WO1992004398A1 - Granular agglomerate and process for its manufacture - Google Patents

Granular agglomerate and process for its manufacture Download PDF

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Publication number
WO1992004398A1
WO1992004398A1 PCT/EP1991/001574 EP9101574W WO9204398A1 WO 1992004398 A1 WO1992004398 A1 WO 1992004398A1 EP 9101574 W EP9101574 W EP 9101574W WO 9204398 A1 WO9204398 A1 WO 9204398A1
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WO
WIPO (PCT)
Prior art keywords
gelatin
extruder
agglomerate
particles
gelatine
Prior art date
Application number
PCT/EP1991/001574
Other languages
German (de)
French (fr)
Inventor
Peter Koepff
Helmuth Stahl
Eberhard Dick
Brigitte Uhe
Klaus BRÄUMER
Original Assignee
Deutsche Gelatine-Fabriken Stoess Ag
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 Deutsche Gelatine-Fabriken Stoess Ag filed Critical Deutsche Gelatine-Fabriken Stoess Ag
Publication of WO1992004398A1 publication Critical patent/WO1992004398A1/en

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Classifications

    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
    • A23G3/00—Sweetmeats; Confectionery; Marzipan; Coated or filled products
    • A23G3/34—Sweetmeats, confectionery or marzipan; Processes for the preparation thereof
    • A23G3/50—Sweetmeats, confectionery or marzipan; Processes for the preparation thereof characterised by shape, structure or physical form, e.g. products with supported structure
    • A23G3/54—Composite products, e.g. layered, coated, filled
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
    • A23G3/00—Sweetmeats; Confectionery; Marzipan; Coated or filled products
    • A23G3/34—Sweetmeats, confectionery or marzipan; Processes for the preparation thereof
    • A23G3/346—Finished or semi-finished products in the form of powders, paste or liquids
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/70—Fixation, conservation, or encapsulation of flavouring agents
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00—Shaping or working of foodstuffs characterised by the products
    • A23P10/20—Agglomerating; Granulating; Tabletting
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00—Shaping or working of foodstuffs characterised by the products
    • A23P10/20—Agglomerating; Granulating; Tabletting
    • A23P10/25—Agglomeration or granulation by extrusion or by pressing, e.g. through small holes, through sieves or between surfaces
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
    • C09B67/0092—Dyes in solid form
    • C09B67/0095—Process features in the making of granulates
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/0097—Dye preparations of special physical nature; Tablets, films, extrusion, microcapsules, sheets, pads, bags with dyes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09H—PREPARATION OF GLUE OR GELATINE
    • C09H9/00—Drying of glue or gelatine
    • C09H9/04—Drying of glue or gelatine in the form of granules, e.g. beads
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
    • A23G2200/00—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF containing organic compounds, e.g. synthetic flavouring agents
    • A23G2200/10—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF containing organic compounds, e.g. synthetic flavouring agents containing amino-acids, proteins, e.g. gelatine, peptides, polypeptides
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
    • A23G2220/00—Products with special structure
    • A23G2220/20—Products with special structure with a composite structure, e.g. laminated products, coated products, microstructures, e.g. with encapsulated ingredients

Definitions

  • the invention relates to a method according to the preamble of patent claim 1.
  • FIG. 1 schematically examples of the inner
  • the agglomerate according to the invention is not thermoplastic and contains water-containing gelatin as a binder, which firmly binds the individual solid particles to one another. It is important to use the smallest possible amount of gelatin so that the properties of the gelatin do not adversely affect the properties of the solid particles which are in the foreground.
  • the binding capacity is still sufficient if the vol .-% of gelatin is smaller than the vol .-% of pores in the agglomerate grains, so that the gelatin does not completely fill the pores.
  • the amount of water attributable to the gelatin contained in the granular agglomerate should correspond to the natural water content of gelatin. This depends on the prevailing air humidity ("equilibrium moisture"). It is usually between about 10 and 12% by weight, but can be up to about 16% by weight at high atmospheric humidity.
  • the rheological properties of the agglomerates correspond to those of the starting materials. This means that in the case of non-thermoplastic solid starting materials, the agglomerates produced therefrom also have these properties to have .
  • agglomerate according to the invention allows rapid dispersion and dissolution, for example in the case of so-called “instant products”, that separation processes, for example in the case of agglomerated medicines and animal feed, can be avoided and that appropriate additives can also be used in the Agglomera ⁇ tion can achieve a depot effect, especially with fertilizers and pesticides.
