EP0826781A2 - Zusammensetzung eines nichtzentrifugierten Zuckers und Verfahren zur Herstellung eines Zuckerproduktes - Google Patents

Zusammensetzung eines nichtzentrifugierten Zuckers und Verfahren zur Herstellung eines Zuckerproduktes Download PDF

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Publication number
EP0826781A2
EP0826781A2 EP97202392A EP97202392A EP0826781A2 EP 0826781 A2 EP0826781 A2 EP 0826781A2 EP 97202392 A EP97202392 A EP 97202392A EP 97202392 A EP97202392 A EP 97202392A EP 0826781 A2 EP0826781 A2 EP 0826781A2
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Prior art keywords
sugar
granule
weight
composition
preparation
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EP97202392A
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English (en)
French (fr)
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EP0826781A3 (de
EP0826781B1 (de
Inventor
Takeo Mizutani
Tadashi Ebashi
Kozo Yamada
Toshiaki Sugitani
Masaaki Kodomari
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Mitsui DM Sugar Co Ltd
Kumphawapi Sugar Co Ltd
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Mitsui Sugar Co Ltd
Kumphawapi Sugar Co Ltd
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Priority claimed from JP19072497A external-priority patent/JP3702984B2/ja
Priority claimed from JP21390897A external-priority patent/JP3779800B2/ja
Application filed by Mitsui Sugar Co Ltd, Kumphawapi Sugar Co Ltd filed Critical Mitsui Sugar Co Ltd
Publication of EP0826781A2 publication Critical patent/EP0826781A2/de
Publication of EP0826781A3 publication Critical patent/EP0826781A3/de
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    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B30/00—Crystallisation; Crystallising apparatus; Separating crystals from mother liquors ; Evaporating or boiling sugar juice
    • C13B30/02—Crystallisation; Crystallising apparatus
    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B50/00—Sugar products, e.g. powdered, lump or liquid sugar; Working-up of sugar

Definitions

  • the present invention relates to a noncentrifugal sugar composition in which cane juice is used as a starting material.
  • the present invention relates also to a process for the preparation of a noncentrifugal sugar composition.
  • the present invention relates further to a process for the preparation of granule-formed sugar, particularly to the process in which a step of drying, cooling and conditioning sugar is simplified.
  • Cane sugar is classified roughly into two groups.
  • One is noncentrifugal sugar (i.e. molasses-containing sugar) which is prepared by solidifying concentrated cane juice as a whole without separating molasses from sugar crystal
  • centrifugal sugar i.e. molasses-removed sugar
  • various nutritionally valuable minor components which are contained in the cane juice are removed as impurities without being used effectively. They are, for example, reducing sugars such as glucose and fructose, abundant minerals such as calcium, potassium and magnesium, and vitamins which are considered to be effective for keeping health.
  • Brown soft sugar is almost equal to the refined sugar in contents of nutrition components and minerals, and in flavor.
  • Sugar enriched with nutritional components and minerals lacks a natural balance.
  • Sho-60-30700/1985 discloses a method of removing salty and bitter tastes components and of maintaining nutrition and flavor components in the brown sugar by means of electrodialysis in combination with a prior method for the brown sugar preparation.
  • Japanese Patent Application Laid-open No. Sho-60-133900/1985 discloses a process for the preparation of a less colored brown sugar, wherein after removing foreign substances by filtration, the cane juice is heated to be concentrated, after that the juice is heated again with addition of a small amount of milk lime, and then cooled to solidify.
  • any of the applications described above does not refer to the changes in flavor and color of the noncentrifugal sugar compositions with the passage of time.
  • solidification refers to a state of sugar in which sugar solidifies to lose fluidity, and is a large factor of deteriorating the commercial value of sugar products. Accordingly, less solidification is a very preferable property of sugar.
  • a process for the preparation of sugar mainly comprises a step of preparing sugar syrup, a step of heating and evaporating the sugar syrup, a step of crystallizing the sugar syrup to obtain sugar, and a step of drying and conditioning the sugar. If the step of drying and conditioning sugar syrup is not sufficiently carried out on sugar which has been transformed to crystallize by, for example, boiling, and pelletized or granulated, a problem of solidification happens during the storage of the product to lose its commercial value.
  • the step of drying and conditioning is composed of three sub-steps: drying with a dryer, cooling with a cooler and conditioning in a hopper. More specifically, in the drying procedure, sugar products are dried with a dryer in order to decrease the moisture of the sugar products so as to prevent them from solidifying. For example, in the case of granulated sugar, the moisture is about 0.6 to 1.5 % by weight when it leaves a centrifugal machine. It is then dried to a moisture of about 0.02 % by weight with a dryer at about 50 to 75 °C. If the sugar product is fed directly to a hopper without being dried with a dryer, there is high possibility of solidifying because of its uncontrolled moisture.
  • the sugar product dried with a dryer is cooled with a cooler to about 35 to 45 °C. If the sugar product dried with a dryer is fed directly to a hopper without the cooling procedure, there is high possibility of solidifying due to heat held in the sugar product and/or to moisture remaining partly.
  • the cooled sugar product is homogenized in a hopper in order to level its moisture and thereby to prevent it from solidifying.
  • the sugar product cooled with a cooler is conditioned in a hopper in which dry air is supplied, to remove moisture which is contained in crystals of sugar and which would cause the sugar to solidify. After the conditioning, the sugar is packed in a bag and shipped.
  • dryers are well known to be used in the drying procedure, such as fluidized bed dryers, flash jet dryers and rotary dryers.
  • Various sugar coolers are known to be used in the cooling procedure, such as rotating-type drum coolers and vacuum-type belt coolers.
  • all of the machines takes high costs for equipment. Accordingly, installation of the equipment may lead to increased costs of the product.
  • a purpose of the present invention is to provide a noncentrifugal sugar composition which maintains natural flavor as original from a sugar cane and which is less colored and excellent in stability with the passage of time.
  • Another purpose of the present invention is to provide a process for the preparation of a noncentrifugal sugar composition which maintains natural flavor as original from a sugar cane and which is less colored and excellent in stability with the passage of time.
  • Another purpose of the present invention is to provide, at lower costs, a process for the preparation of granule-formed sugar which maintains original flavor and nutritional components and which is easy to handle.
