EP0037026B1 - Verfahren zur Herstellung eines lagerstabilen, leichtlöslichen Granulates mit einem Gehalt an Bleichaktivatoren - Google Patents

Verfahren zur Herstellung eines lagerstabilen, leichtlöslichen Granulates mit einem Gehalt an Bleichaktivatoren Download PDF

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Publication number
EP0037026B1
EP0037026B1 EP81102083A EP81102083A EP0037026B1 EP 0037026 B1 EP0037026 B1 EP 0037026B1 EP 81102083 A EP81102083 A EP 81102083A EP 81102083 A EP81102083 A EP 81102083A EP 0037026 B1 EP0037026 B1 EP 0037026B1
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EP
European Patent Office
Prior art keywords
weight
percent
water
bleach activator
granulating
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
Application number
EP81102083A
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German (de)
English (en)
French (fr)
Other versions
EP0037026A1 (de
Inventor
Herbert Dr. Saran
Martin Dr. Witthaus
Eduard Dr. Smulders
Karl Schwadtke
Günther Dr. Vogt
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
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Filing date
Publication date
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Application filed by Henkel AG and Co KGaA filed Critical Henkel AG and Co KGaA
Priority to AT81102083T priority Critical patent/ATE14594T1/de
Publication of EP0037026A1 publication Critical patent/EP0037026A1/de
Application granted granted Critical
Publication of EP0037026B1 publication Critical patent/EP0037026B1/de
Expired 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
    • C11D3/39—Organic or inorganic per-compounds
    • C11D3/3902—Organic or inorganic per-compounds combined with specific additives
    • C11D3/3905—Bleach activators or bleach catalysts
    • C11D3/3935—Bleach activators or bleach catalysts granulated, coated or protected
    • 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
    • C11D17/0039—Coated compositions or coated components in the compositions, (micro)capsules