  • the granular agglomerates according to the invention are particularly advantageously produced with the aid of extruders, in particular screw extruders, in a single work cycle.
  • the ability of the gelatin to dissolve in water is used. Any viscosity can be set by means of temperature and amount of solvent. Solvents other than water are also suitable, for example glycerol or mixtures of glycerol and water.
  • the extruders used to produce the agglomerate according to the invention are preferably co-rotating twin-screw extruders with a relatively long process length.
  • the long process length of the twin-screw extruder is necessary because all of the work processes essential for the production of the agglomerate take place in the extruder: the binder (gelatin, gelatin hydrolyzate or a mixture of gelatin and gelatin hydrolyzate) is dissolved in the solvent, heated, Additives are added that become agglomerating substances added and incorporated homogeneously.
  • a twin screw extruder is advantageous because it can be used to achieve particularly good homogenization. Homogenization is achieved on the one hand by kneading in the gap between the two screws and the use of special mixing parts, on the other hand, with the double screws rotating in the same direction, no complete chamber shut-off is achieved, so that the mass can flow back around the two screws . Both effects guarantee a sufficient mixing of the binder with the solvent and incorporation of the solid particles and homogenization of the highly viscous pseudoplastic mass to be extruded.
  • the binder e.g. B. gelatin
  • the liquid solvent e.g. B. water.
  • D is the inside diameter of the screw extruder.
  • the dusty solids to be compacted are added.
  • the addition can take place, for example, via a stuffing screw known per se.
  • the viscosity of the mass is greatly increased by adding the substances. Depending on the particle size and amount, the viscosity can increase to a multiple of the low-viscosity gelatin solution.
  • FIG. 1 shows schematically a first typical form of the internal or microscopic structure of an agglomerate according to the invention.
  • Individual particles 1 of a solid for example a dust-like pigment, are (due to the processing described in the extruder, in particular screw extruder) essentially completely surrounded by a thin gelatin skin, which binds the individual particles firmly to one another or agglomerates due to their adhesive force. Here remain between the individual Particles 1 gelatin-free pores 3.
  • the agglomerate shown schematically in FIG. 2 differs from that according to FIG. 1 essentially in that the gelatin 3 contains the particles 1 - z. B. because of poor wettability - is not completely encased, but is only present in some areas on the circumference of the particles and there is an "adhesion" of the individual particles.
  • the relative amount of gelatin is so small that the pores between the particles 1 are not completely filled with gelatin 2.
  • 300 g / h gelatin with a water content of about 11% by weight corresponding to the equilibrium moisture content are metered continuously into a first area (feed zone) of a twin-screw extruder of 48 D.
  • 300 g / h of water are continuously added at another metering point via a valve. The temperature in this area rises steadily from 25 to 80 ° C. over its length.
  • the temperature is increased to 95 ° C.
  • the gelatin is completely and homogeneously dissolved in this area with the help of the double screw.
  • the granular agglomerate obtained in this way is very strong and the individual grains have a smooth surface.
  • Example 2 The procedure is as in Example 1. However, 500 g / h of gelatin are metered in and 250 g / h of water are added via a valve. 2 kg / h of sugar are fed in via a stuffing screw. The pseudoplastic mass obtained in this way is extruded at a pressure of 20 bar. The extruded strands are dried and granulated into a granular agglomerate.
  • the agglomerate is suitable, for example, as a compound for use in the confectionery industry.
  • Example 4 The procedure is as in Example 1. However, 250 g / h of gelatin hydrolyzate are used when the same amount of water is added. 2 kg / h of a mixture of sugar, citric acid, yellow and red color and orange aroma are added via the stuffing screw. There is no separation of the individual components, but rather a granular agglomerate of these components results, which can be fed to further processing in the confectionery industry.
  • Example 4
  • Example 2 The procedure is as in Example 2. However, 125 g / h gelatin hydrolyzate and 125 g / h gelatin are used. The water addition is unchanged. 250 g / h of herbicides are then continuously mixed into the solution thus obtained.
  • Additives in particular plasticizers, emulsifiers, wetting agents and / or non-stick agents, can be added to the gelatin fed into the screw extruder in a known manner.
  • Suitable plasticizers are, for example, glycerol or sorbitol, for example amine oxide or Na lauryl sulfate are suitable as wetting agents.