  • the present inventors have made a lot of researches to improve the quality of noncentrifugal sugar. As the results, we have found that by greatly decreasing a moisture of a composition so comprising cane juice and sucrose and/or liquid sucrose as to have particular properties produced is a noncentrifugal sugar composition which is excellent in stability with the passage of time and has rich flavor. These findings have led to the present invention.
  • the present invention first provides noncentrifugal sugar composition comprising cane juice and sucrose or liquid sucrose or both, characterized in that the color value is not more than A12000, the purity is 93.1 to 86.0 % by weight and the moisture is not more than 2.0 % by weight.
  • the present invention secondly provides a process for the preparation of a noncentrifugal sugar composition, characterized in that the process comprises the following steps: cane juice is filtered; a pH of the juice is adjusted to 5.0-6.0; sucrose or liquid sucrose or both is added to adjust a purity of the mixture to a range of 95.1 to 87.0 % by weight; the mixture is heated and evaporated; and then the mixture is cooled to solidify with a strong shearing force being applied to obtain granules.
  • the present inventors also have found that when a purity of sugar syrup before a heating and evaporation step is adjusted to 87.0 to 95.1 and the sugar syrup after a heating and evaporation step is crystallized with a strong shearing force being applied to obtain granule-formed sugar, a process of drying and conditioning sugar may be simplified into only one procedure with a hopper which corresponds to the prior conditioning procedure, without using a costly dryer or cooler.
  • the granule-formed sugar thus obtained has functions as a healthy food having original flavor and nutritional components and is excellent in fluidity and hard to solidify.
  • the present invention thirdly provides a process for the preparation of granule-formed sugar which comprises a step of preparing sugar syrup, a step of heating and evaporating the sugar syrup, a step of crystallizing the sugar syrup to obtain sugar and a step of drying, cooling and conditioning the sugar, characterized in that
  • Fig. 1 shows an apparatus and a schematic procedure used in Example 3 for preparing the present composition.
  • Fig. 2 shows an apparatus and a schematic procedure used in Example 6 for preparing the present granule-formed sugar.
  • the present composition contains cane juice and sucrose and/or liquid sucrose.
  • a weight ratio of the cane juice to sucrose (and/or liquid sucrose) depends on purity of the cane juice.
  • the composition should contain the cane juice and sucrose (and/or liquid sucrose) so as to have a purity of 93.1 to 86.0 % by weight of the whole composition. Preferably, the purity is 93.1 to 89.0 % by weight. If the purity is too high, sugar cane flavor may almost disappear. If the purity is too low, a production rate on machinery in a continuous process is lower, and adhesion of solid materials on the inside of the machine occurs remarkably as well. These decrease the efficiency of the production.
  • purity (polarization/total solid) x 100 wherein the polarization is measured in the Spencer method which is described in "Handbook of Sugar Production", edited by the Research Society of Japan Sugar Refineries' Technologists, Asakura Shoten, June 30, 1962; and the total solid is indicated in % (w/w).
  • a percent ratio of a solid weight of the cane juice to a weight of the noncentrifugal sugar composition is adjusted to 30-70 % by weight.
  • cane juice mean mill juice obtained by crushing sugar cane or extracted juice obtained by extracting sugar cane.
  • sucrose and/or liquid sucrose are not restricted to particular ones. Use may be made of one or more of granulated sugars, raw sugars, white soft sugars, which are crystal sugars, and fine liquor which is liquid sugar.
  • a reducing sugar content is 3.5-6.5 % by weight and an ash content is 1.1-2.5 % by weight.
  • the reducing sugar content is determined in the methylene blue method.
  • the reducing sugars in the present composition include glucose, fructose, and so on.
  • the ash content is indicated in a value determined as sulfate salts.
  • Elements which may be contained in the present composition include calcium, potassium, magnesium, etc.
  • the present composition may further contain vitamins such as B 1 , B 2 , B 6 and pantothenic acid in addition to the aforesaid components. These vitamins are components originated from cane juice.
  • color value is not more than AI2000, preferably not more than AI1500. If the color value is too high, coloring is strong, then application of the composition is restricted. There is no particular lower limit in the color value, but it is usually at least AI600.
  • the color value (AI) is obtained according to the description in "Handbook of Sugar Production", edited by the Research society of Japan Sugar Refineries' Technologists, Asakura Shoten, June 30, 1962, as follows :
  • a sample is dissolved in water to prepare a test solution of about 25 % (w/w) concentration, and then the pH thereof is adjusted to 7.0, of which Brix degree (Bx) is measured with a refractometer for Bx measurement. Subsequently, absorbance (ABS) of the test solution (pH 7.0) is measured at 560 nm on a spectrophotometer.
  • Bx Brix degree
  • ABS absorbance
  • AI (1000 x ABS x 100)/(b x (Bx) x g) (2) wherein ABS is absorbance; b is an optical path length (cm) of a cell in the spectrophotometer; Bx is a Brix degree (g/g); and g is the specific gravity (g/ml) of the test liquid.
  • the composition has yellowish white to light brown color. Accordingly, it is possible to use the present composition in wider applications, compared to the prior products of noncentrifugal sugars, such as brown sugar and O-tung.
  • the moisture value of the present composition is not more than 2.0 % by weight, preferably 1.3 % by weight. If the moisture value is too high, it is impossible to prevent it from coloring and deteriorating in flavor with the passage of time.
  • the moisture is preferably at least 0.4 % by weight owing to the restriction in the preparation procedure that a production efficacy lowers as the drying time is longer, or for the reason that natural flavor of a sugar cane decreases during a long drying treatment.
  • the moisture value is measured using a method of drying under reduced pressure at 75 °C for 3 hours.
  • the moisture value when the moisture value is thus controlled, it is possible to prevent the composition from coloring and deteriorating in flavor with the passage of time; in addition, the composition exhibits surprisingly better fluidity, which is an important factor for sugar products, than that of the prior art noncentrifugal sugar; and this fluidity is nearly same as that of granulated sugar which is known to exhibit good fluidity among sugar products.
  • Good fluidity is a very preferable characteristic because the product obtained is then easy to handle in use and a working efficiency is good in the preparation of the product, particularly in packaging procedures.
  • the present composition is preferably prepared as follows:
  • cane juice is filtered in order to remove foreign substances without purifying it with lime as in the prior art.
