing Date Title
ES16020434T ES2953916T3 (es) 2016-11-04 2016-11-04 Partículas coloreadas para detergentes y procedimiento de producción de las mismas
EP16020434.3A EP3318622B1 (de) 2016-11-04 2016-11-04 Gefärbte partikel für waschmittel und herstellungsverfahren dafür

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP16020434.3A EP3318622B1 (de) 2016-11-04 2016-11-04 Gefärbte partikel für waschmittel und herstellungsverfahren dafür

Publications (2)

Publication Number Publication Date
EP3318622A1 EP3318622A1 (de) 2018-05-09
EP3318622B1 true EP3318622B1 (de) 2023-07-05

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EP (1) EP3318622B1 (de)
ES (1) ES2953916T3 (de)

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US711796A (en) 1902-04-24 1902-10-21 Alfred B Tarbox Wire-rope block.
US4609473A (en) 1984-11-26 1986-09-02 Colgate Palmolive Company Bentonite-sulfate fabric softening particulate agglomerate, processes for manufacture and use thereof, and detergent compositions containing it
DE4009618A1 (de) 1990-03-26 1991-10-02 Henkel Kgaa Spruehgetrocknetes, avivierend wirkendes waschmitteladditiv
EP2009086B1 (de) * 2007-06-26 2013-03-27 Sociedad Anonima Minera Catalano-Aragonesa (Samca) Verfahren zum Einfärben nicht-adsorbierender Mineralien und dadurch erhaltenes Produkt
WO2009063725A1 (ja) 2007-11-16 2009-05-22 Kao Corporation 洗剤ビルダー顆粒
US8318652B2 (en) * 2009-08-25 2012-11-27 Milliken & Company Colored speckles comprising a porous carrier and a releasing agent layer
CN102504977B (zh) * 2011-11-03 2013-04-17 广州立白企业集团有限公司 一种用于粉状、片状或粒状织物洗涤剂的颜色粒子组合物

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
MUNINDRA BISEN ET AL: "Classroom Segregation of Granular Material in Two and Three-Dimensional Units", 1 October 2016 (2016-10-01), XP055652267, Retrieved from the Internet <URL:https://link.springer.com/content/pdf/10.1007/s12045-016-0402-9.pdf> [retrieved on 20191212] *

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Publication number Publication date
ES2953916T3 (es) 2023-11-17
EP3318622A1 (de) 2018-05-09

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