  • Mg stearate or montan waxes have proven to be useful as anti-adhesive agents.
  • the amount of water in which the gelatin is dissolved can be between 50 and 300% by weight based on the weight of the gelatin.
  • the screw extruder is operated at temperatures between 30 and 140 ° C., preferably at temperatures between 30 and 100 ° C.
  • the increased pressure prevailing in the extruder can be between 5 and 100 bar.

Abstract

Described is a granular agglomerate consisting of dispersed particles of at least one solid and a binder holding the particles together in the agglomerate, pores remaining open between the particles. The agglomerate has the following characteristics: the binder is hydrous gelatine; the gelatine content, expressed as a percentage by volume, is lower than the pore content so that the gelatine does not completely fill the pores; and the amount of water contained, originating from the water content of the gelatine, is less than 2 % by wt. of the total weight of the agglomerate. The agglomerate is produced in an extruder, in particular a screw-feed extruder, to which the required amounts of gelatine and solids are supplied. A highly viscous composition is extruded as a continuous extrusion, dried to the required low water content and the extrusion granulated to give a granular agglomerate.

Description

Körniges Agglomerat und Verfahren zu seiner Herstellung Granular agglomerate and process for its production
Die Erfindung betrifft ein Verfahren nach dem Oberbegriff des Patentanspruchs 1.The invention relates to a method according to the preamble of patent claim 1.
Ein solches Verfahren ist aus der JP 59-042 846 A (Der- went-Referat Nr. 84-097 618/16) bekannt.Such a method is known from JP 59-042 846 A (Derating Section No. 84-097 618/16).
Dabei gelangt jedoch kein Extruder zur Anwendung, in dem zunächst eine niedrigviskose Gelatinelösung hergestellt wird, mit der anschließend sofort und ebenfalls im Extru¬ der die dispersen Partikel überzogen werden.However, no extruder is used here, in which a low-viscosity gelatin solution is first produced, with which the disperse particles are then coated immediately and also in the extruder.
Es ist Aufgabe der Erfindung, ein gattungsgemäßes Verfah¬ ren so zu verbessern, daß das Agglomerat rasch und einfach hergestellt werden kann.It is an object of the invention to improve a generic method in such a way that the agglomerate can be produced quickly and easily.
Die Aufgabe wird erfindungsgemäß durch die kennzeichnenden Merkmale des Patentanspruchs 1 gelöst.The object is achieved by the characterizing features of claim 1.
Es ist ungewöhnlich, eine niedrigviskose Lösung unmittel¬ bar in einem Extruder herzustellen. Normalerweise werden in einem Extruder nur hochviskose Massen verarbeitet. Ebenfalls ungewöhnlich ist es, die zu agglomerierenden Partikel unmittelbar in dem Extruder, in dem die niedrig¬ viskose Lösung hergestellt wird, mit dieser Lösung zu überziehen und zu agglomerieren. Die nachstehende Beschreibung bevorzugter Ausführungsfor¬ men der Erfindung dient im Zusammenhang mit einigen Bei¬ spielen und einer Zeichnung der weiteren Erläuterung. Auf der Zeichnung zeigen:It is unusual to produce a low-viscosity solution directly in an extruder. Normally, only highly viscous masses are processed in an extruder. It is also unusual to coat and agglomerate the particles to be agglomerated with this solution directly in the extruder in which the low-viscosity solution is produced. The following description of preferred embodiments of the invention serves in connection with some examples and a drawing for further explanation. Show on the drawing:
Figur 1 und 2 schematisch Beispiele für den innerenFigures 1 and 2 schematically examples of the inner
Aufbau eines erfindungsgemäßen Agglo- merates.Structure of an agglomerate according to the invention.