  • the filtration manner is not restricted to particular one. Any method widely used in the food industry such as screen filtration, diatomaceous earth filtration, precision filtration and ultrafiltration may be preferably applied.
  • the pH of the cane juice after the filtration treatment becomes 4.8-5.8 depending on the cultivars of the sugar cane.
  • sucrose and/or liquid sucrose is mixed to the above cane juice to adjust the purity to the aforesaid range.
  • the mixture is then heated to be concentrated.
  • the heating temperature is preferably 125 -130 °C.
  • the concentrated liquid sugar is cooled to crystallize.
  • the cooling and crystallization may be carried out while applying a strong shear force with the aid of, for example, a universal mixer or nauta mixer in the case of batch production, or an extruder, kneader or turbulizer in the case of continuous production.
  • granulated product may be obtained. It may be dried, if needed, to adjust its moisture value to the aforesaid range.
  • the composition obtained may be in any form depending on the treatment. In the case where the cooling is carried out with stirring, the composition is in a granule form, which may be ground on a mill to obtain powder.
  • the present composition keeps natural flavor originated from sugar cane. As it has no strong flavor nor coloring like brown sugar has, it may be used not only in any particular foods, but widely in general foods. Its applications are in various sweeteners in powder, granule, cube, paste, liquid, and any other forms, and in foods containing sweeteners, such as drinks, e.g. coffee, tea, soft drinks, aerated drinks, dairy drinks, and sweet drinks from fermented rice; candies e.g. hard candies and soft candies; confectioneries e.g. tablet sweet, fondant, icing, jelly, mousse, chocolate, cookie, cake, ice cream, sherbet and chewing gum; and sweetened foods e.g. sweet pickles, dressing and various sauces. Besides the foods, it may be used in other applications, for example, in oral drags including Chinese medicines, e.g., in a sugar-coated tablet or for seasoning a tablet body.
  • sweeteners such as drinks, e.g. coffee, tea,
  • composition is excellent in fluidity as mentioned above and also excellently easy to be formed into tablets, it may be an excellent material for tablet sweets.
  • the present composition has effects of improving acrid taste of soy sauce and giving deepness and roasted aroma to the taste of soy sauce. These effects are attained by compatibility of the present composition with soy sauce. These effects may be exhibited, for example, when the present composition is used in sauce for Mitarashi-dango, i.e. dumplings with brown sauce, seasonings for laver or sauce for Donburi, i.e. rice in a bowl which is covered with cooked materials.
  • the present composition has an effect of suppressing undesirable odors of food ingredients, i.e. deodorant effect. Accordingly, when the present composition is used for sweetness in cooking, undesirable odors from food ingredients, for example, onions, meats, or fishes, may be suppressed to improve the quality of taste in meals. For example, when the present composition is used for seasonings for meats such as grilled meats or grilled chickens, seasonings for fishes, canned meats or fishes, or Tsukudani, i.e. foods, such as fishes, boiled down in soy sauce, this effect may be exhibited.
  • undesirable odors from food ingredients for example, onions, meats, or fishes
  • Tsukudani i.e. foods, such as fishes, boiled down in soy sauce
  • the present composition has a flavor originated from a sugar cane which emphasizes a desirable taste that food ingredients have.
  • a sugar cane which emphasizes a desirable taste that food ingredients have.
  • the present composition when used in instant coffee, its taste feels like that of coffee roasted with charcoal.
  • sweet potatoes or pumpkin croquettes flavor from food ingredients is enhanced. The above effect may be thus exhibited.
  • flavor which the present noncentrifugal sugar composition has may be exhibited as such in foods and, in addition, the flavor originated from the present noncentrifugal sugar composition may change during cooking to generate a desirable taste.
  • the present composition when used in hard candies, Rakugan, i.e. rice-flour cakes, or skin of manju, i.e. buns with a bean-jam filling, these effects may be exhibited.
  • the present noncentrifugal sugar composition has an effect of coordinating entire taste of a cooked food to make it more delicious, when it is used in cooking.
  • acidity is softened to coordinate their taste. The above effect may be thus exhibited.
  • the present composition has a remarkably small moisture, compared to noncentrifugal sugar products of the prior art originated from cane juice.
  • a moisture value is about 5-8 % by weight in brown sugar lump, and about 3-6 % by weight in O-tung.
  • Table 1 shows examples of analysis data of noncentrifugal sugar products originated from a sugar cane. These data are cited from "Process for the Preparation of Cane Sugar", Korin Shoin, April 5, 1963, page 7, Table 1.6 for brown sugar lump and page 8, Table 1.9 for O-tung). Meanwhile the moisture is not more than 2% by weight in the present composition.
  • the present process for the preparation of granule-formed sugar comprises a step of preparing sugar syrup, a step of heating and evaporating the sugar syrup, a step of crystallizing the sugar syrup and a step of drying, cooling and conditioning sugar.
  • the present invention improves the prior processes for the preparation of granule-formed sugar to shorten the prior processes.
  • the step of drying, cooling and conditioning sugar may be carried out only with a hopper without steps using a dryer and a cooler. This is due to the restricted purity of sugar syrup of the a particular range and the strong shearing force applied in crystallization.
  • the step of preparing sugar syrup and the step of heating and evaporating the sugar syrup may be carried out in a way conventional in this field.
  • the purity of a product may be 86.0 to 93.1 % by weight, preferably 89.0 to 93.1 % by weight because some parts of sucrose are decomposed in the subsequent steps.
  • the granule-formed sugar has less flavor or less nutritional components. Further, in the step of drying, cooling and conditioning sugar, if transformed and crystallized granule-formed sugar is introduced into a hopper with its moisture and temperature remaining high, there is a high risk that it solidifies with each other because of its high purity. Accordingly, it is impossible to prepare the envisaged granule-formed sugar which may be dried directly in a hopper. Meanwhile, if the purity is too low, in the step of crystallizing the sugar syrup, for example, in a horizontal continuous crystallizing machine with high speed paddles, a continuous production speed decreases and, furthermore, adhesion of solid materials to the inside of the machine occurs remarkably. In addition, in the next step of drying, cooling and conditioning the sugar, a larger amount of dry air and more drying time are needed, which results in the need for a larger hopper or more hoppers. This increases costs.