Definitions

  • Bleach activators are taken to mean compounds which react in aqueous solutions containing hydrogen peroxide or perhydrates to form peracids which have a bleaching action.
  • the particularly effective bleach activators include N-acylated amines, amides and glycolurils, as described, for example, in DE-B-1 162 967, DE-B-1 291 317, DE-A-2 038 106 and DE-B-1 594 865 are known.
  • DE-B-1 162 967 proposes to provide these bleach activators with a water-soluble coating agent before further use, in particular before use in detergents and bleaching agents, wherein the coating agent can consist, for example, of carboxymethyl cellulose.
  • This coating agent dissolved in water, can be sprayed onto the activator in finely divided form, after which the coated material is dried.
  • the recommendation is made to granulate the activator before coating, but there are no indications as to how and with which granulation aids this should be carried out. If one works according to the specifications of DE-B-1 162 967 and sprays such a bleach activator, for example the tetraacetylethylene diamine, with an aqueous carboxymethyl cellulose solution in a granulator, considerable problems arise. This is because aqueous solutions containing more than 5% by weight of carboxymethyl cellulose can no longer be handled in industrial granulation processes because of their high viscosity and gel-like nature.
  • the same water-soluble salts which bind water of crystallization can also be used as granulation aids or the dry premixes can be sprayed with an aqueous solution of film-forming substances, such as cellulose derivatives or other water-soluble polymers of natural or synthetic origin, and simultaneously granulated.
  • film-forming substances such as cellulose derivatives or other water-soluble polymers of natural or synthetic origin
  • the invention is based on the object of developing a process for the production of readily pourable, uniformly coated and thus very stable bleach activator granules which have a substantially higher content, for example one of 90 percent by weight and more, of active substance.
  • the invention is a process for the preparation of storage-stable, easily soluble granules containing bleach activators, the implementation of which is carried out in a mixing and granulating device from 90 to 98 percent by weight (based on anhydrous constituents) a compound from the class of N-acylated amines, amides, diketopiperazines and glycolurils and having an average particle size of 0.01 to 0.8 mm powdery bleach activator with 10 to 2 percent by weight (based on anhydrous constituents) one from a compound of the Class of the water-soluble cellulose ether, starch and starch ether existing granulation aid in such a way that the powdery bleach activator in a 1st mixing stage with 50 to 100 percent by weight of the total to be used as pourable powder with an average grain size of 0.01 to 0.8 mm present granulating aid mixed ht, whereupon in a second mixing and granulation stage the mixture is moistened and granulated with water
  • Average grain size of 0.01 to 0.8 mm is understood to mean one in which more than 50 percent by weight, preferably at least 80 percent by weight of the particles, has a grain size of 0.01 to 0.8 mm and not more than 25 Weight percent, preferably not more than 10 weight percent, have a grain size of 0.8 to at most 1.6 mm and not more than 25 weight percent, preferably not more than 10 weight percent, have a grain size of less than 0.01 mm.
  • the grain size of the fine particles is not limited at the bottom, but dust-fine particles can also be present. The additional use of such dusty fractions, which are common in technical, unclassified powder products with a broad grain spectrum, represents an additional advantage of the process.
  • N-acylated amines, diamines, amides and glycolurils are suitable as bleach activators.
  • These are, for example, tetraacetylmethylene diamine, tetraacetylethylene diamine, diacetylaniline, diacetyl-p-toluidine, 1,3-diacetyl-5,5-dimethylhydantoin, tetraacetylglycoluril, tetrapropionylglycoluril, 1,4-diacetyl-2,5-diketopipe-rin -Diacetyl-3,6-dimethyl-2,5-diketopiperazine.
  • Tetraacetylethylenediamine is preferably used as the bleach activator.
  • the pulverulent bleach activator is mixed with part of the granulation aid, which is also in powder form.
  • the proportion of the granulation aid used in this stage is 50 to 100, preferably 80 to 95 percent by weight of the total granulation aid used. Accordingly, the total amount or only part of the granulation aid can be added in the 1st mixing stage.
  • the second variant, in which only part of the granulation aid is dry-mixed and the rest is introduced as a solution in the second stage, is the preferred method of operation.
  • the average grain size of the granulating aid is 0.01 to 0.8 mm according to the above definition.
  • the grain size of the powdered granulation aid is expediently as large or smaller than the grain size of the bleach activator.
  • the particle size of the granulating aid is advantageously 0.01 to 0.4 mm, the proportion of particles with a particle size of 0.4 to 1.6 mm 25 Weight percent and in particular 10 weight percent does not exceed.
  • the granulation aid consists of a water-soluble cellulose ether, water-soluble starch or a water-soluble starch ether.
  • cellulose ethers are methyl cellulose, ethyl cellulose, hydroxyethyl cellulose, methyl hydroxyethyl cellulose, methyl hydroxypropyl cellulose, carboxymethyl cellulose (as sodium salt) and methyl carboxymethyl cellulose (sodium salt).
  • depolymerized starch can be considered as starch.
  • Suitable starch ethers are, for example, carboxymethyl starch, hydroxyethyl starch and methyl starch. Sodium carboxymethyl cellulose has proven to be particularly suitable.
  • the two powdery components can be mixed in conventional batch-wise or continuously operating mixing devices which are generally equipped with rotating mixing elements. Depending on the effectiveness of the mixing device, the mixing times for a homogeneous mixture are generally between 30 seconds and 5 minutes.
  • powdery disintegrants which are customary in the tablet industry can be added, provided that the cellulose and starch ethers used do not already have a certain explosive effect.
  • Usable disintegrants are, for example, partially degraded starch, starch ether, polyvinyl polypyrrolidone, formaldehyde casein and swellable magnesium aluminosilicates (Veegum). The proportion of such disintegrants can be 0 to 2 percent by weight of the anhydrous granules.
  • the dry powder mixture is then moistened with water or an aqueous solution of the remaining granulating aid and granulated.
  • the mixer of the first mixing stage is also suitable for a granulation process, the mix can remain therein during the granulation process.
  • a pelletizer for example a pelletizing drum or onto a rotating pelletizer, and to carry out the pelletizing process there or to complete it.
  • part of the granulating liquid is expediently introduced into the mixer, for example in its end region, after the end of the first mixing stage, in order to moisten the material to be mixed and to counteract the formation of dust. For example, 5 to 70 percent of the granulation liquid is added during the post-mixing and 95 to 30 percent of the liquid during the subsequent granulation.
  • the granulating aid used in the second mixing and granulation stage is preferably used in a 0.5 to 5 percent by weight solution. Solutions with a higher concentration and containing up to 10 percent by weight of granulation aids are only recommended if they are sufficiently low-viscosity. If sodium carboxymethyl cellulose is used in a provenance as is usually used in detergents, the concentration is advantageously not more than 4 percent by weight.