Das erfindungsgemäße Agglomerat ist nicht thermoplastisch und enthält als Bindemittel wasserhaltige Gelatine, welche die einzelnen Feststoffpartikel fest aneinander bindet. Dabei ist es wichtig, eine möglichst geringe Menge an Ge¬ latine einzusetzen, so daß die Eigensphaften der Gelatine die an sich im Vordergrund stehenden Eigenschaften der Feststoffpartikel nicht nachteilig beeinträchtigen. Das Bindevermögen ist auch dann noch ausreichend, wenn der Vol.-%-Anteil an Gelatine kleiner als der Vol.-%-Anteil der Poren in den Agglomeratkörnern ist, so daß die Gelati¬ ne die Poren nicht voll ausfüllt. Weiterhin soll die in dem körnigen Agglomerat enthaltene auf die Gelatine zu¬ rückgehende Wassermenge dem natürlichen Wassergehalt von Gelatine entsprechen. Dieser ist von der herrschenden Luftfeuchtigkeit abhängig ( "Gleichgewichstfeuchte" ) . Er liegt normalerweise zwischen etwa 10 und 12 Gew.-%, kann jedoch bei hoher Luftfeuchtigkeit bis zu etwa 16 Gew.-% betragen.The agglomerate according to the invention is not thermoplastic and contains water-containing gelatin as a binder, which firmly binds the individual solid particles to one another. It is important to use the smallest possible amount of gelatin so that the properties of the gelatin do not adversely affect the properties of the solid particles which are in the foreground. The binding capacity is still sufficient if the vol .-% of gelatin is smaller than the vol .-% of pores in the agglomerate grains, so that the gelatin does not completely fill the pores. Furthermore, the amount of water attributable to the gelatin contained in the granular agglomerate should correspond to the natural water content of gelatin. This depends on the prevailing air humidity ("equilibrium moisture"). It is usually between about 10 and 12% by weight, but can be up to about 16% by weight at high atmospheric humidity.
Die rheologischen Eigenschaften der Agglomerate entspre¬ chen denen der Ausgangsstoffe. Dies bedeutet, daß bei nicht thermoplastischen festen Ausgangsstoffen auch die daraus hergestellten Agglomerate diese Eigenschaften haben .The rheological properties of the agglomerates correspond to those of the starting materials. This means that in the case of non-thermoplastic solid starting materials, the agglomerates produced therefrom also have these properties to have .
Von Vorteil ist es bei dem erfindungsgemäßen Agglomerat, daß es ein schnelles Dispergieren und Auflösen, beispiels¬ weise bei sogenannten "Instantprodukten" gestattet, daß EntmischungsVorgänge, beispielsweise bei agglomerierten Arznei- und Futtermitteln, vermieden werden können und daß sich auch durch entsprechende Zusätze bei der Agglomera¬ tion eine Depotwirkung, insbesondere bei Düngemitteln und Pflanzenschutzmitteln erreichen läßt.It is advantageous with the agglomerate according to the invention that it allows rapid dispersion and dissolution, for example in the case of so-called “instant products”, that separation processes, for example in the case of agglomerated medicines and animal feed, can be avoided and that appropriate additives can also be used in the Agglomera¬ tion can achieve a depot effect, especially with fertilizers and pesticides.
Besonders vorteilhaft werden die erfindungsgemäßen körni¬ gen Agglomerate mit Hilfe von Extrudern, insbesondere Schneckenextrudern in einem einzigen Arbeitsdurchlauf her¬ gestellt.The granular agglomerates according to the invention are particularly advantageously produced with the aid of extruders, in particular screw extruders, in a single work cycle.
Dabei wird die Fähigkeit der Gelatine ausgenutzt, sich in Wasser zu lösen. Mittels Temperatur und Lösungsmittelmenge läßt sich jede beliebige Viskosität einstellen. Auch ande¬ re Lösungsmittel als Wasser kommen in Frage, beispielswei¬ se Glycerin oder Mischungen von Glycerin und Wasser.The ability of the gelatin to dissolve in water is used. Any viscosity can be set by means of temperature and amount of solvent. Solvents other than water are also suitable, for example glycerol or mixtures of glycerol and water.
Bei den zur Herstellung des erfindungsgemäßen Agglomerats verwendeten Extrudern handelt es sich vorzugsweise um gleichläufige DoppelSchneckenextruder von relativ großer Verfahrenslänge. Die große Verfahrenslänge des Doppel- schneckenextruders ist erforderlich, da im Extruder alle für die Herstellung des Agglomerats wesentlichen Arbeits¬ prozesse ablaufen: Das Bindemittel (Gelatine, Gelatinehy- drolysat oder eine Mischung aus Gelatine und Gelatinehy- drolysat) wird im Lösungsmittel gelöst, erwärmt, Additive werden beigemischt, die zu agglomerierenden Stoffe werden zugegeben und homogen eingearbeitet.The extruders used to produce the agglomerate according to the invention are preferably co-rotating twin-screw extruders with a relatively long process length. The long process length of the twin-screw extruder is necessary because all of the work processes essential for the production of the agglomerate take place in the extruder: the binder (gelatin, gelatin hydrolyzate or a mixture of gelatin and gelatin hydrolyzate) is dissolved in the solvent, heated, Additives are added that become agglomerating substances added and incorporated homogeneously.
