WO2004028675A1 - Dispositif melangeur et couvercle, leur utilisation et procede de modification et de derivation d'hydrates de carbone - Google Patents

Dispositif melangeur et couvercle, leur utilisation et procede de modification et de derivation d'hydrates de carbone Download PDF

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Publication number
WO2004028675A1
WO2004028675A1 PCT/AT2003/000261 AT0300261W WO2004028675A1 WO 2004028675 A1 WO2004028675 A1 WO 2004028675A1 AT 0300261 W AT0300261 W AT 0300261W WO 2004028675 A1 WO2004028675 A1 WO 2004028675A1
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WO
WIPO (PCT)
Prior art keywords
mixing device
carbohydrates
mixing
discharge
mixer
Prior art date
Application number
PCT/AT2003/000261
Other languages
German (de)
English (en)
Inventor
Dietmar Grüll
Ondrej Mikla
Marnik Wastyn
Original Assignee
Südzucker Aktiengesellschaft Mannheim/Ochsenfurt
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 Südzucker Aktiengesellschaft Mannheim/Ochsenfurt filed Critical Südzucker Aktiengesellschaft Mannheim/Ochsenfurt
Priority to EP03797967A priority Critical patent/EP1542791A1/fr
Priority to AU2003260156A priority patent/AU2003260156A1/en
Publication of WO2004028675A1 publication Critical patent/WO2004028675A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
    • C08B37/0087—Glucomannans or galactomannans; Tara or tara gum, i.e. D-mannose and D-galactose units, e.g. from Cesalpinia spinosa; Tamarind gum, i.e. D-galactose, D-glucose and D-xylose units, e.g. from Tamarindus indica; Gum Arabic, i.e. L-arabinose, L-rhamnose, D-galactose and D-glucuronic acid units, e.g. from Acacia Senegal or Acacia Seyal; Derivatives thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F31/00—Mixers with shaking, oscillating, or vibrating mechanisms
    • B01F31/40—Mixers with shaking, oscillating, or vibrating mechanisms with an axially oscillating rotary stirrer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/70—Mixers specially adapted for working at sub- or super-atmospheric pressure, e.g. combined with de-foaming
    • B01F33/71—Mixers specially adapted for working at sub- or super-atmospheric pressure, e.g. combined with de-foaming working at super-atmospheric pressure, e.g. in pressurised vessels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/75—Discharge mechanisms
    • B01F35/754—Discharge mechanisms characterised by the means for discharging the components from the mixer
    • B01F35/75425—Discharge mechanisms characterised by the means for discharging the components from the mixer using pistons or plungers
    • B01F35/754251—Discharge mechanisms characterised by the means for discharging the components from the mixer using pistons or plungers reciprocating in the mixing receptacle
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/75—Discharge mechanisms
    • B01F35/754—Discharge mechanisms characterised by the means for discharging the components from the mixer
    • B01F35/75455—Discharge mechanisms characterised by the means for discharging the components from the mixer using a rotary discharge means, e.g. a screw beneath the receptacle
    • B01F35/754551—Discharge mechanisms characterised by the means for discharging the components from the mixer using a rotary discharge means, e.g. a screw beneath the receptacle using helical screws
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B17/00—Apparatus for esterification or etherification of cellulose
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B30/00—Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
    • C08B30/12—Degraded, destructured or non-chemically modified starch, e.g. mechanically, enzymatically or by irradiation; Bleaching of starch
    • C08B30/16—Apparatus therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
    • B01F2101/06—Mixing of food ingredients
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
    • B01F2101/21—Mixing of ingredients for cosmetic or perfume compositions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
    • B01F2101/22—Mixing of ingredients for pharmaceutical or medical compositions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2215/00—Auxiliary or complementary information in relation with mixing
    • B01F2215/04—Technical information in relation with mixing
    • B01F2215/0413—Numerical information
    • B01F2215/0418—Geometrical information
    • B01F2215/0431—Numerical size values, e.g. diameter of a hole or conduit, area, volume, length, width, or ratios thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2215/00—Auxiliary or complementary information in relation with mixing
    • B01F2215/04—Technical information in relation with mixing
    • B01F2215/0413—Numerical information
    • B01F2215/0436—Operational information
    • B01F2215/0463—Numerical power values
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2215/00—Auxiliary or complementary information in relation with mixing
    • B01F2215/04—Technical information in relation with mixing
    • B01F2215/0413—Numerical information
    • B01F2215/0436—Operational information
    • B01F2215/0468—Numerical pressure values
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2215/00—Auxiliary or complementary information in relation with mixing
    • B01F2215/04—Technical information in relation with mixing
    • B01F2215/0413—Numerical information
    • B01F2215/0436—Operational information
    • B01F2215/0481—Numerical speed values

