EP0570881B1 - Procédé de fabrication de granulés pauvres en poussière - Google Patents

Procédé de fabrication de granulés pauvres en poussière Download PDF

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Publication number
EP0570881B1
EP0570881B1 EP93108002A EP93108002A EP0570881B1 EP 0570881 B1 EP0570881 B1 EP 0570881B1 EP 93108002 A EP93108002 A EP 93108002A EP 93108002 A EP93108002 A EP 93108002A EP 0570881 B1 EP0570881 B1 EP 0570881B1
Authority
EP
European Patent Office
Prior art keywords
aqueous solution
granules
hydrate
suspension
temperature
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
EP93108002A
Other languages
German (de)
English (en)
Other versions
EP0570881A2 (fr
EP0570881A3 (en
Inventor
Frank Dr. Jaekel
Gerd Dr. Reinhardt
Gerhard Nöltner
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.)
Clariant Produkte Deutschland GmbH
Original Assignee
Clariant GmbH
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
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Application filed by Clariant GmbH filed Critical Clariant GmbH
Publication of EP0570881A2 publication Critical patent/EP0570881A2/fr
Publication of EP0570881A3 publication Critical patent/EP0570881A3/de
Application granted granted Critical
Publication of EP0570881B1 publication Critical patent/EP0570881B1/fr
Anticipated expiration legal-status Critical
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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
    • C11D3/3907—Organic compounds
    • 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
    • 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
    • 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
    • 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
    • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
    • 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
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/39—Organic or inorganic per-compounds
    • C11D3/3945—Organic per-compounds