Ein DoppelSchneckenextruder ist deshalb von Vorteil, weil sich mit seiner Hilfe eine besonders gute Homogenisierung erzielen läßt. Die Homogenisierung wird zum einen durch das Kneten im Spalt zwischen den beiden Schnecken und den Einsatz spezieller Mischteile erreicht, zum anderen wird aber bei den in gleicher Richtung umlaufenden Doppel- Schnecken keine vollständige KammerabSperrung erreicht, so daß die Masse um die beiden Schnecken herum zurückströmen kann. Beide Effekte garantieren eine ausreichende Vermi¬ schung des Bindemittels mit dem Lösungsmittel sowie Einar¬ beitung der Feststoffpartikel und Homogenisierung der zu extrudierenden, hochviskosen pseudoplastischen Masse.A twin screw extruder is advantageous because it can be used to achieve particularly good homogenization. Homogenization is achieved on the one hand by kneading in the gap between the two screws and the use of special mixing parts, on the other hand, with the double screws rotating in the same direction, no complete chamber shut-off is achieved, so that the mass can flow back around the two screws . Both effects guarantee a sufficient mixing of the binder with the solvent and incorporation of the solid particles and homogenization of the highly viscous pseudoplastic mass to be extruded.
In einem ersten Bereich des Schneckenextruders wird das Bindemittel, z. B. Gelatine, an einer ersten Dosierstation zugegeben. Über eine weitere Dosierstation erfolgt die Zu¬ gabe des flüssigen Lösungsmittels, z. B. Wasser. Bei¬ spielsweise über eine Länge von 15 D wird unter kontinu¬ ierlicher Temperaturerhöhung und unter steigendem Druck gemischt. In einem Endabschnitt dieses ersten Bereiches, der eine Länge von 20 bis 25 D haben kann, erfolgt die weitere Auflösung der Gelatine und die Homogenisierung der Lösung. ( "D" ist der Innendurchmesser des Schneckenextru¬ ders. )In a first area of the screw extruder, the binder, e.g. B. gelatin, added at a first metering station. The liquid solvent, eg. B. water. For example, over a length of 15 D, the mixture is mixed while continuously increasing the temperature and under increasing pressure. In an end section of this first area, which can have a length of 20 to 25 D, the gelatin is further dissolved and the solution is homogenized. ("D" is the inside diameter of the screw extruder.)
In einem anschließenden zweiten Bereich, der eine Länge von 13 bis 18 D haben kann, erfolgt die Zugabe der zu kom- paktierenden staubförmigen Feststoffe. Die Zugabe kann beispielsweise über eine an sich bekannte Stopfschnecke erfolgen. Durch die Zugabe der Stoffe wird die Viskosität der Masse stark erhöht. Je nach Teilchengröße und Menge kann die Viskosität auf ein Vielfaches der niedrigviskosen Gelati¬ nelösung ansteigen.In a subsequent second area, which can have a length of 13 to 18 D, the dusty solids to be compacted are added. The addition can take place, for example, via a stuffing screw known per se. The viscosity of the mass is greatly increased by adding the substances. Depending on the particle size and amount, the viscosity can increase to a multiple of the low-viscosity gelatin solution.
Diese nunmehr hochviskose, "pseudoplastische" Masse wird durch eine Strangdüse gepreßt und als Endlosstrang ausge¬ formt, wobei gleichzeitig auch mehrere Stränge aus mehre¬ ren Düsenö fnungen austreten können. Die Stränge werden z. B. mit einem Förderband abgezogen. Gleichzeitig wird durch Verdampfung des Lösungsmittels, beispielsweise im Warm¬ luftstrom, der Strang auf Gleichgewichtsfeuchte getrocknet so daß die nun wieder auf ihren natürlichen Wassergehalt zurückgeführte Gelatine nur einen geringen Volumanteil der Poren im Inneren des Agglomerats ausfüllt.This now highly viscous, "pseudoplastic" mass is pressed through a strand die and shaped as an endless strand, wherein at the same time several strands can emerge from several nozzle openings. The strands are z. B. deducted with a conveyor belt. At the same time, the strand is dried to equilibrium moisture by evaporation of the solvent, for example in a hot air stream, so that the gelatin, which is now returned to its natural water content, only fills a small volume of the pores in the interior of the agglomerate.