Definitions

  • the invention relates to the use of a mixing device for the physical modification and / or chemical derivatization of carbohydrates, proteins and mixtures thereof.
  • the invention relates to a mixing device for the physical modification and / or chemical derivatization of carbohydrates, proteins and mixtures thereof with a discharge device.
  • the invention further relates to the use of the mixing device with the discharge device for the physical modification and / or chemical derivatization of carbohydrates, proteins and mixtures thereof.
  • the invention further relates to a method for the physical modification and / or chemical derivatization of carbohydrates, proteins and mixtures thereof.
  • a discontinuous process is known from US Pat. No. 3,527,606, in which starch in particle form is suspended in a thickener with a stirring agent for mechanical treatment of the material to be modified by means of centrifugal force.
  • the starch particles are flung against the wall of the thickening cooker in order to achieve heat transfer between the particles and the wall for modification.
  • extruder Another device that is also used and common in many other fields of application is the extruder, in which the material to be treated is subjected to a continuously working process.
  • the extruder housing can be equipped with a cooling or heating jacket, as a result of which a constant process temperature is maintained.
  • the retention times of the material to be treated in the extruder housing depend on the length of the extruder screw, but this often turns out to be disadvantageous because the retention times are limited thereby. Negative results are also due to the permanent forced movement of the material and the operating conditions in the extruder housing, which can only be changed slightly. When using this process for the production of plasticized starch, the production of highly viscous products is not guaranteed, since the starch molecules in the extruder are exposed to excessive thermal and mechanical stress and are degraded in the process.
  • a similar continuous starch modification method is described in EP 710 670 B1, the starch to be modified being in a continuous powder stream via an inlet opening into a closed cylindrical one Turboreactor housing is introduced with a cooling or heating jacket.
  • a paddle wheel the blades of which are arranged helically on the shaft, is used for centrifuging and the simultaneous advancement of the reaction material in the direction of an outlet opening.
  • Any drying can be achieved by means of a turbo dryer, which is arranged at the outlet opening of the turbo-reactor and has a similar structure to the turbo-reactor.
  • the end product produced by this process consists of a dry product, in particular a dry powder.
  • the object of the present invention is now to improve and simplify the treatment of carbohydrates, proteins and / or mixtures thereof, so that on the one hand a wide range of starting materials can be used and on the other hand diverse. e.g. viscous properties of the end product are obtained, the above-mentioned problems being avoided.
  • a mixing device comprising a mixing chamber with a movable mixer and a sealingly guided press plate, as described in AT 382 090 B, for the physical modification and / or chemical derivatization of high molecular weight and / or low molecular weight carbohydrates, proteins and / or mixtures thereof is used.
  • This device known per se - below also referred to as a press mixer or press mixer - for physical modification and / or chemical derivatization corresponds to a combination of the continuous and discontinuous (in batches) operations described above.
  • the modified carbohydrates, proteins and / or mixtures thereof or end products produced in this way are advantageous as functional raw materials and / or additives in areas of application which range from the food, cosmetics and pharmaceuticals industry, dishwashing detergents industry to the textile industry and paper industry to the construction and plastics industries.
  • the products provided according to the present invention can be used for the production of insulating, insulating and building materials, such as composite materials, ceramic products, chipboard, plasterboard, packaging materials.
  • Such a wide range of applications for such products is based on the fact that the mixing system used according to the invention makes it easy to individually control and control the operating conditions within the mixing device.
  • the mixing device u used according to the invention includes a sealable seal Mixing chamber or a reactor vessel with a mixing tool and a sealingly guided axially movable base plate, which functions as a press plate.
  • the required reaction conditions of the material to be converted can be set individually using the rotatable and, independently of this, oscillatable mixer.
  • the applied mechanical energy of the mixing tool heats, for example, powdery starch to such an extent that it converts to a plasticized mass with a natural water content.
  • An additional admixture of solvent, such as when using conventional devices, is therefore no longer necessary, and a subsequent drying process, as with the autoclave process, is unnecessary.
  • the individual adaptation of the operating conditions of the mixing device used according to the invention also includes working under vacuum, as a result of which treatment of inulin, for example, delivers particularly good results.
  • the reactions can also be influenced using the press plate for applying pressure.
  • hydrophobizing substances have a lubricating effect during their treatment and the use of conventional devices, in particular the extruder, all too often leads to considerable problems of consistency in the product to be treated.
  • high-molecular carbohydrates there is a wide range of, among other things, high-molecular carbohydrates. Viscous properties can be achieved by means of the mixing device used according to the invention if native starch and / or degraded and / or already physically and / or chemically modified derivatives thereof are used. In addition to unchanged, high-molecular carbohydrates, carbohydrates that have already been treated can also be used as the starting material, as a result of which the properties of these materials can be further improved or changed with the aid of the above-mentioned mixing device, and therefore a wide range of uses of such treated products is also created.