  • sugar syrup As the sugar syrup, use is made of sugar syrup prepared by adding sucrose and/or liquid sucrose to cane juice to adjust its purity to 87.0 to 95.1 % by weight.
  • a weight ratio of the sucrose and/or liquid sucrose to the cane juice is dependent upon the purity of cane juice.
  • a percentage of a solid weight of the cane juice to a weight of the granule-formed sugar that is, (solid weight of the cane juice)/(the granule-formed sugar weight) x 100, is adjusted to 30-70 % by weight.
  • the sugar syrup having the aforesaid purity may be obtained, for example, in the manner as mentioned above, that is, by filtering cane juice and then adjusting the pH of the juice to 5.0 to 6.0, to which sucrose and/or liquid sucrose is added.
  • the sugar syrup may be prepared by subjecting cane juice to a clarification procedure in which milk lime is added to the cane juice and the juice is added, and then adding sucrose and/or liquid sucrose.
  • the former without a clarification procedure with milk lime
  • the former is preferred because the granule-formed sugar obtained finally is better in quality (i.e., coloring is suppressed and the flavor and nutrition components remain) and, therefore, may be used widely.
  • the step of preparing the sugar syrup may be preferably carried out as follows : first, cane juice is filtered in order to remove foreign substances without clarifying it with milk lime.
  • the filtration method includes those widely used in the food industry such as screen filtration, diatomaceous earth filtration, precision filtration and ultrafiltration. Among these, the ultrafiltration is preferred. Most preferred is the ultrafiltration with a fractionating molecular weight of 150,000 or less, more particularly 30,000 to 150, 000.
  • use may be preferably made of tubular type ultrafilter membranes, plate-type ultrafilter membranes, spiral ultrafilter membranes and hollow yarn-type ultrafilter membranes.
  • the pH of the cane juice after the filtration treatment becomes 4.8-5.8 depending on the cultivars of the sugar cane.
  • the purity of the cane juice after the pH adjustment is adjusted to 87.0 to 95.1 % by weight using sucrose and/or liquid sucrose.
  • the sugar syrup thus obtained is fed to the next step of heating and evaporating the sugar syrup.
  • the step of heating and evaporating the sugar syrup may be preferably carried out in the following manner. That is, a three-step plate-type heat exchanger is used to concentrate the sugar syrup, where two steps of concentration under reduced pressure and one step of concentration under atmospheric pressure are conducted in this order. Then, the concentration may be efficiently carried out with the decomposition of sucrose and the coloring being suppressed.
  • the plate-type heat exchanger having three steps steam energy is more efficiently used, compared to a plate-type evaporator station of only one step or a reduced pressure evaporator station of only one step, because the steam generated in the first step is reused in the second step.
  • sugar syrup having a purity of 87.0 to 95.1 % by weight from the prior step is heated to be concentrated from about Bx 28 to about Bx 40 in the first plate-type heat exchanger.
  • the concentrate is separated from steam with a vapor separator under reduced pressure.
  • the concentrate obtained is fed to the second plate-type heat exchanger and heated to be concentrated from about Bx 40 to about Bx 65. Meanwhile, the steam separated in the first vapor separator is supplied to a steam site of the second plate-type heat exchanger. After the second step, the concentrate is separated from steam with a vapor separator under reduced pressure.
  • the concentrate obtained is heated to be concentrated from about Bx 65 to about Bx 93 in the final plate-type heat exchanger. Under atmospheric pressure, the concentrate obtained is separated from steam with a vapor separator.
  • the sugar syrup concentrated to about Bx 93 is fed to the step of crystallizing the sugar syrup and is transformed and crystallized. Particularly, in the case where a horizontal continuous crystallizing machine with high speed paddles is used in the next step of crystallizing the sugar syrup, it is preferred to concentrate the sugar syrup to a Brix range of about 90.5 to 95.3 in the step of heating and evaporating the sugar syrup in order to attain better transformation and crystallization.
  • concentration does not sufficiently progress, that is, a Brix is too low, it is sometimes difficult to carry out the transformation and crystallization with a horizontal continuous crystallizing machine with high speed paddles. If concentration is carried out excessively, that is, a Brix is too high, the fluidity becomes bad before entering the horizontal continuous crystallizing machine with high speed paddles and, consequently, solidification occurs. This causes a problem that pipes are clogged.
  • the outlet temperature of the concentrate of the plate-type heat exchanger is set to about 127 °C by reference to the conversion table. In this manner, it is possible to carry out the step of heating and evaporating the sugar syrup efficiently by monitoring the outlet temperature of a concentrate of the final plate-type heat exchanger, that is, inlet temperature of the vapor separator, without need of directly measuring the Bx after the concentration.
  • the sugar syrup after concentrated is then fed to the step of crystallizing the sugar syrup.
  • Means for carrying out it include a universal mixer, nauta mixer, extruder, kneader, colloidal mill or horizontal continuous crystallizing machine with high speed paddles.
  • the horizontal continuous crystallizing machine with high speed paddles is preferred.
  • the horizontal continuous crystallizing machine with high speed paddles is a kind of continuous mixing and dispersing machine and is used as a crystallizing machine in the present process. Typical example of it is turbulizer.
  • the crystallization using the horizontal continuous crystallizing machine with high speed paddles is preferably carried out in the following manner.
  • heated dry air is introduced.
  • a relative humidity of the heated dry air is RH 10 % or less.
  • An air volume of the heated dry air is 9 to 30 Nm 3 / min. when the horizontal continuous crystallizing machine with high speed paddles is operated at a discharge speed of granule-formed sugar of 1 ton / hour.
  • With the aforesaid relative humidity and air volume it is possible to keep the moisture of the granule-formed sugar from the horizontal continuous crystallizing machine with high speed paddles at 2.5 % by weight or below.
  • the moisture of the granule-formed sugar from the horizontal continuous crystallizing machine with high speed paddles can be made uniform and lower.
  • the next step of drying, cooling and conditioning sugar may be carried out satisfactory.
  • the temperature of the heated dry air is preferably at least 60 °C, more preferably at 82 to 88 °C. If the temperature of the heated dry air is too low, the sugar syrup is cooled to become a candy-like state before the crystallization occurs. Then, the candy-like materials adhere to the inside of the horizontal continuous crystallizing machine with high speed paddles. This increases a load on the machine and causes the machine to stop. Further, due to the presence of the dry air of a too low temperature, evaporation of water by heat of crystallization becomes insufficient.