Aufgrund der starken Klebekraft der Gelatine erreicht man, daß bei nur geringen Mengen an Gelatine nach Austreiben des Lösungsmittels ein noch fest zusammenhängender Strang vorliegt. Der Strang wird anschließend mit einem an sich bekannten Granulator auf beliebige Korngröße geschnitten, so daß sich als Endprodukt ein körniges Agglomerat ergibt.Due to the strong adhesive strength of the gelatin, it is achieved that with only small amounts of gelatin, after the solvent has been expelled, a strand which is still firmly connected is present. The strand is then cut to any grain size using a known granulator, so that the end product is a granular agglomerate.
Die Figur 1 zeigt schematisch eine erste typische Form des inneren oder mikroskopischen Aufbaus eines erfindungsgemä¬ ßen Agglomerates. Einzelne Partikel 1 eines Feststoffes, beispielsweise eines staubförmigen Pigments, sind (auf¬ grund der beschriebenen Verarbeitung im Extruder, insbe¬ sondere Schneckenextruder) im wesentlichen vollständig von einer dünnen Gelatinehaut umgeben, welche aufgrund ihrer Klebekraft die einzelnen Partikel fest aneinander bindet oder agglomeriert. Dabei verbleiben zwischen den einzelnen Partikeln 1 gelatinefreie Poren 3.FIG. 1 shows schematically a first typical form of the internal or microscopic structure of an agglomerate according to the invention. Individual particles 1 of a solid, for example a dust-like pigment, are (due to the processing described in the extruder, in particular screw extruder) essentially completely surrounded by a thin gelatin skin, which binds the individual particles firmly to one another or agglomerates due to their adhesive force. Here remain between the individual Particles 1 gelatin-free pores 3.
Das in Figur 2 schematisch dargestellte Agglomerat unter¬ scheidet sich von demjenigen nach Figur 1 im wesentlichen dadurch, daß die Gelatine 3 die Partikel 1 - z. B. wegen schlechter Benetzbarkeit - nicht vollständig umhüllt, son¬ dern nur bereichsweise am Umfang der Partikel vorhanden ist und dort eine "Verklebung" der einzelnen Partikel be¬ wirkt. Die relative Gelatinemenge ist so gering, daß die Poren zwischen den Partikeln 1 nicht voll mit Gelatine 2 gefüllt sind.The agglomerate shown schematically in FIG. 2 differs from that according to FIG. 1 essentially in that the gelatin 3 contains the particles 1 - z. B. because of poor wettability - is not completely encased, but is only present in some areas on the circumference of the particles and there is an "adhesion" of the individual particles. The relative amount of gelatin is so small that the pores between the particles 1 are not completely filled with gelatin 2.
Beispiel 1example 1
In einen ersten Bereich (Einzugszone) eines Doppelschnek- kenextruders von 48 D werden kontinuierlich 300 g/h Gela¬ tine mit einem der Gleichgewichtsfeuchte entsprechenden Wassergehalt von etwa 11 Gew.-% eindosiert. In dem glei¬ chen Bereich werden an einer anderen Dosierstelle über ein Ventil kontinuierlich 300 g/h Wasser zugegeben. Die Tempe¬ ratur in diesem Bereich steigt über dessen Länge hinweg stetig von 25 auf 80° C.300 g / h gelatin with a water content of about 11% by weight corresponding to the equilibrium moisture content are metered continuously into a first area (feed zone) of a twin-screw extruder of 48 D. In the same area, 300 g / h of water are continuously added at another metering point via a valve. The temperature in this area rises steadily from 25 to 80 ° C. over its length.
In einem anschließenden Bereich des Extruders wird die Temperatur auf 95° C gesteigert. Die Gelatine wird in die¬ sem Bereich mit Hilfe der DoppelSchnecke vollständig und homogen gelöst.In a subsequent area of the extruder, the temperature is increased to 95 ° C. The gelatin is completely and homogeneously dissolved in this area with the help of the double screw.