  • native starch as a starting product is particularly favorable when the native starch is made from starch from corn, waxy maize, amylomais, potatoes, amylose-free potatoes, sweet potatoes, wheat, wax wheat, roe, barley, oats, aranthanth, tapioca, cassava, rice, Wax rice, peas and millet is selected.
  • These easily available substances are not only inexpensive, but also have extremely good properties with regard to their treatment or further processing and their industrial applicability.
  • the starting materials include sugars and sugar alcohols.
  • such materials can be optimally processed into viscous end products.
  • they are also a good starting material in the chemical industry, in particular in the food and pharmaceutical industries, but also as a starting product for polymers, raw materials for washing, plasticizers, emulsifiers and the like.
  • sugar selected from sucrose, maltose, fructose, as well as glucose and palatinose®, is used.
  • hydrogenated derivatives such as e.g. Palatinit®, sorbitol, mannitol, xylitol, maltitol, lactitol and other sugars and sugar alcohols listed in Ulimann's Encyclopedia of Industrial Chemistry, 4th edition, volume 24, pages 749-793 can be used.
  • vegetable proteins can be mentioned as proteins, such as naturally occur together with the abovementioned starting products, but also animal protein, such as casein.
  • the use of the mixing plant used gives particularly good results if it is used for the production of carbohydrates, starting from mono- and / or disaccharides and / or their sugar alcohols. More precisely, the production of carbohydrates is the re-synthesis of carbohydrates, and the polycondensation which is generally used to build up new carbohydrates is very efficient with the aid of the device according to the invention. It is clear that monomers or mixtures of the individual monomers (mono-, disaccharides and their sugar alcohols) are used, which are press-mixed in the mixing plant. In this way, for example, sugar substitutes, which are used for the production of low-calorie foods, such as Polydextrose®, can be produced quickly and without great effort.
  • Another object of the invention is to provide an improved mixing device for the physical modification and / or chemical derivatization of high molecular and / or low molecular weight carbohydrates, proteins and / or mixtures thereof.
  • This is a modified mixing device, which has been described in part above, whereby this concept for the treatment of the starting materials mentioned is to be optimized.
  • the mixing device in question has at least one mixer and at least one sealing plate which is guided in a sealing manner in a mixing chamber which can be sealed by means of a cover.
  • a discharge device with a feed part and with a discharge part is provided.
  • a discharge device is provided, but is not further specified. It is known that a moderate and gentle process is required for the discharge of modified or plasticized carbohydrates, so that the end product to be obtained can be removed from the mixing plant with satisfactory consistency and viscous properties. Especially during the discharge process, there is often the problem of insufficient, reduced expansion or inflation of the plasticized end products, since the treated material is discharged or squeezed out of the conversion device too quickly and / or inconsistently, so that the gelatinized material is inhomogeneous, i.e. only on its surface, expanding. Such a misconduct of implementation and discharge can even lead to the expanded discharge product developing a hardness comparable to that of glass and thus being a completely unusable product.
  • the high-pressure-resistant sealing device described in EP 916 877 A2 for the homogenization or dispersion of sensitive liquid phases or solids has a high-pressure-resistant mixing container with an axially displaceably mounted rotor as a mixing tool and a plate-shaped element or pressure plate mounted above it.
  • the circumference of the pressure plate is equipped with a plurality of sealing elements. The mix to be treated is when the rotor and the plate-shaped element received and sheared in a gap between the rotor and the plate-shaped element.
  • the shear also acts on the material and, on the other hand, the sealing elements ensure that the mixing container is securely sealed against atmospheric influences, but it does not offer a solution Disadvantages mentioned above during the discharge process of the treated material.
  • a discharge device is not specified here either.
  • the discharge device of a mixing device comprises forced conveying, such as a screw conveyor, preferably a single-screw extruder, and is preferably arranged on the cover of the mixing chamber, other arrangements, horizontally or vertically along the reaction container, are also conceivable , Cell wheel locks, spindle pumps such as Mohno pumps, gear pumps or the like can also be used as forced conveyors. Forced conveyance as a discharge device creates an extended combination of the continuous and discontinuous treatment concept of Starting products for the preservation of broadband viscous properties, since the pressure conditions applied to the positively conveyed material can be controlled.
  • the unlimited control of the retention time and the application of pressure allows the discharge product to be fully expanded in order to achieve optimal, high-quality and, above all, homogeneous material properties.
  • the continuous movement of the discharge material creates a removal in defined, determinable batches, so that the discharge product can be removed from the mixing device as a sales manufacturer, but also as an easily processable strand.
  • the discharge device it is also conceivable for the discharge device to be heatable or coolable, so that an additional temperature effect or temperature maintenance on the positively conveyed material is possible.
  • a vacuum connection is provided in the area of the forced conveyance of the discharge device, so that negative pressure conditions within the discharge device and in the reaction container are permitted.
  • the arrangement of the discharge device is disadvantageously designed such that it, preferably the extruder, is guided across the cover.
  • Such a design of the cover which corresponds to the lid of the mixing container, provides simple, direct access to the discharge device from the mixing chamber and thus at the same time a discharge or squeezing out of the material from the mixing chamber, which is forced but very controlled. takes place.
  • connection is realized through at least one opening in the cover of the mixing chamber. More than one connection can also be provided, as a result of which the material to be mixed from the mixing chamber is taken up unhindered by the discharge device via the feed section of the forced conveying means, in particular of the extruder.