  • a peripheral speed of paddles, that is, linear velocity of paddles, of the crystallizing machine is generally 25 to 45 m / sec., preferably 30 to 40 m / sec. so as to narrow particle size distribution.
  • granule formed sugar is prepared from sugar syrup having a purity of 97.1 to 99.9 in an industrial scale with a horizontal continuous crystallizing machine with high speed paddles.
  • granule-formed sugar having a high purity has a high risk that it solidifies in a hopper.
  • the granule-formed sugar obtained from the step of crystallizing sugar syrup is fed to the next step of drying, cooling and conditioning sugar.
  • a conveyor is generally used for transporting the granule-formed sugar crystallized in the step of crystallizing sugar syrup to a hopper used in the step of drying, cooling and conditioning sugar.
  • the conveyor preferably comprises a means for efficiently removing vapor which is generated from the granule-formed sugar during it is transported. Such efficient removing of vapor may be carried out by ventilation, i.e. by blowing and sucking air.
  • the moisture of the granule-formed sugar transported may be controlled by controlling the amount of air.
  • the conveyor includes, for example, a screw conveyor, a vibration conveyor, a continuous flow conveyor and a belt conveyor.
  • a moisture value of the granule-formed sugar just before entering the hopper is preferably at most 2.0 % by weight.
  • the granule-formed sugar from the prior step of crystallizing the sugar syrup has a temperature of about 110 to 120 °C.
  • the vapor generated from the granule-formed sugar is efficiently removed during the transportation to a hopper with the conveyor and the granule-formed sugar itself radiates heat, it is cooled to about 100 °C.
  • the granule-formed sugar is introduced from the conveyor into a hopper through the bottom of which dry air is blown in and directly dried, cooled and conditioned there, without passing through a dryer or a cooler as in the prior art.
  • a temperature of the dry air which is blown in the hopper is preferably about 40 to 50 °C.
  • a relative humidity of the dry air is preferably RH 35 % or less at this temperatures.
  • the granule-formed sugar is dried in the hopper to a moisture value of at most 1.3 % by weight, preferably at most 0.9 % by weight and at least 0.4 % by weight.
  • the relative humidity of the dry air is necessarily at most RH 35 %.
  • the moisture value of the granule-formed sugar just before entering the hopper from the conveyor is preferably at most 2.0 % by weight in order to prevent it from solidifying in the hopper.
  • the hopper used in the present invention includes a sugar bin, a silo, a reservoir or a bin.
  • the granule-formed sugar prepared by the present process may be used in wider applications, compared to the prior noncentrifugal sugar such as brown sugar and O-tung, because its color value is not more than AI 2000. Accordingly its application for food is not restricted to particular ones, but may be used in general.
  • the granule-formed sugar prepared by the present process has a moisture value of at most 1.3 % by weight, preferably at most 0.9 % by weight. If the moisture value is too high, it is impossible to prevent the granule-formed sugar from coloring or losing its flavor with the passage of time. However, the moisture is preferably at least 0.4 % by weight, because natural flavor of sugar cane decreases during a long drying treatment if the drying is carried out in such conditions that the moisture becomes too low. The moisture is measured using a method where drying is conducted under reduced pressure at 75 °C for 3 hours.
  • the granule-formed sugar prepared by the present process has very preferable characteristics. That is, the particle size distribution is narrow and the coefficient of variation is small.
  • a noncrystal part i.e. syrup part, is present in a very stable state in the granule-formed sugar. Accordingly, it is excellent in fluidity and hard to solidify.
  • the granule-formed sugar is easy to handle in use as well as keeps its quality in storage and its working efficiency is good in the preparation of the product, particularly in packaging procedures.
  • a color value (AI) was measured in accordance with the aforesaid formula (2) from a Bx (Brix degree) and absorbance (ABS) at 560 nm, with the Bx being measured on a refractometer for Bx measurement. pH was measured on a pH meter.
  • Solid Weight Ratio, Cane Juice Granulated Sugar moisture, % Purity, % Reducing Sugars, % Ash, % Color Value (AI) 1 3:7 0.6 93.1 3.5 1.1 640 2 4:6 0.8 91.7 4.2 1.4 800 3 5:5 0.8 90.1 5.0 1.8 1070 4 7:3 1.1 87.0 6.5 2.5 1500 5 10:0 ( Ref. Ex.) 1.2 82.3 8.7 3.5 2000
  • Noncentrifugal sugar compositions were prepared as in Example 1, Nos. 2 and 4, except that moisture values were varied at the final drying process.
  • Samples (a) to (e) have the same composition as No.2 in which a solid weight ratio of cane juice to granulated sugar was 4:6 and purity was 91.7%, except for moisture value.
  • Samples (f) to (j) have the same composition as No.4 in which a solid weight ratio of cane juice to granulated sugar was 7:3 and purity was 87.0%, except for moisture value.
  • moisture value is important in a noncentrifugal sugar composition and if it exceeds 2%, the change with the passage of time in color value is large, and flavor deteriorates, too.
  • the composition of which water content is not more than 2% is colored little and keeps natural flavor originated from sugar cane after about ten months storage.
  • This solution was sent to a thin-film vacuum evaporator (3) with a heating area of 17 m 2 by a pump (2) at a rate of 190 liters per hour to exchange heat with steam via a bulkhead plate. And it was concentrated until Bx 92 was attained, and then it was separated from vapor by a vapor separator (4).
  • the concentrated solution was then sent to a turbulizer (6), ex Hosokawa Micron Corporation, 1900 rpm, by a pump (5) at a rate of 87 liters per hour.
  • the concentrated solution solidified immediately due to a strong shearing force caused by paddles at high speed inside the turbulizer.
  • the granulated noncentrifugal sugar composition with moisture of about 4% was thus prepared in a production efficiency of about 78 kg/hour.
  • the granulated noncentrifugal sugar composition obtained was dried in a fluidized bed dryer (7), Fuji Paudal Co., Ltd., MDD-3000N, to obtain moisture of the product of 0.8%.
  • the granulated noncentrifugal sugar composition after the drying was sieved on a sifter (8) in order to uniform the particle size, after that it was cooled in a hopper (9) through which dry air was blown to obtain a product (11).