Definitions

  • Granulated and therefore free-flowing bulk goods are used in numerous Production areas, e.g. in the detergent industry in increasing Dimensions used and replace the powdery, poorly flowing products.
  • EP-A-376 360 describes a process for producing solid, free-flowing, bleach-active granules containing at least one water-insoluble peroxyacid contain hydrate-forming inorganic material, known, the manufactured granules due to low tendency to dust formation ("dust-free") should honor.
  • the bleach-active granules are to be produced by mixing solid peracid such as diperoxydodecanoic acid (DPDA) with anhydrous hydrate-forming inorganic material, such as sodium sulfate, take place, the Water content of the mixture below the maximum hydrate water content of the hydrate-forming inorganic material must lie and the temperature during of the mixing process less than the hydration temperature of the must be hydrate-forming inorganic material.
  • DPDA diperoxydodecanoic acid
  • the object of the present invention is an inexpensive and energy-saving process for the production of low-dust granules, especially those that contain temperature-sensitive substances to deliver.
  • the invention relates to a method for producing low-dust Granules, characterized in that on a particulate starting material an aqueous solution or suspension of a hydrate-forming compound is applied, the particulate starting material during the Applying the aqueous solution or suspension a temperature below the Has transition temperature of the hydrate-forming compound and the aqueous Solution or suspension a temperature above the transition temperature has, then or simultaneously granulated and the granules obtained optionally dried.
  • Granular constituents which are suitable for the production of granules or the granules themselves are used as particulate starting materials for the process according to the invention.
  • the terms granulate components and granules are to be understood broadly. It has been shown that the process according to the invention is not limited to certain granule components or granules, but rather that all granule components and granules can be used as particulate starting materials to which an aqueous solution of a hydrate-forming compound can be applied.
  • Granules or granule constituents such as are known from the detergent, paint or pharmaceutical industry are preferably used.
  • the method according to the invention is particularly preferred below with the described granules and granulate components.
  • temperature-sensitive substances examples include enzymes such as lipases and amylases Suitable bleaching agents and bleach activators are mentioned in EP-A-376 360.
  • Suitable agglomerates are in EP-A-376 360 called, preferably agglomerates consisting of a Peracid and an organic, water-insoluble compound, such as lauric acid, Find use.
  • Suitable bleach activators are preferably tetraacetylethylene diamine (TAED), Tetraacetylmethylene diamine, tetraacetylglycol unil (TAGU), Diacetyldioxohexahydrotriazine (DADHT), pentaacetylglucose (PAG), Acetoxibenzenesulfonate Sodium, Nonanoyloxibenzenesulfonate Sodium (NOBS) and benzoyloxybenzenesulfonate sodium (BOBS).
  • TAED tetraacetylethylene diamine
  • TGU tetraacetylmethylene diamine
  • TAGU tetraacetylglycol unil
  • DADHT Diacetyldioxohexahydrotriazine
  • PAG pentaacetylglucose
  • Acetoxibenzenesulfonate Sodium Nonanoyloxibenzene
  • the polymer Film formers are preferred in aqueous solution on the particulate Starting materials applied. Your concentration in the solution is 5 to 50% by weight, preferably 10 to 30% by weight.
  • the share of film-forming Substance on the granules is 1 to 15, preferably 3 to 12 wt .-%.
  • the granules may be specific contains additional components.
  • additional components examples of this are chelating systems, Dyes and agents for regulating the pH. It is known that metals are able to catalyze organic or inorganic per-compounds decompose. To overcome this problem, the granules can up to 3% by weight of a chelating agent can be added.
  • Preferred compounds are inorganic or organic phosphates or phosphonates or Aminomethylene carboxylic acids. Examples of this are Ethylenediaminetetramethylenephosphonic or carboxylic acids or Diethylenetriaminepentamethylenephosphonic acid or its salts.
  • Means of Adjusting the pH will change or maintain the pH value used within the granules. Examples include citric acid, Fatty acid or succinic acid or salts such as silicates, phosphates or Sodium bisulfate.
  • Granules are used as starting materials and to reduce these granules with the aid of the process according to the invention Granules are processed further. Have the finished granules used generally the typical granulate structure as described above has been.
  • transition temperature is to be understood as the temperature at which the hydrate-forming compound releases or takes up the bound water of crystallization. If sodium sulfate is used as the hydrate-forming compound, the transition temperature is 32.5 ° C. Below this transition temperature, the sodium sulfate forms a decahydrate with the water of crystallization. Above this temperature, most of the crystal water is released again.
  • Sodium acetate, sodium carbonate, zinc nitrate, sodium sulfate, magnesium sulfate, magnesium nitrate, lithium bromide, sodium phosphate, sodium hydrogen phosphate or mixtures thereof are preferably used.
  • Suitable apparatus for the production of the low-dust granules are, for example, mixers, extruders or pelletizing machines.
  • Suitable mixers are those which can be operated batchwise or continuously and which permit mixing under high shear forces. Examples of such batch mixers are "Dry Dispenser” ® (Baker, Perkins, Peterborough, GB) "Diosna-Pharmamix” ® (Diercks, Osnabschreib, DE) "Matrix” ® (Fielder Ltd., Eastlake, GB) “Baumeister” ® (Ruberg, Paderborn, DE) “Ruberg high-performance mixer” ® (Ruberg, Paderborn, DE) "MTI, type EM” ® (MTL, Detmold, DE) and “Eirich Mixers” ® (Eirich Hardheim, DE).
  • Lödige Ploughshare Mixer ® (Lödige Maschinenfabrik, Paderborn) "Lödige Recycler CB” ® (from Lödige Maschinenfabrik, Paderborn).
  • An example of a continuously operated mixer is the “Konax continuous mixer” ® (Ruberg, Paderborn, DE).
  • extruders are “Alma” ®, Unica “®,” Xtruder “®, and” Werner Pfleiderer “®.
  • common pelleting machines are the products from Simon Heesen or the Maromarizer from Russel Finings Ltd., London, GB.
  • Other apparatuses that can be used to produce the low-dust granules by the process according to the invention are fluidized bed mixers in which different temperature levels can be set.
  • the particulate starting material is placed in a suitable apparatus, preferably given a fluidized bed granulator.
  • the particulate starting material consists of the individual Granulate components, so the water-insoluble advantageously Components, such as active substance, optionally with the addition of part of the hydrate-forming compound, presented in the apparatus and the device remaining water-soluble components with the solution of hydrate-forming Connection applied.
  • active substance such as peracid
  • hydrate-forming compound in a fluidized bed granulator in one Weight ratio of 3 to 8, preferably 4 to 7 to one submitted.
  • Finished Granules are usually made without further additives and without pretreatment Work steps introduced into the apparatus.
  • the temperature of the granules or granulate components set so that they are below the transition temperature of the used hydrate-forming compound.
  • the following temperature specifications refer to the use of Sodium sulfate as a hydrate-forming compound with a transition temperature 32.5 ° C. With regard to this particular transition temperature specified temperature ranges can be used when using other hydrate-forming Connections are transmitted analogously.
  • a moderate air flow flows through with a temperature up to 37 ° C, preferably 22 to 35 ° C, the granule components or granules.
  • the air temperature should be chosen so that a strong thermal Load on the feed of the fluidized bed granulator is avoided and can are also above 37 ° C. It is essential that the particulate Starting materials have a temperature below 32.5 ° C, preferably up to 20 ° C.
  • aqueous, preferably saturated, aqueous sodium sulfate solution is applied to the granules or granule constituents, the temperature of the solution being above 32.5 ° C., preferably up to 40 ° C.
  • the application is usually carried out by spraying, but, depending on the apparatus, can also be carried out by dropping, blasting, addition via a distributor rake, addition via a distributor weir or other measures known to the person skilled in the art.
  • the aqueous solution can contain additional components such as water-soluble surfactants and / or film-forming coating substances.
  • composition of the aqueous solution is preferred 90-98% by weight of hydrate-forming compound, for example anhydrous sodium sulfate, 2 - 10% by weight of coating substance, such as polyacrylic acid and 0-10% by weight of surfactant, such as ®Hostapur SAS.
  • hydrate-forming compound for example anhydrous sodium sulfate
  • coating substance such as polyacrylic acid
  • surfactant such as ®Hostapur SAS.
  • the concentration of the aqueous solution is usually between 30-70% by weight, preferably 50-60% by weight. It has been shown that it is advantageous to choose the concentration of the solution so that the weight ratio of particulate starting materials to solution is approximately the same. It is also possible to use supersaturated solutions in which the solids are finely dispersed or suspensions of poorly soluble or insoluble solids.
  • the aqueous solution or suspension can also be water-miscible, organic Contain solvents such as alcohols, ethers or esters, these being organic Solvents must not react with the raw materials used.
  • the temperature of the particulate is Starting materials below the transition temperature of the hydrate-forming Connection and the temperature of the solution above the Conversion temperature, taking care that the temperature of the sprayed particulate starting materials always below the Transformation temperature.
  • Starting materials it is advisable to while spraying granulate. But it is also conceivable that the solution partially or completely is sprayed on and then the granulation takes place. It has shown, that the process of granulation with improved properties of the used granules in terms of mechanical strength and thus low-dust granules.
  • the amount of solution is preferably granted so that it primarily arises Wet granules between 8 and 20 wt .-% water.
  • Suitable processes can be used for spraying and granulating Connect drying steps, if necessary, in the same apparatus, however can also be carried out using other gentle methods.
  • the additional drying is only necessary if a particularly low one Water content of the granules according to the invention is desired.
  • the method according to the invention has been shown that by the selected Temperature ratio between the particulate starting materials and the Solution, after spraying part of the hydrate-forming compound crystallized out and a heat of crystallization released Drying effect of the granules is achieved.
  • the low-dust granules produced in this way have one Granule size distribution in the range from 0.1 to 5 mm, preferably 0.4 to 3 mm.
  • Granules produced subsequently inert coatings of various Kind be it in the form of closed films or in the form of deposited powder, to apply, but it is just an advantage of the present invention without one get along such measure.
  • a particularly preferred area of application for the granules is the bleaching of textiles in Connection with a washing treatment.
  • the granules can be used for this Purpose in a uniform form, i.e. can be used without further admixtures, however, they are preferably used as sprinkled mixtures with others Active substances that are necessary for textile treatment are made up.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Detergent Compositions (AREA)
  • Glanulating (AREA)
  • Medicinal Preparation (AREA)
  • Manufacturing Of Micro-Capsules (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Claims (8)