  • This opening it is advantageous if it has a slit-like, has an elongated shape, but circular, rectangular, elliptical or similarly shaped openings can also be provided.
  • connection opening of the discharge device is arranged off-center in the cover. Such an eccentric arrangement ensures that the material to be discharged reaches the feed section of the extruder optimally.
  • the mixer of the mixing device and the sealing plate of the mixing chamber which is guided in a sealing manner can be displaced in the direction of the cover.
  • the converted material is thereby moved in the direction of the cover or cover by the oscillating and rotatable mixing tool and is forced into the connection opening, which is connected to the discharge device, by the press plate, which is also sealingly guided in the direction of the cover.
  • the mixer strips the material at the opening edges of the connection or its border, so that all of the material is removed from the mixing chamber.
  • the arrangement of this connection opening can also be formed in the center or in the edge area, although complete emptying of the mixing chamber must be ensured, so that no remaining, unused mix remains in the mixing chamber.
  • This inventive feature of the preferred axial displaceability of the mixer and the plate also serves not only for the maximum but metered discharge of the material to be mixed from the mixing chamber, but also for a thorough emptying thereof.
  • the mixer and the sealing plate of the mixing chamber which is guided in a sealing manner, can be moved close to the connection opening of the discharge device.
  • valves it is advantageous if the cover of the mixing chamber is provided with valves.
  • pressure conditions such as vacuum
  • loading, ventilation, gassing or evacuation for example in the form of a safety valve
  • This also includes the possibility of metering in gaseous or liquid components or reagents or else removing undesirable, in particular volatile, by-products from the reaction of the treated starting products arise.
  • Equipping the cover with valves has the particular advantage that continuous working conditions can be achieved; ie the valves are used for loading the chamber with fresh raw material and / or additional other components, in order to be removed immediately after sufficient, controlled conversion of the mixed material by means of the discharge device, with a refill with fresh raw material being able to take place via the valves at the same time without to stop operating the system.
  • the valves are kept closed until the activated discharge process of the mixture is completed via the discharge device, so that the mixing chamber and the discharge extruder are completely emptied.
  • the system can then be subjected to cleaning by introducing cleaning agent (or water) into the mixing chamber, for example via valves or closable through openings, and keeping the system in operation until the interior of the system has been completely emptied.
  • pressure or temperature sensors for checking the mixing chamber are arranged on the underside of the cover facing the mixing chamber.
  • the number as well as the arrangement and position can be configured as required.
  • These sensors serve as control means; Accordingly, the type and type of the sensors should be selected in such a way that they enable accurate observation and possible correction of the reaction conditions of the mixing components in the mixing chamber. For example, if the energy required for the materials to be treated is inadequate, it can be detected by means of the temperature sensors and quickly compensated for by switching on heat. In this context, it is conceivable that such controls or regulations can be taken over by a connected computer or can also be carried out manually.
  • a discharge valve is provided on the discharge part of the discharge device or the extruder.
  • the type or type of valve is to be selected as a function of the material properties, the discharge part being removable or interchangeable with other different discharge parts.
  • the discharge zone with the controllable passage opening can be adapted to any shape (depending on the subsequent use or further processing) of the discharged substance.
  • a cutting device with a rotating knife blade can be attached to the end of the discharge device.
  • the sealing plate guided in the mixing chamber is provided with mechanical seals, which are preferably made of hardened metal.
  • mechanical seals which are preferably made of hardened metal.
  • Conventional O-rings made of rubber material, Teflon-coated rubber, seals made of Viton or comparable materials can also be used, whereby it must be ensured that, depending on the material or mixture used, no harmful effects on the resilience or durability of these seals are brought about.
  • a mixing device with a discharge device is particularly advantageous if it is used for the production of carbohydrates or new synthesis, starting from mono- and / or disaccharides and / or their sugar alcohols.
  • Another object of the present invention is to provide a method for the physical modification and / or chemical derivatization of high molecular and / or low molecular weight carbohydrates, proteins and / or mixtures thereof.
  • Usual methods such as the continuous and discontinuous processes explained at the beginning, are on the one hand. tels extruder and on the other hand by autoclave. It is also known that these two application methods can be connected in series and / or in parallel in order to take advantage of each individual method. However, even in such an arrangement, these techniques cannot overcome all of the disadvantages, as is the case, for example, with the reaction times of the conventional methods, which, inter alia, have already been discussed at the beginning.
  • the object of the present method is that the advantages of both continuous and discontinuous treatment methods mentioned above can be carried out in one process step. It is among other things also the aim of optimally modifying the starting products to be implemented, even with very little to no water content, the plasticized end product easily and, above all, it can be regulated, the necessary reagents added as desired and volatile by-products withdrawn at any time.
  • the above objects are achieved in that the starting products are press-mixed by means of a press plate and a mixer, the guidance of the press plate and the mixer taking place decoupled from one another.