  • composition thus obtained had color value of AI650 and purity of 93.0%. It was yellowish white granules with natural flavor originated from a sugar cane.
  • a noncentrifugal sugar composition was prepared using the same apparatus as used in Example 3, but at a changed solid content ratio of cane juice to granulated sugar and a changed production rate so as to obtain a granulated composition.
  • the purity and production rate of the composition finally obtained are shown in Table 5 below.
  • the preparation could be stably carried out at a production rate of 78 kg/hour for about ten hours, whereas for Product B at a production rate of 60 kg/hour for about five hours.
  • Product C as adhesion of solid materials to the inside the turbulizer occurred, stable preparation at a production rate of 40 kg/ hour could be carried out only for about two hours. From these results, it is seen that a higher purity of a product is better for increasing a production efficiency and a yield.
  • Product D having purity of 85.0% was prepared in the same procedure as above. Adhesion of solid materials to the inside the turbulizer occurred so remarkably that the product could be hardly prepared at a production rate of 40 kg/hour.
  • the angle of repose and the angle of exhausting which are indices of fluidity, were determined on composition No. 4 (prepared in Example 1 and having a weight ratio of a total solid content of cane juice to granulated sugar of 7 : 3, an average particle size of 660 ⁇ m, coefficient of variation of 0.15 and moisture value of 1.1 %), white soft sugar, A, ex Mitsui Sugar Co., Ltd. and granulated sugar, GM, ex Mitsui Sugar Co., Ltd.
  • the angle of repose and the angle of exhausting were determined as follows :
  • a sample was dropped from a sample hopper to a disc stand for determination having a diameter of 40 mm. The dropping was stopped at the moment when a stack of a sample was highest and then the angle of a slope of the stack was determined.
  • sample fluidity angle of repose angle of exhausting composition No.4 from Example 1 34 40 white soft sugar 62 - granulated sugar 35 41
  • the present noncentrifugal sugar composition had excellent fluidity, i.e., lower angles of repose and exhausting, compared to white soft sugar. Further, it exhibits nearly the same angles of repose and exhausting as those of granulated sugar which is known to exhibit better fluidity among many kinds of sugars.
  • composition No. 2 having a weight ratio of a total solid content of cane juice to granulated sugar of 4:6 was dried in a MIDGET-DRYER, Fuji Poudal Co., Ltd., with flowing warm air at 50 ° until moisture of 0.6% was attained. It was then sieved with test sieves to obtain a classified product having a particle size of 840-250 ⁇ m.
  • the mixture was made into tablets in a tablet machine, type HU-T, Hata Iron Works Ltd., in conditions of a tablet making pressure of 500 kg and a tablet diameter of 5 mm.
  • Composition No. 2 used did not adhere to the tablet machine and was excellent in fluidity which is important to a material for tablet sweets.
  • the tablet sweets obtained had a good flavor which is natural and profound.
  • the batter obtained using composition No.1 had a natural flavor originated from sugar cane, unlike the control batter.
  • the batter obtained using composition No.1 was easy to shape and exhibited good dispersiveness when it was mixed with flour (i.e. few undissolved lumps) and smoothness on the surface of the pancake, as same as in the control batter.
  • the one obtained using white soft sugar had fish odor, whereas the other obtained using composition No.4 had a preferable flavor with the fish odor being suppressed.
  • the coffee bavarois with composition No.4 had a simple sweetness and roasted coffee flavor, that is, advanced flavor, compared to the control with white soft sugar.
  • noncentrifugal sugar composition No.4 obtained in Example 1 After 70 g of noncentrifugal sugar composition No.4 obtained in Example 1 were dissolved in warm water and this solution was cooled, 100 g of flour and 2/3 teaspoon of a blowing agent were added to the solution. The mixture obtained was made into a mass, which was then divided into 12 equal parts to prepare a skin for manju, i.e., buns with a bean-jam filling. Next, 150 g of adzuki beans were boiled in water which were then decanted. The adzuki beans thus boiled were boiled again in water until the beans were softened. The boiling water was drained through a sieve. 150 g of noncentrifugal sugar composition No.4 obtained in Example 1 were added to the beans.
  • the skin itself exhibits flavor originated from a noncentrifugal sugar composition and, therefore, had a good taste, compared to the control with white soft sugar.
  • the cane juice was heated to about 70 °C on a plate heater and then filtered through a tubular type ultrafilter membrane (type MH-25, Daicel Chemical Industries Ltd., and an effective membrane area of 2 m 2 x 30 tubes) with a fractionating molecular weight of 100,000.
  • a tubular type ultrafilter membrane type MH-25, Daicel Chemical Industries Ltd., and an effective membrane area of 2 m 2 x 30 tubes
  • Fine liquor, sucrose solution, having Bx 58.0 and a purity of 99.3 % was mixed with this filtered cane juice having Bx 19.8 and a purity of 84.5 % to prepare sugar syrup having Bx 28.0 and a purity of 91.2 % in a blend tank.
  • This sugar syrup was then heated and evaporated from Bx 28.0 to Bx 40.0 with a first plate-type heat exchanger. Under reduced pressure, the concentrated syrup was separated from steam with a vapor separator. The concentrated syrup thus obtained was fed to a second plate-type heat exchanger and heated and evaporated from Bx 40 to Bx 65. Further, under reduced pressure, the concentrated syrup was separated from steam with a vapor separator. The concentrated syrup thus obtained was heated and evaporated from Bx 65 to Bx 93 with a third plate-type heat exchanger. Under atmospheric pressure, this concentrated syrup having Bx 93 was separated from steam with a vapor separator. The value of Bx was read from a conversion table which shows relation between liquid temperatures and Bx's of sugar liquid under atmospheric pressure. That is, because the outlet temperature of the third plate-type heat exchanger, i.e., inlet temperature of the vapor separator, was about 127 °C, the value of Bx 93 was obtained.
  • the sugar syrup which had been concentrated to Bx 93 was fed to a horizontal continuous crystallizing machine with high speed paddles (turbulizer, ex Hosokawa Micron Corporation, 800 rpm, 30 inchs paddles) and then crystallized.