In einem anschließenden Bereich werden über eine Stopf¬ schnecke 2,7 kg/h staubförmiger Farbstoff zudosiert und homogen in die Gelatinelösung eingemischt. Die nunmehr hochviskose, pseudoplastische Masse wird unter einem Druck von 40 bar und bei einer Temperatur von 95° C aus einer Strangdüse mit vier Öffnungen extrudiert. Die Stränge wer¬ den während des Abzuges im Luftstrom getrocknet und an¬ schließend granuliert.In a subsequent area, 2.7 kg / h of dust-like dye are metered in via a stuffing screw and mixed homogeneously into the gelatin solution. The now highly viscous, pseudoplastic mass is under pressure of 40 bar and at a temperature of 95 ° C extruded from a strand nozzle with four openings. The strands are dried in a stream of air during removal and then granulated.
Das so erhaltene körnige Agglomerat ist sehr fest und die einzelnen Körner haben eine glatte Oberfläche.The granular agglomerate obtained in this way is very strong and the individual grains have a smooth surface.
Beispiel 2Example 2
Man verfährt wie in Beispiel 1. Es werden jedoch 500 g/h an Gelatine eindosiert und über ein Ventil werden 250 g/h an Wasser zugegeben. Über eine StopfSchnecke werden 2 kg/h an Zucker zugeführt. Die so gewonnene pseudoplastische Masse wird mit einem Druck von 20 bar extrudiert. Die ex- trudierten Stränge werden getrocknet und zu einem körnigen Agglomerat granuliert. Das Agglomerat eignet sich bei¬ spielsweise als Compound zur Verwendung in der Süßwarenin¬ dustrie.The procedure is as in Example 1. However, 500 g / h of gelatin are metered in and 250 g / h of water are added via a valve. 2 kg / h of sugar are fed in via a stuffing screw. The pseudoplastic mass obtained in this way is extruded at a pressure of 20 bar. The extruded strands are dried and granulated into a granular agglomerate. The agglomerate is suitable, for example, as a compound for use in the confectionery industry.
Beispiel 3Example 3
Man verfährt wie in Beispiel 1. Es werden jedoch 250 g/h an Gelatinehydrolysat bei Zugabe der gleichen Wassermenge verwendet. Über die StopfSchnecke werden 2 kg/h einer Mischung aus Zucker, Zitronensäure, gelber und roter Farbe sowie Orangenaroma zudosiert. Es tritt keine Entmischung der Einzelkomponenten ein, sondern es ergibt sich vielmehr ein körniges Agglomerat aus diesen Komponenten, welches einer Weiterverarbeitung in der Süßwarenindustrie zuge¬ führt werden kann. Beispiel 4The procedure is as in Example 1. However, 250 g / h of gelatin hydrolyzate are used when the same amount of water is added. 2 kg / h of a mixture of sugar, citric acid, yellow and red color and orange aroma are added via the stuffing screw. There is no separation of the individual components, but rather a granular agglomerate of these components results, which can be fed to further processing in the confectionery industry. Example 4
Man verfährt wie in Beispiel 2. Es werden jedoch 125 g/h Gelatinehydrolysat und 125 g/h Gelatine verwendet. Die Wasserzugabe ist unverändert. In die so gewonnene Lösung werden anschließend kontinuierlich 250 g/h an Herbiziden eingemischt.The procedure is as in Example 2. However, 125 g / h gelatin hydrolyzate and 125 g / h gelatin are used. The water addition is unchanged. 250 g / h of herbicides are then continuously mixed into the solution thus obtained.
Der in den Schneckenextruder eingegebenen Gelatine lassen sich in bekannter Weise jeweils Additive, insbesondere Weichmacher, Emulgatoren, Benetzungsmittel und/ oder Anti- haftmittel beimischen. Geeignete Weichmacher sind bei¬ spielsweise Glycerin oder Sorbit, als Benetzungsmittel kommen beispielsweise Aminoxid oder Na-Lauryl-Sulfat in Frage. Als Antihaftmittel haben sich Mg-Stearat oder Mon¬ tanwachse als brauchbar erwiesen.Additives, in particular plasticizers, emulsifiers, wetting agents and / or non-stick agents, can be added to the gelatin fed into the screw extruder in a known manner. Suitable plasticizers are, for example, glycerol or sorbitol, for example amine oxide or Na lauryl sulfate are suitable as wetting agents. Mg stearate or montan waxes have proven to be useful as anti-adhesive agents.