  • the amount of granulating liquid applied is to be measured so that a moist one, not yet Granules tend to cake. This is achieved when the water content of the moist granules is between 10 and 35, preferably 15 to 25 percent by weight. Powder mixtures with a small particle size range and a higher proportion of powdered granulating aids can absorb larger amounts of granulating liquid than less fine-grained mixtures with a small part) of granulating aids.
  • a dye or a white pigment can be added to the dry powder mixture or the granulating liquid for coloring or to cover the inherent color of the raw materials.
  • a dye or a white pigment can be added to the dry powder mixture or the granulating liquid for coloring or to cover the inherent color of the raw materials.
  • generally 0.01 to 0.1 percent by weight, based on the finished product, of dye or pigment is sufficient.
  • the water content of the mixture is then reduced to less than 2, preferably less than 1 percent by weight.
  • the excess water can be removed by drying with the addition of heat, the temperature of the granules expediently not exceeding 100 ° C. and below the melting temperature of the bleach activator. Dryers that do not adversely change the granular structure of the product are suitable, for example tray, vacuum or fluidized bed dryers.
  • the dried granules should contain less than 2, preferably less than 1 percent by weight of water.
  • the granulate is intended for later use in detergents or is to be used for washing purposes in which a certain content of such salts does not interfere, which are usually used in detergents or in washing processes and which can crystallize with the absorption of water of crystallization, the The excess water is also removed by mixing the moist granules with such dehydrating, essentially water-free or low-water salts.
  • Such salts are sodium tripolyphosphate, sodium sulfate, sodium carbonate, sodium silicate and low-water sodium aluminosilicates capable of ion exchange and mixtures thereof.
  • the amount to be used depends on the water binding capacity of the salts concerned and the water content of the moist granules.
  • the mixing ratio of tripolyphosphate to moist granules is 1: 3 to 1: 1.5, in particular 1 2 to 1: 1.
  • Mixing can be carried out in conventional mixers or granulating devices, the process for producing the Wet granules used with mixing devices equipped mixing devices can be used immediately. In this way, simplified, in particular energy-saving, processing is possible since the necessary drying stage can be saved.
  • foam inhibitors are customary known defoamers, preferably polysiloxanes, and mixtures thereof with microfine silica. Examples of these are polydimethylsiloxane with a content of approximately 1-10 percent by weight of microfine silica.
  • the proportion of such polysiloxane defoamers can be 1 to 5 percent by weight, preferably 2 to 4 percent by weight, based on the finished granulate.
  • the defoamer can be added in the first mixing stage; however, the defoamer can also be dispersed in the granulating liquid which, in order to avoid segregation processes, should contain part of the granulating aid in this case.
  • the granules produced in the manner indicated have a favorable grain spectrum. Any existing flashover and fine fractions can be sieved and returned to the process after the coarse fractions have been ground.
  • the granules are easy to pour, non-sticky and, with due regard for the complete coating of the activator particles, very stable. Its high proportion of active substance, 90 and more percent by weight, is particularly advantageous. They can be used with advantage in detergents, bleaches, oxidizers and disinfectants and retain their good properties even when mixed with the active ingredients contained in these agents.
  • Tetraacetylethylenediamine with an average grain size of 0.01 to 0.8 mm was used as the bleach activator.
  • the grain fraction between 0.8 and 1.6 mm was 5 weight percent, the fraction under 0.01 mm 10 weight percent.
  • Example 42.0 kg of the powdery tetraacetylethylenediamine used in Example 1 were in a drum mixer equipped with rotating mixing elements (L ⁇ DIGE mixer) with 2.24 kg Na carboxymethyl cellulose of the grain size given in Example 1 (88.2 percent of the total amount used) for 2 minutes mixed and then sprayed with continuous mixing with a solution of 170.4 g Na carboxymethyl cellulose in 5.51 kg water (3% by weight) for the purpose of binding dust-like components.
  • the mix was transferred to a continuously operating mixing granulator (capacity 800 kg / h).
  • the outlet of this mixer was connected to the inlet via conveyor belts so that the product could be circulated.
  • the majority of the granules were dried in a vacuum drying device at 67 mbar (50 torr) over a period of 24 hours to a water content of less than 1 percent by weight.
  • 3 kg of the moist granules were dried in a fluidized bed dryer with air having an inlet temperature of 57 ° C. for 10 minutes to the same degree of drying. In both cases, the proportion of granules with a grain size of 0.5 to 1.5 mm was 65 percent by weight.
  • the rollover and fine fractions were sieved out and, after grinding the coarse fractions, entered into the subsequent granulation process.
  • the granules had the same advantageous properties as in Example 1 and had the following composition (anhydrous substance):
  • Example 2 In a continuous mixer, 95 parts by weight of the tetraacetylethylenediamine used in Example 1 were continuously mixed with 5 parts by weight of Na carboxymethyl cellulose. In the last third of the mixer, 10 parts by weight of a solution of 0.34 parts by weight of Na-carboxymethyl cellulose in 11 parts by weight of water (3 percent solution) were sprayed continuously onto the material to be mixed with dust by means of nozzles.
  • the moistened mixture passed into a continuously operating granulator (see Example 2), where it was sprayed and granulated with 10 parts by weight of a solution of 96.33% by weight of water, 3% by weight of Na-carboxymethyl cellulose and 0.67% by weight of dye (see Example 1) has been.
  • the goods came from the granulator onto a conveyor belt, from which a partial flow of 70 percent by weight was discharged and a partial stream of 30 percent by weight was returned to the granulator. After drying, the finished granules had the following composition:
  • 67 percent by weight of the granules had a particle size range between 0.5 and 1.5 mm.
  • the fine material sieved out after drying and the ground flap were also continuously returned to the granulator.
  • Example 4 was repeated, but the polysiloxane defoamer had been dispersed in the aqueous granulation liquid containing carboxymethyl cellulose. In terms of its properties, the product corresponded to that of Example 4.
  • Example 42.0 kg of the powdery tetraacetylethylenediamine used in Example 1 were in a drum mixer equipped with rotating mixing elements (L ⁇ DIGE mixer) with 2.24 kg Na carboxymethyl cellulose of the grain size given in Example 1 (88.2 percent of the total amount used) for 2 minutes mixed and then sprayed with continuous mixing with a solution of 170.4 g Na carboxymethyl cellulose in 5.51 kg water (3% by weight) for the purpose of binding dust-like components.
  • the mix was transferred to a continuously operating mixing granulator (capacity 800 kg / h).
  • the outlet of this mixer was connected to the inlet via conveyor belts so that the product could be circulated.
  • 4.3 kg of a 3 percent solution of Na-carboxymethyl cellulose (corresponding to 129 g) were fed in through the rotating shaft of the granulation mixer.