  • the crystallizing machine was operated in the following conditions; a peripheral speed of the paddles of 32 m/sec., a relative humidity of heated dry air introduced into the crystallizing machine of 4.5 % (at a temperature of 85 °C) and an air volume of 12 Nm 3 /min. per ton of the granule-formed sugar discharged from the crystallizing machine per hour.
  • the concentrated sugar syrup was subjected to a strong shearing force by the paddles of the crystallizing machine to crystallize quickly.
  • the granule-formed sugar was thus prepared at a production capacity of about 1.1 tons/hour.
  • the granule-formed sugar from the crystallizing machine had a temperature of about 110 to 120 °C and a purity of 90.6 % and a moisture of 2.0 %.
  • the granule-formed sugar obtained in step 3 was introduced into a hopper in which dry air (temperature of about 45 °C and relative humidity of 25 %) was blown in a volume of 15 m 3 /min. per 30 tons of the granule-formed sugar, via a screw conveyor having a structure of efficiently removing vapor generated from the granule-formed sugar by air ventilation, that is, by blowing and sucking air.
  • dry air temperature of about 45 °C and relative humidity of 25
  • a screw conveyor having a structure of efficiently removing vapor generated from the granule-formed sugar by air ventilation, that is, by blowing and sucking air.
  • the granule-formed sugar entered the hopper from the screw conveyor, it had a temperature of about 100 °C and a moisture of 1.5 %.
  • the step of drying, cooling and conditioning the sugar in the hopper was carried out for 24 hours until the moisture of the granule-formed sugar reached equilibrium moisture.
  • the moisture of the granule-formed sugar after the conditioning was 0.8 %.
  • the granule-formed sugar was screened on a sifter having 16 mesh-screen. The part passed through the screen was granule-formed sugar product (A).
  • the granule-formed sugar thus obtained had a purity of 90.6 %, a moisture of 0.8 % and a color value (AI) of 1030. It was yellowish white granule-formed sugar with natural flavor originated from sugar cane. This granule-formed sugar had excellent properties such as excellent fluidity and less solidified.
  • the sugar syrup was prepared as in step 1 in Example 6, except that the purity of the sugar syrup was adjusted to 85.8 %. Next, the same procedures as in steps 2 and 3 in Example 6 were repeated. However, in step 3, completely crystallized one as well as incompletely crystallized one came out of the turbulizer together. In addition, remarkable adherence of solidified materials to the inside of the turbulizer occurred and, therefore, the production efficiency decreased gradually.
  • the incompletely crystallized part was fed together to the next step 4 in Example 6, that is, fed to a hopper via the screw conveyor, solidification occurred easily and, in addition, a longer processing time was needed for the step of drying, cooling and conditioning sugar, compared to that in Example 6. Further, no satisfactory product was obtained. It has been found that when a purity is so low, continuous industrial production is difficult to carry out.
  • the sugar syrup was prepared as in step 1 in Example 6, except that the purity of the sugar syrup was adjusted to 95.7 %. Next, the same procedures as in steps 2 and 3 in Example 6 were repeated.
  • the granule-formed crystallized sugar was fed to step 4 in Example 6.
  • the granule-formed sugar on the screw conveyor immediately before entering the hopper had a temperature of about 100 °C and a moisture of 1.5 % by weight. It has been found that when the purity is so high, granule-formed sugar solidify easily in a hopper in the step of drying, cooling and conditioning sugar. In addition, this granule-formed sugar was easily solidified during the storage.
  • the granule-formed sugar obtained in step 3 was dried to a moisture of 0.7 % by weight in a fluidized bed dryer, MDD-3000N, ex Fuji Paudal Co., Ltd., in which warm air of about 60 to 70 °C was blown, and then cooled in a cooler until the temperature of the granule-formed sugar became about 30 to 35 °C. Subsequently, it was conditioned in a hopper for 24 hours until the moisture of the granule-formed sugar reached equilibrium moisture. After the conditioning, in order to uniform the particle size, the granule-formed sugar was screened on a sifter to obtain granule-formed sugar product (B).
  • a fluidized bed dryer MDD-3000N, ex Fuji Paudal Co., Ltd.
  • the granule-formed sugar had a purity of 90.5 %, a moisture of 0.7 % and a color value (AI) of 1120. It was yellowish white granule-formed sugar with natural flavor originated from sugar cane.
  • the loading test was carried out as follows. Each of Product A and product B was packed in each two small sugar bags (OP20 ⁇ m/PE60 ⁇ m). A load of 120 kg was put on the whole area of these four bags. This load corresponds to a weight of 12 stacks of large sugar bags of 20 kg. These four bags were taken out and observed one month and 2 months after the test was started.
  • the granule-formed sugar product which is produced via the step of drying, cooling and conditioning sugar according to the present process is different in physical properties with simplified procedures and decreased costs of equipments, compared to the product treated according to the prior art process (i.e., three steps of drying, cooling and conditioning).
  • the granule-formed sugar product obtained by the present process and the granule-formed sugar product obtained by the prior art process had approximately the same moisture value, the granule-formed sugar product obtained by the prior art process started to solidify slightly two months after the loading test started, while the product obtained by the present process did not solidify.
  • the granule-formed sugar was slowly dried with dry air.
  • the granule-formed sugar is generally composed of crystals each of which is covered with syrup film or molasses part. Microscopically, this slow drying according to the invention enhances crystallization of sucrose contained in syrup film sufficiently to shift the granule in a stable state. Meanwhile, macroscopically, the granule-formed sugar is in a homogeneous stable state as a whole where non-crystalline parts, i.e., molasses part, is not localized and minimized in volume.
  • step of drying, cooling and conditioning sugar is carried out in one step with a hopper, it is expected that because non-crystalline parts are present very stably in the granule-formed sugar after dried, the granule-formed sugar is hard to solidify, compared to the product treated in the prior art step of drying, cooling and conditioning sugar.
  • the granule-formed sugar crystallized in step 3 was introduced to a hopper via a screw conveyor.
  • the granule-formed sugar on the screw conveyor before entering the hopper had a temperature of about 100 °C and a moisture of 1.6 % by weight.
  • air having a relative humidity of 25, 30, 35, 40, 45, 50 or 60 % was fed through the bottom of it.
  • the step of drying, cooling and conditioning sugar was carried out for 24 hours until the moisture of the granule-formed sugar reached equilibrium moisture.