Generell kann die Wassermenge, in welcher die Gelatine gelöst wird, zwischen 50 und 300 Gew.-% bezogen auf das Gelatinegewicht liegen. Im Schneckenextruder arbeitet man bei Temperaturen zwischen 30 und 140° C, vorzugsweise bei Temperaturen zwischen 30 und 100° C. Der im Extruder herr¬ schende, erhöhte Druck kann zwischen 5 und 100 bar liegen. In general, the amount of water in which the gelatin is dissolved can be between 50 and 300% by weight based on the weight of the gelatin. The screw extruder is operated at temperatures between 30 and 140 ° C., preferably at temperatures between 30 and 100 ° C. The increased pressure prevailing in the extruder can be between 5 and 100 bar.

Claims

P a t e n t a n s p r ü c h eP a t e n t a n s r u c h e
Verfahren zum Herstellen eines körnigen Agglomerats bestehend aus dispersen Partikeln wenigstens eines Feststoffes und aus diese Partikel agglomerierender Gelatine, wobei zwischen den Partikeln Poren frei bleiben, gekennzeichnet durch folgende Schritte:Process for producing a granular agglomerate consisting of disperse particles of at least one solid and of these particles agglomerating gelatin, wherein pores remain free between the particles, characterized by the following steps:
A. Man stellt in einem ersten Bereich eines Extru¬ ders, insbesondere Schneckenextruders durch konti¬ nuierliche Zugabe von Gelatine und Lösungsmittel, insbesondere Wasser, unter Erwärmung eine niedrig¬ viskose Gelatinelösung her;A. In a first area of an extruder, in particular a screw extruder, a low-viscosity gelatin solution is produced by heating by continuously adding gelatin and solvent, in particular water;
B. man bringt in einen anschließenden Bereich des Ex¬ truders unter fortgesetzter Erwärmung wenigstens einen zu agglomerierenden Feststoff in die nie¬ drigviskose Gelatinelösung ein und erzeugt durch homogenes Vermischen des Feststoffes mit der Lö¬ sung und unter Druck eine hochviskose pseudoplas¬ tische Masse;B. at least one solid to be agglomerated is introduced into the low-viscosity gelatin solution in a subsequent area of the extruder with continued heating, and a highly viscous pseudoplastic mass is produced by homogeneously mixing the solid with the solution and under pressure;
C. man extrudiert diese hochviskose pseudoplastische Masse aus dem Extruder durch eine Düse in Form ei¬ nes Stranges;C. this highly viscous pseudoplastic mass is extruded from the extruder through a nozzle in the form of a strand;
D. man trocknet den Strang vor und granuliert ihn zu dem körnigen Agglomerat und E. man trocknet schließlich das Granulat auf Gleich¬ gewichtsfeuchte.D. the strand is pre-dried and granulated into the granular agglomerate and E. Finally, the granules are dried to equilibrium moisture.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß man die Gelatine durch Gelatinehydrolysat oder eine Mischung aus Gelatine und Gelatinehydrolysat er¬ setzt.2. The method according to claim 1, characterized in that the gelatin is replaced by gelatin hydrolyzate or a mixture of gelatin and gelatin hydrolyzate.
3. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß man die Gelatine mit Weichmachern, Emulgatoren, Benetzungsmitteln und/oder Antihaftmitteln versetzt.3. The method according to claim 1, characterized in that the gelatin is mixed with plasticizers, emulsifiers, wetting agents and / or non-stick agents.
4. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß man mit Bezug auf die Gelatine zwischen 50 und 300 Gew.-% an Wasser als Lösungsmittel zugibt.4. The method according to claim 1, characterized in that with respect to the gelatin between 50 and 300 wt .-% of water as a solvent is added.
5. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß man das Lösen und Vermischen im Extruder bei Tem¬ peraturen zwischen 30 und 100° C vornimmt.5. The method according to claim 1, characterized in that one carries out the dissolving and mixing in the extruder at temperatures between 30 and 100 ° C.
6. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß man das Lösen und Vermischen im Extruder bei Drücken zwischen 5 und 100 bar vornimmt.6. The method according to claim 1, characterized in that one carries out the dissolving and mixing in the extruder at pressures between 5 and 100 bar.
7. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß der Strang im Luftstrom getrocknet wird. 7. The method according to claim 1, characterized in that the strand is dried in an air stream.
PCT/EP1991/001574 1990-09-03 1991-08-20 Granular agglomerate and process for its manufacture WO1992004398A1 (en)

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