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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)
  • Cosmetics (AREA)
EP81102083A 1980-03-28 1981-03-20 Verfahren zur Herstellung eines lagerstabilen, leichtlöslichen Granulates mit einem Gehalt an Bleichaktivatoren Expired EP0037026B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT81102083T ATE14594T1 (de) 1980-03-28 1981-03-20 Verfahren zur herstellung eines lagerstabilen, leichtloeslichen granulates mit einem gehalt an bleichaktivatoren.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3011998 1980-03-28
DE3011998A DE3011998C2 (de) 1980-03-28 1980-03-28 Verfahren zur Herstellung eines lagerstabilen, leichtlöslichen Granulates mit einem Gehalt an Bleichaktivatoren

Publications (2)

Publication Number Publication Date
EP0037026A1 EP0037026A1 (de) 1981-10-07
EP0037026B1 true EP0037026B1 (de) 1985-07-31

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EP81102083A Expired EP0037026B1 (de) 1980-03-28 1981-03-20 Verfahren zur Herstellung eines lagerstabilen, leichtlöslichen Granulates mit einem Gehalt an Bleichaktivatoren

Country Status (5)

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US (1) US4372868A (enrdf_load_stackoverflow)
EP (1) EP0037026B1 (enrdf_load_stackoverflow)
JP (1) JPS56149500A (enrdf_load_stackoverflow)
AT (1) ATE14594T1 (enrdf_load_stackoverflow)
DE (2) DE3011998C2 (enrdf_load_stackoverflow)

Cited By (4)

* Cited by examiner, † Cited by third party
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US7279453B2 (en) 2001-02-22 2007-10-09 Henkel Kommanditgesellschaft Auf Aktien Foam regulating granulate
US7316995B2 (en) 2003-02-10 2008-01-08 Henkel Kommanditgesellschaft Auf Aktien Detergents or cleaning agents comprising a water-soluble building block system and a cellulose derivative with dirt dissolving properties
US7375072B2 (en) 2003-02-10 2008-05-20 Henkel Kommanditgesellschaft Auf Aktien Bleach-containing laundry detergents or cleaning compositions comprising water-soluble builder system and soil release-capable cellulose derivative
US7456143B2 (en) 2002-12-20 2008-11-25 Henkel Kommanditgesellschaft Auf Aktien (Henkel Kgaa) Bleach-containing washing or cleaning agents containing a sulfate/silicate coated percarbonate