  • the press plate which can preferably be guided axially, exposes the material to feed on the one hand and to compressive stress on the other.
  • the effect of the mixer on the starting products to be modified is the homogenization, i.e. the mixing, and additional thermomechanical treatment by applying pressure and temperature to the starting products to be modified.
  • the decoupled guidance of the two construction parts enables the mix to be handled independently of one another.
  • the starting products are extremely flexible and therefore easier to implement. This consists primarily in the controllable and individually adjustable residence times, which means that the reactions can run better and above all completely.
  • the pressure and temperature conditions can be regulated within the mixing device used for this purpose. The result of this is that the chemical consumption required for the modification is better matched to the mixture to be treated, which also reduces it considerably, which is advantageous from an economic point of view.
  • the starting products are press-mixed completely or almost solvent-free.
  • the almost solvent-free treatment consists in an extremely small addition of, preferably water, to e.g. Bring carbohydrates into a hydrated state.
  • this can also be done without the addition of water, since the natural water content of the starting products can be used for hydration due to the mode of action of the press plate or through the application of a defined pressure.
  • this is particularly advantageous when processing inulin, since the production of highly esterified products produces typical amounts of water which would have to be removed for the reaction to proceed favorably.
  • this is no longer necessary, since it is also possible to work under negative pressure conditions. This not only creates economic savings in terms of water consumption, but also reduces the consumption of other chemical additional reagents, which are known to be required for incorporating the starting products into aqueous systems.
  • Discharge device consists in the conditions by which the substances are continuously, but according to the invention, forcedly conveyed in a controlled form. If the starting products for their modification are press-mixed with a small amount of solvent or water added according to the invention, the expansion of the material, which is important for starch production, can be completely or homogeneously achieved and, above all, a more favorable quality of the plasticized starch.
  • the end product can be removed constantly and completely from the mixing system in a completely or - if necessary - almost ready-to-sell, preferably strand-like, condition.
  • the finished end product is easy to handle, in particular can be further comminuted and / or better ground, which is important, for example, in the production of starch.
  • Example 1 the preparation of carboxymethylinulin
  • Example 2 the breakdown of guar gum
  • Example 3 the hydrophobization of potato starch.
  • the mixing chamber of the press mixing plant is heated to 60 ° C riert. 2000 g of Inulin ST (from Orafti, BE) are filled into the mixing chamber. 719 g of sodium monochloroacetate are added, the mixing chamber is closed and the press plate is put into operation at the medium level. The contents of the mixing chamber are 5 min. At 150 rpm and an oscillation frequency of 10 strokes / min. homogenized with the mixer. After 5 minutes, the press mixer is switched off, the lid is opened and 50 g of sodium hydroxide microbeads are added. At approx. 30 rpm and frequency 10, nitrogen is blown in through a valve for 60 seconds and vented through another valve. After purging with nitrogen, the valves are closed.
  • the speed of the stirrer is set to 250 rpm and the frequency to 15 strokes / min. raised and the press plate moved to a higher level. Under these conditions, the contents of the mixing chamber are treated mechanothermally. During this treatment, the temperature in the container rose from 55 ° C to 85 ° C. After 10 minutes the mixer speed is reduced to 50 rpm and the oscillation is switched off. The contents of the mixing chamber are continuously discharged in the form of a strand by the discharge device. The product strand is shredded, ground and analyzed. The content of glycolic acid and sodium monochloroacetate is determined by means of HPLC and the reaction efficiency is calculated.
  • the mixing chamber of the press mixer is heated to 100 ° C. 2000 g of conventional guar gum is poured into the mixing chamber and enough ml of deionized water is added that the dry matter of the mass is 55%.
  • the mixing chamber is closed and the press plate is set to a high operating level.
  • the contents of the mixing chamber are vented through the valve.
  • the content of the mixing chamber is at 15 strokes / min. homogenized with the mixer.
  • the speed of the mixer is kept so that a constant temperature is maintained in the mixing chamber. Under these conditions, the contents of the mixing chamber are treated mechanothermally. This increases during this treatment Temperature in the chamber and is kept constant at the desired level. Under these conditions, the contents of the mixing chamber are treated mechanothermally for different lengths of time.
  • the press plate is moved down and the mixer speed is set to approx. 50 rpm.
  • the contents of the mixing chamber are continuously discharged through the discharge device under extrusion conditions in the form of a strand.
  • the product strand is shredded, ground and analyzed.
  • the viscosity of a 10% solution is measured using a Brookfield RVT viscometer with a suitable spindle at 20 ° C and 50 rpm.
  • the mixing chamber of the press mixer is heated to 100 ° C. 2000 g of native potato starch (Starchina 20,000 from Agrana Zucker and Starch AG, AT) and 50 g of sodium hydroxide microbeads are filled into the mixing chamber. 247 g of lauric acid are added, the mixing device is closed and the press plate is started. The content of the mixing device is 5 minutes at 150 rpm and oscillation frequency of 10 strokes / min. homogenized with the mixer. After 5 minutes, nitrogen is blown in through a valve at about 30 rpm and frequency 10 for 60 seconds and vented through the further valve. After purging with nitrogen, the valves are closed. The speed of the mixer is set to 250 rpm and the frequency to 15 strokes / min.
  • the press plate is also driven at high speed.