  • the relation between relative humidity of the dry air and moisture of granule-formed sugar after the step of drying, cooling and conditioning sugar is as shown in Table 8.
  • step 3 granule-formed sugar was crystallized with a horizontal continuous crystallizing machine with high speed paddles in the same conditions as in Example 6.
  • the granule-formed sugar was fed via a screw conveyor to a hopper from which vapor was being sucked.
  • the moisture value of the granule-formed sugar just before entering the hopper was adjusted to 2.5, 2.0, 1.6, 1.3 or 1.0 %.
  • the states of these granule-formed sugar were observed.
  • the results are as shown in Table 10.
  • the conditions of the dry air fed through the bottom of the hopper were same as in Example 6.
  • Example 6 optimum conditions for ultrafiltration carried out in Example 6 were examined.
  • step 1 in Example 6 cane juice was filtered through a tubular type ultrafilter membrane (type MH-25, Daicel Chemical Industries Ltd., and an effective membrane area of 2 m 2 x 3 tubes) with a fractionating molecular weight of 10,000, 30,000, 40,000, 100,000, 150,000 or 500,000. Fine liquor was mixed with this filtered cane juice in a blend tank to prepare sugar syrup so that the purity of the sugar syrup was 91.0 %.
  • step 2 the sugar syrups were concentrated to Bx 93 using a plate-type heat exchanger, and then the concentrated syrup were separated from steam with a vapor separator.
  • step 3 crystallization was carried out with a horizontal continuous crystallizing machine with high speed paddles (turbulizer, ex Hosokawa Micron Corporation, 2800 rpm, 8-inch paddle) with a speed of paddles of 29.8 m/sec.
  • step 4 the step of drying, cooling and conditioning the sugar was carried out in a hopper.
  • the conditions in steps 3 and 4 were same as in Example 6.
  • Example 6 All of the steps in Example 6 were repeated except that the speed of paddles of the crystallizing machine in step 3 in Example 6 was 15, 20, 25, 30, 35, 40, 45 or 50 m/sec. The state of the granule-formed sugar just after coming out of the crystallizing machine and the drying state of it in a hopper were observed.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Confectionery (AREA)
  • Non-Alcoholic Beverages (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Beans For Foods Or Fodder (AREA)
EP19970202392 1996-07-31 1997-07-31 Zusammensetzung eines nichtzentrifugierten Zuckers und Verfahren zur Herstellung eines Zuckerproduktes Expired - Lifetime EP0826781B1 (de)

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JP21692996 1996-07-31
JP21692996 1996-07-31
JP216929/96 1996-07-31
JP19072497 1997-07-02
JP190724/97 1997-07-02
JP19072497A JP3702984B2 (ja) 1996-07-31 1997-07-02 含蜜糖組成物
JP21390897 1997-07-25
JP21390897A JP3779800B2 (ja) 1997-07-25 1997-07-25 顆粒糖製造方法
JP213908/97 1997-07-25

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0944742A1 (de) * 1996-11-15 1999-09-29 Amalgamated Research, Inc. Verfahren zur klärung von zuckerrübensaft

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110172532A (zh) * 2019-06-19 2019-08-27 福建省农业科学院亚热带农业研究所（福建省农业科学院蔗麻研究中心） 一种用桂圆提取物制作的红糖

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US3194682A (en) * 1963-04-03 1965-07-13 American Sugar Sugar product and method of producing same
US3257236A (en) * 1964-07-07 1966-06-21 Nat Sugar Refining Company Method of making sugar
GB1247866A (en) * 1968-03-15 1971-09-29 Canada And Dominion Sugar Comp Process for the production of soft sugar
GB1460614A (en) * 1974-04-16 1977-01-06 Tate & Lyle Ltd Production of crystalline sugar
US4159210A (en) * 1978-06-15 1979-06-26 Amstar Corporation Maple sugar product and method of preparing and using same
EP0052413A2 (de) * 1980-10-22 1982-05-26 Amstar Corporation Kristallisiertes, in Wasser leicht zerstreubares, wärmeempfindliche, saure oder Hochinvertzuckerstoffe enthaltendes Zuckerprodukt
US5281279A (en) * 1991-11-04 1994-01-25 Gil Enrique G Process for producing refined sugar from raw juices
EP0655507A2 (de) * 1993-11-12 1995-05-31 Applexion Verfahren zur Herstellung von Kristallzucker aus einem wässrigen Zuckersaft, z.B. Zuckerrohr-oder Zuckerrübesaft

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JPS5912278B2 (ja) * 1976-04-01 1984-03-22 三井製糖株式会社 甘庶汁から栄養糖を製造する方法

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Publication number Priority date Publication date Assignee Title
US3194682A (en) * 1963-04-03 1965-07-13 American Sugar Sugar product and method of producing same
US3257236A (en) * 1964-07-07 1966-06-21 Nat Sugar Refining Company Method of making sugar
GB1247866A (en) * 1968-03-15 1971-09-29 Canada And Dominion Sugar Comp Process for the production of soft sugar
GB1460614A (en) * 1974-04-16 1977-01-06 Tate & Lyle Ltd Production of crystalline sugar
US4159210A (en) * 1978-06-15 1979-06-26 Amstar Corporation Maple sugar product and method of preparing and using same
EP0052413A2 (de) * 1980-10-22 1982-05-26 Amstar Corporation Kristallisiertes, in Wasser leicht zerstreubares, wärmeempfindliche, saure oder Hochinvertzuckerstoffe enthaltendes Zuckerprodukt
US5281279A (en) * 1991-11-04 1994-01-25 Gil Enrique G Process for producing refined sugar from raw juices
EP0655507A2 (de) * 1993-11-12 1995-05-31 Applexion Verfahren zur Herstellung von Kristallzucker aus einem wässrigen Zuckersaft, z.B. Zuckerrohr-oder Zuckerrübesaft

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0944742A1 (de) * 1996-11-15 1999-09-29 Amalgamated Research, Inc. Verfahren zur klärung von zuckerrübensaft
EP0944742A4 (de) * 1996-11-15 2001-01-24 Amalgamated Res Inc Verfahren zur klärung von zuckerrübensaft

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EP0826781A3 (de) 2000-01-12
EP0826781B1 (de) 2004-11-24
DE69731697D1 (de) 2004-12-30
AU731295B2 (en) 2001-03-29

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