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DE3504628A1 (de) * 1985-02-11 1986-08-14 Henkel KGaA, 4000 Düsseldorf Verfahren zur herstellung eines rieselfaehigen granulats
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DE60000022T2 (de) 1999-03-05 2002-03-14 Rohm And Haas Co., Philadelphia Verbesserte teilchenförmige Zusammensetzungen
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US7550156B2 (en) 2001-11-23 2009-06-23 Rohm And Haas Company Optimised pellet formulations
JP2006506516A (ja) * 2002-11-14 2006-02-23 ザ プロクター アンド ギャンブル カンパニー 封入ガラスケア活性塩を含有するすすぎ補助剤
ES2275207T5 (es) * 2003-02-10 2011-12-09 HENKEL AG & CO. KGAA Agente de lavado, que contiene agentes de blanqueo, con derivado de la celulosa con capacidad para el desprendimiento de la suciedad, con actividad sobre el algodón.
DE10351321A1 (de) * 2003-02-10 2004-08-26 Henkel Kgaa Verstärkung der Reinigungsleistung von Waschmitteln durch eine Kombination von Cellulosderivaten
JP2006517245A (ja) * 2003-02-10 2006-07-20 ヘンケル・コマンディットゲゼルシャフト・アウフ・アクチエン 発泡調節剤としてのセルロース誘導体の使用
EP1592764B1 (de) * 2003-02-10 2007-01-03 Henkel Kommanditgesellschaft auf Aktien Erhöhung der wasseraufnahmefähigkeit von textilien
ATE363525T1 (de) * 2003-02-10 2007-06-15 Henkel Kgaa Verstärkung der reinigungsleistung von waschmitteln durch cellulosederivat und hygroskopisches polymer
US20070244028A1 (en) * 2004-05-17 2007-10-18 Henkel Kgaa Washing Agent With Bleach Boosting Transition Metal Complex Optionally Generated in Situ
DE102005026544A1 (de) 2005-06-08 2006-12-14 Henkel Kgaa Verstärkung der Reinigungsleistung von Waschmitteln durch Polymer
DE102005026522B4 (de) 2005-06-08 2007-04-05 Henkel Kgaa Verstärkung der Reinigungsleistung von Waschmitteln durch Polymer
US7709437B2 (en) * 2006-04-27 2010-05-04 Oci Chemical Corp. Co-granulates of bleach activator-peroxide compounds
GB0710559D0 (en) * 2007-06-02 2007-07-11 Reckitt Benckiser Nv Composition
EP2103678A1 (en) * 2008-03-18 2009-09-23 The Procter and Gamble Company Detergent composition comprising a co-polyester of dicarboxylic acids and diols
EP2103675A1 (en) * 2008-03-18 2009-09-23 The Procter and Gamble Company Detergent composition comprising cellulosic polymer
DE102018209002A1 (de) * 2018-06-07 2019-12-12 Henkel Ag & Co. Kgaa Waschmittelzusammensetzung mit Fließgrenze

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL130608C (enrdf_load_stackoverflow) * 1959-06-19
DE2048331A1 (de) * 1970-10-01 1972-04-06 Henkel & Cie GmbH, 4000 Dusseldorf Feste, pulverförmige bis kornige Mittel zur Herstellung von kaltwirksamen Bleich flotten, insbesondere von kaltwirksamen blei chenden Waschlaugen, und Verfahren zur Her stellung dieser Mittel
US4009113A (en) * 1971-04-30 1977-02-22 Lever Brothers Company Protection of materials
AT326611B (de) * 1972-07-31 1975-12-29 Henkel & Cie Gmbh Als bestandteil von pulverförmigen wasch- und bleichmitteln geeignetes bleichhilfsmittel

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7279453B2 (en) 2001-02-22 2007-10-09 Henkel Kommanditgesellschaft Auf Aktien Foam regulating granulate
US7456143B2 (en) 2002-12-20 2008-11-25 Henkel Kommanditgesellschaft Auf Aktien (Henkel Kgaa) Bleach-containing washing or cleaning agents containing a sulfate/silicate coated percarbonate
US7316995B2 (en) 2003-02-10 2008-01-08 Henkel Kommanditgesellschaft Auf Aktien Detergents or cleaning agents comprising a water-soluble building block system and a cellulose derivative with dirt dissolving properties
US7375072B2 (en) 2003-02-10 2008-05-20 Henkel Kommanditgesellschaft Auf Aktien Bleach-containing laundry detergents or cleaning compositions comprising water-soluble builder system and soil release-capable cellulose derivative

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DE3171538D1 (en) 1985-09-05
EP0037026A1 (de) 1981-10-07
DE3011998A1 (de) 1981-10-08
DE3011998C2 (de) 1982-06-16
US4372868A (en) 1983-02-08
JPS56149500A (en) 1981-11-19
JPH0340080B2 (enrdf_load_stackoverflow) 1991-06-17
ATE14594T1 (de) 1985-08-15

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