  • the contents of the mixing chamber are treated mechanothermally. During this treatment, the temperature in the container rises to 140 ° C. After 10 minutes, the speed of the mixer is reduced to 50 rpm and the oscillation is switched off. The contents of the container are continuously discharged in the form of a strand via the discharge device. The expanded product line is shredded, ground and analyzed. The content of bound lauric acid is determined and the reaction efficiency is calculated.
  • Figure 1 is a sketched overall view of the invention with mixing device and discharge device.
  • FIG. 2 is a top view of the discharge device according to FIG. 1 seen from the mixing chamber;
  • FIG. 3 shows a variant of the discharge device from FIG. 2;
  • FIG. 4 shows a top view of the discharge device of an embodiment of the invention
  • FIG. 5 shows a sectional view of the arrangement according to FIG. 3 in the discharge plane
  • FIG. 6 is a detailed view V of FIG. 5th
  • the mixing device 1 with discharge device 5 is shown sketched, the mixing chamber 2 with sealingly guided press plate 3 and mixer 4 can be seen in the illustrated body 1 'of the device 1.
  • the mixing chamber 2 or the reaction container essentially consists of a pressure-resistant cylinder (usually up to 30 bar) with, for example, 10 1 capacity and allows external temperature control, for example in the form of a double-wall heater (not shown).
  • the mixer 4 is axially displaceable and is positioned at the position shown near the cover 6 of the mixing chamber 2, the mixer shaft 4 'being guided through the plate 3, while the press plate 3 is shown on the bottom of the mixing chamber; ie: is in the starting position or rest position.
  • the press plate 3 can have a simple mechanical seal 3 ', for example made of hardened metal.
  • a mixer for example, is used as a mixer 4, which can rotate and / or oscillate at a selectable speed, torque and oscillation frequency. For example, there are (maximum) speed ranges up to 350 rpm, torque ranges up to 1500 Nm and Oscillation frequencies up to 30 strokes / min. reachable.
  • the axially movable, sealingly guided reactor base or the pressure plate 3 can change the reaction volume in the mixing chamber 2 during the treatment of the material to be mixed and can also apply a corresponding pressure, while the mixer 4 brings about an optimal homogenization.
  • the discharge device 5 in the form of an extruder is integrated in the cover 6 or connected to it (only shown in a hint).
  • the feed section 5 'of the extruder is arranged in the extension of the mixer shaft 4'.
  • the extruder screw (not shown) runs transversely to the mixer shaft 4 'in the cover 6 of the mixing chamber 2.
  • FIG. 2 shows a view of the discharge device 5 according to FIG. 1, the cover 6 being visible from the mixing chamber 2.
  • the cover 6 has an opening 8, which in the example shown is designed in an oval shape and is arranged off-center.
  • the opening 8 represents the connection of the mixing chamber 2 with the discharge device 5.
  • an extruder screw 10 is visible, which can correspond to that of a conventional single-screw extruder.
  • the screw flight 10 '- indicated by dashed lines according to FIG. 2 - preferably has a diameter of approximately 30 mm.
  • valves 9 allow the mixing chamber 2 to be charged with liquid, solid or gaseous substances under constant pressure.
  • a safety valve 9 ' is also provided, which can be activated for ventilation of the system.
  • the third valve 9 ′′ is used to discharge volatile by-products that arise from the reaction of the polysaccharides to be treated, such as aggressive gases, for example chlorides or gaseous hydrochloric acid.
  • pressure and / or temperature sensors 11 are shown, with which the reaction conditions inside the Mixing chamber 2 can be detected.
  • the discharge zone 7 of the extruder with extrusion nozzle 7 ' is positioned in the extension of the extruder screw 10. In the left part of FIG. 2, the motor 12 is arranged in the axial direction of the extruder screw 10.
  • FIG. 3 shows a variant of the discharge device 5, as in FIG. 2, the motor 12 of the extruder 5 being arranged perpendicular to the axis of the extruder screw 10.
  • the pressure and / or temperature sensors 11 are positioned differently from those in FIG. 2.
  • Fig. 4 shows an embodiment of the invention, wherein the cover 6 is shown in a view from the mixing chamber 2. An embodiment is shown here which differs from that according to FIGS. 2 and 3.
  • the equipment elements of the discharge device 5, in particular the cover 6, show different arrangements and larger dimensions.
  • the opening 8 is arranged centered.
  • FIG. 5 shows a sectional view of the arrangement according to FIG. 3, the view showing a section along the longitudinal axis of the extruder screw 10, which is guided transversely through the cover 6.
  • the material to be mixed from the mixing chamber 2 is taken in via the intake part 5 '(not shown) through the connection opening 8 (indicated by dashed lines) and conveyed in the direction of the discharge part 7 by the thread of the extruder screw 10 along the screw flight 10' in order to pass via a discharge channel 7 '' to be pressed out with the discharge valve 14 '' open.
  • FIG. 5 also shows valves 9 and pressure or temperature sensors 11, which are arranged similarly to FIGS. 2 and 3.
  • FIG. 6 shows the detailed view V of the discharge zone 7 according to FIG. 5.
  • the discharge valve 14 ′′ which is connected to the extruder screw 10 or the extruder shaft 13 (indicated by broken lines) via the screw element or the screw screw 15 is shown.
  • the modified material is discharged or squeezed out via the discharge channel 14 'in such a way that the closable discharge channel 14' is opened by loosening a locking means 16, preferably a locking screw, on the top of the discharge valve 14 ''. Loosening the locking means 16 causes an axially arranged slide 17 to move accordingly, whereby the discharge channel 14 '- here in the lower part of the discharge valve 14''- can be exposed.
  • the material is transported with the help of the extruder screw 10 into the discharge zone 7 and over the discharge channel 14 'in order to be removed there in a metered manner.
  • the modified material can thus be subjected to a further treatment, such as grinding or cutting, more easily.
  • the discharge part 7 typically has a diameter of 2 to 10 mm and withstands a pressure of approximately 30 bar.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Materials Engineering (AREA)
  • Biochemistry (AREA)
  • Medicinal Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Emergency Medicine (AREA)
  • General Health & Medical Sciences (AREA)
  • Molecular Biology (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