  1. Procédé de préparation de granulés pauvres en poussière, caractérisé en ce qu'on applique sur une matière de départ particulaire une solution ou une suspension aqueuse d'un composé formant des hydrates, la matière de départ particuliare ayant au cours de l'application de la solution ou suspension aqueuse, une température inéfrieure à la température de transition du composé formant des hydrates et la solution aqueuse ayant une température supérieure à la température de transition, on granule ensuite ou simultanément, et éventuellement on sèche le granulé obtenu.
  2. Procédé selon la revendication 1, caractérisé en ce qu'on utilise comme matière de départ particulaire des granulé ou leurs composants.
  3. Procédé selon la revendication 2, caractérisé en ce que on utilise des granulés à activité de blanchiment ou leurs constituants.
  4. Procédé selon la revendication 1, caractérisé en ce qu'on utilise comme composé formant des hydrates le bromure de lithium, l'acétate de sodium, le carbonate de sodium, le phosphate de sodium, l'hydrogénophosphate de sodium, le sulfate de magnésium, le nitrate de magnésium, le nitrate de zinc, de préférence le sulfate de sodium ou leurs mélanges.
  5. Procédé selon la revendication 1, caractérisé en ce que la solution ou la suspension aqueuse contient des substances d'enrobage hydrosolubles et éventuellement des agents de surface.
  6. Procédé selon la revendication 1, caractérisé en ce que la solution ou la suspension aqueuse contient des solvants organiques miscibles à l'eau, de préférence des alcools, des éthers et/ou des esters.
  7. Procédé selon la revendication 1, caractérisé en ce que la solution ou la suspension aqueuse présente une concentration de 30 à 70 % en poids, de préférence de 50 à 60 % en poids.
  8. Procédé selon une des revendications 1 à 7, caractérisé en ce l'application de la solution aqueuse est réalisée par coulée goutte à goutte, par jet, par addition à travers une grille de distributeur, par additition au moyen d'un déversoir-distributeur ou de préférence par pulvérisation.
EP93108002A 1992-05-19 1993-05-17 Procédé de fabrication de granulés pauvres en poussière Expired - Lifetime EP0570881B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4216517 1992-05-19
DE4216517 1992-05-19