La présente invention concerne l'utilisation d'un dispositif mélangeur comprenant une chambre de mélange (2) pourvue d'un mélangeur mobile (4) et d'une plaque de pression (3) guidée de manière à compacter aux fins de modification physique et/ou de dérivation chimique d'hydrates de carbone à poids moléculaire élevé et/ou à faible poids moléculaire, de protéines et/ou de leurs mélanges. L'invention concerne également un dispositif mélangeur destiné à la modification physique et à la dérivation chimique d'hydrates de carbone à poids moléculaire élevé et/ou à faible poids moléculaire, de protéines et/ou leurs mélanges comprenant au moins un mélangeur, au moins une plaque de pression (3) guidée de manière à rendre compact dans une chambre de mélange (2) fermée par un couvercle (6) et un dispositif de sortie (5) pourvu d'un élément d'entrée (5) et d'un élément de sortie (7). L'invention concerne aussi l'utilisation d'un dispositif de mélange pour une modification physique et/ou une dérivation chimique d'hydrates de carbone à poids moléculaire élevé et/ou à faible poids moléculaire, de protéines et/ou leurs mélanges. L'invention concerne enfin un procédé de modification physique et/ou de dérivation chimique d'hydrates de carbone à poids moléculaire élevé et/ou à faible poids moléculaire, de protéines et/ou leurs mélanges.
PCT/AT2003/000261 2002-09-27 2003-09-08 Dispositif melangeur et couvercle, leur utilisation et procede de modification et de derivation d'hydrates de carbone WO2004028675A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP03797967A EP1542791A1 (fr) 2002-09-27 2003-09-08 Dispositif melangeur et couvercle, leur utilisation et procede de modification et de derivation d'hydrates de carbone
AU2003260156A AU2003260156A1 (en) 2002-09-27 2003-09-08 Mixing device and covering device, use thereof and method for modifying and derivatising carbohydrates