Publications (3)

Publication Number Publication Date
EP0570881A2 EP0570881A2 (fr) 1993-11-24
EP0570881A3 EP0570881A3 (en) 1994-08-24
EP0570881B1 true EP0570881B1 (fr) 1998-11-25

Family

ID=6459235

Family Applications (1)

Application Number Title Priority Date Filing Date
EP93108002A Expired - Lifetime EP0570881B1 (fr) 1992-05-19 1993-05-17 Procédé de fabrication de granulés pauvres en poussière

Country Status (8)

Country Link
US (1) US6066365A (fr)
EP (1) EP0570881B1 (fr)
JP (1) JPH0691153A (fr)
AT (1) ATE173757T1 (fr)
CA (1) CA2096480A1 (fr)
DE (1) DE59309147D1 (fr)
DK (1) DK0570881T3 (fr)
ES (1) ES2124752T3 (fr)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19611014A1 (de) * 1996-03-21 1997-09-25 Henkel Kgaa Verfahren zur Herstellung rieselfähiger Wasch- oder Reinigungsmittel
US6596683B1 (en) 1998-12-22 2003-07-22 The Procter & Gamble Company Process for preparing a granular detergent composition
ATE409219T1 (de) * 1998-12-22 2008-10-15 Procter & Gamble Verfahren zur herstellung einer körnigen reinigungsmittelzusammensetzung
KR100366556B1 (ko) 2000-04-26 2003-01-09 동양화학공업주식회사 세제용 입상 코티드 과탄산나트륨과 이의 제조방법
DE10221742A1 (de) * 2002-05-16 2003-12-04 Henkel Kgaa Gerüststoffgranulate
DE10361100A1 (de) † 2003-06-13 2005-01-05 Henkel Kgaa Lagerstabile Kapseln auf Basis von Peroxycarbonsäuren
JP4326418B2 (ja) 2004-07-16 2009-09-09 株式会社東京精密 フィルム剥離方法およびフィルム剥離装置
US20160213079A1 (en) * 2015-01-22 2016-07-28 Fred R. Amsler, JR. Quick release suspenders

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4126573A (en) * 1976-08-27 1978-11-21 The Procter & Gamble Company Peroxyacid bleach compositions having increased solubility
US4091544A (en) * 1977-02-11 1978-05-30 The Procter & Gamble Company Drying process
US4497757A (en) * 1983-01-31 1985-02-05 The Procter & Gamble Company Energy efficient hydration process
US4867895A (en) * 1987-01-13 1989-09-19 The Clorox Company Timed-release bleach coated with an amine with reduced dye damage
GB8810630D0 (en) * 1988-05-05 1988-06-08 Unilever Plc Process for preparing bodies containing peroxyacid & compositions comprising said bodies
US5049298A (en) * 1988-11-25 1991-09-17 Akzo Nv Process for the preparation of bleaching granules

Also Published As

Publication number Publication date
DE59309147D1 (de) 1999-01-07
CA2096480A1 (fr) 1993-11-20
DK0570881T3 (da) 1999-08-09
ES2124752T3 (es) 1999-02-16
EP0570881A2 (fr) 1993-11-24
US6066365A (en) 2000-05-23
ATE173757T1 (de) 1998-12-15
JPH0691153A (ja) 1994-04-05
EP0570881A3 (en) 1994-08-24

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