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ATA1461/2002 2002-09-27
AT0146102A AT413698B (de) 2002-09-27 2002-09-27 Mischvorrichtung und abdeckvorrichtung, verwendung derselben sowie verfahren zur modifizierung und derivatisierung von kohlenhydraten

Publications (1)

Publication Number Publication Date
WO2004028675A1 true WO2004028675A1 (fr) 2004-04-08

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PCT/AT2003/000261 WO2004028675A1 (fr) 2002-09-27 2003-09-08 Dispositif melangeur et couvercle, leur utilisation et procede de modification et de derivation d'hydrates de carbone

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Country Link
EP (1) EP1542791A1 (fr)
AT (1) AT413698B (fr)
AU (1) AU2003260156A1 (fr)
WO (1) WO2004028675A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1816142A2 (fr) * 2006-02-03 2007-08-08 Gebr. Lödige Maschinenbau Gesellschaft mbH Procédé de préparation d'un épaississant à base de polysaccharides
WO2023170294A1 (fr) * 2022-03-10 2023-09-14 Hs-Tumbler Gmbh Dispositif et procédé pour la production de mélanges

Citations (4)

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US4457629A (en) * 1983-08-26 1984-07-03 Soonchin Liaw Gluten maker for the home
EP0196291A2 (fr) * 1985-03-21 1986-10-01 Wolf-Dieter Kreuziger Dispositif de mélange
GB2280856A (en) * 1993-08-10 1995-02-15 Talleres Miralles S A Mixing and discharging
DE19622979A1 (de) * 1996-06-08 1997-12-11 Albert Kedzierski Universelles Küchengerät

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US3527606A (en) * 1968-03-21 1970-09-08 American Maize Prod Co Method of modifying starch
AU4109493A (en) * 1992-04-20 1993-11-18 Bruce K. Redding Jr. Method and apparatus for the modification of starch and other polymers
US5363747A (en) * 1993-03-05 1994-11-15 Delaware Capital Formation, Inc. Processing vessel having discharge metering/mixing auger
US5401159A (en) * 1994-01-14 1995-03-28 Airlux Electrical Co., Ltd. Pasta maker
ES2149251T3 (es) * 1994-11-03 2000-11-01 Vomm Impianti & Processi Srl Metodo para la modificacion de almidon.
AT1956U1 (de) * 1996-09-25 1998-02-25 Voith Ag J M Einrichtung zum homogenisieren und dispergieren von flüssigen phasen
EP0916877A3 (fr) * 1997-11-14 2000-04-26 J.M. Voith Ag Dispositif d'étanchéité pour hautes pressions et mise en oeuvre d'un tel dispositif
DE10001256A1 (de) * 2000-01-14 2001-07-19 Bayer Ag Kontinuierliches Verfahren und Vorrichtung zur Trocknung und Gelbildung von lösungsmittelhaltigen gelbildenden Polymeren

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Publication number Priority date Publication date Assignee Title
US4457629A (en) * 1983-08-26 1984-07-03 Soonchin Liaw Gluten maker for the home
EP0196291A2 (fr) * 1985-03-21 1986-10-01 Wolf-Dieter Kreuziger Dispositif de mélange
GB2280856A (en) * 1993-08-10 1995-02-15 Talleres Miralles S A Mixing and discharging
DE19622979A1 (de) * 1996-06-08 1997-12-11 Albert Kedzierski Universelles Küchengerät

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of EP1542791A1 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1816142A2 (fr) * 2006-02-03 2007-08-08 Gebr. Lödige Maschinenbau Gesellschaft mbH Procédé de préparation d'un épaississant à base de polysaccharides
EP1816142A3 (fr) * 2006-02-03 2009-12-02 Gebr. Lödige Maschinenbau Gesellschaft mbH Procédé de préparation d'un épaississant à base de polysaccharides
WO2023170294A1 (fr) * 2022-03-10 2023-09-14 Hs-Tumbler Gmbh Dispositif et procédé pour la production de mélanges

Also Published As

Publication number Publication date
ATA14612002A (de) 2005-09-15
AU2003260156A1 (en) 2004-04-19
AT413698B (de) 2006-05-15
EP1542791A1 (fr) 2005-06-22

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