EP1022342A1 - Process and unit for extracting a sugar juice from beet or chicory - Google Patents

Process and unit for extracting a sugar juice from beet or chicory Download PDF

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Publication number
EP1022342A1
EP1022342A1 EP00400130A EP00400130A EP1022342A1 EP 1022342 A1 EP1022342 A1 EP 1022342A1 EP 00400130 A EP00400130 A EP 00400130A EP 00400130 A EP00400130 A EP 00400130A EP 1022342 A1 EP1022342 A1 EP 1022342A1
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Prior art keywords
press
presses
rank
juice
fresh
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EP00400130A
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German (de)
French (fr)
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EP1022342B1 (en
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Robert Guyot
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Maguin SAS
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Maguin SAS
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    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B10/00—Production of sugar juices
    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B10/00—Production of sugar juices
    • C13B10/08—Extraction of sugar from sugar beet with water

Definitions

  • the present invention relates generally to a process and unit for extracting a sweet juice from beets sugar or chicory, and more particularly a process and a unit extraction in which a battery of presses connected in series.
  • the conventional methods of diffusion of the prior art employ extractors in which the cossettes are passed against the current sugar beets and a high temperature extraction solvent such as than hot water, the sugar being extracted by diffusion without there being pressing of the pods.
  • the contact time must be relatively long, which requires large extractors length and maintain the extraction solvent such as water at a high temperature over the entire extraction area; for example at a temperature of the order of 70 ° C.
  • the present invention therefore aims to provide a process for extracting a sweet juice from sugar beets or chicory requiring a less expensive infrastructure, a lower energy cost and which results in an absence of CO 2 release in the atmosphere at the level of purification.
  • the process of the invention makes it possible to obtain a juice better quality than the diffusion methods of the prior art because requiring lower temperatures, the reduced oxidation of the raw material avoids dissolving unsweetened products undesirable and limits microbial development with for consequence of the very reduced levels of organic acids in juices sweets obtained.
  • the invention also relates to a unit for producing a juice. sweet implementing the above process.
  • the first press P1 is supplied with preferably by a vertical flared feed chute, size sufficient to allow a good force-feeding of the press and also a balance perfect as possible between the sugar concentration of the phase cellulosic and liquid phase (like presses later) with fresh Ro grating from sugar beets or chicory.
  • a grater i.e. a raw material beet or chicory, reduced to medium-sized particles from 1.5 to 4 mm, unlike the commonly used caps, favors sugar extraction from cells by leaching / pressing operation.
  • the rasp pressed in the P1 press and partially exhausted R1 is introduced, as before, by a vertical chute into the P2 press of row 2.
  • the partially exhausted rasp from the P2 row 2 press is itself introduced in the press of immediately higher rank and so on until the last press Pn of the battery at the outlet of which we recover a completely exhausted Rn rasp for its storage and its transformation into animal feed.
  • the sweet juice J1 from the first press is recovered, purified and treated in a conventional manner.
  • it it is possible to use a simplified purification of the juice recovered J1 by coagulation / flocculation with a very small amount of lime (1 to 3 g / l), instead of conventional calcocarbon purification.
  • the processed juice is then decanted and the clear juice obtained is, as is conventional, sulfited then filtered.
  • the sludge extracted from the separator or decanter are filtered, for example by means of a precoat with scraping by micrometric advance knife and sugar removal cake by spraying a small amount of hot water and reintroduced into the first press P1 with the fresh grating Ro.
  • the juice Ji of a press Pi of any rank i is recycled in the Ri-2 rasp from the Pi-2 press of rank i-2, except for the J1 juice from the first press P1.
  • At least the juice J2 from the press P2 of rank 2 and recycled into fresh grating Ro is heated by means of a heater at a temperature of 60 to 80 ° C, depending on the climatic conditions outside, before being mixed with the fresh grating Ro to obtain a feed mixture of the first press P1 at a temperature of 20 to 40 ° C.
  • This addition of liquid at high temperature causes a pasteurization of the surface of the fresh grating Ro.
  • the extraction in the presses of the battery will be done at a temperature between 30 ° and 60 ° C, and if necessary can also reheat juices from presses of rows higher than means of heaters.
  • the pressing temperatures of 30-60 ° C are much higher lower than the diffusion temperatures used with the units conventional extraction, which, added to a reduced extraction time and an absence of oxidation, limits the coloring of the extracted juices.
  • An appropriate amount of water, possibly heated to the desired temperature, added upstream of the last Pn press, is generally between 20 and 50% by weight relative to the total weight of freshly grated Ro processed.
  • the amount of water will obviously vary in depending on the extraction sought and the number of presses in the battery.
  • the battery will include from 2 to 5 presses, better 3 to 4 presses.
  • the extraction rate of each press expressed as a percentage of sugar extracted in the pressing juice by compared to the sugar contained in the mixture "grating + juice or water" introduced in the press is between 50 and 80%.
  • Total battery extraction rate (extracted sugar / total sugar contained in fresh grating) is between 94 and 98.5% and depends well obviously the number of presses and the amount of water added before the last press.
  • the sweet juice recovered J1 after evaporation and crystallization conventional, allows to obtain a quality sugar EEC n ° 2 or quality slightly lower depending on the quality of the raw material in the case a grated beetroot.
  • the juice clear obtained is possibly discolored, preconcentrated and used to extract sweet compounds and insulin derivatives.
  • the process of the invention is particularly suitable for small sweets that can process up to 3000 tonnes / day of grated beets or chicory.
  • FIG. 2 shows an extraction unit according to the invention, comprising a battery of 3 twin-screw presses P1, P2, P3.
  • the fresh Ro grating is introduced in the first P1 press by the vertical chute G1 where it is pressed.
  • J1 sweet juice is routed from the press P1 by a line 1a to a tank B1, then from tank B1 via line 1b fitted with a pump to a separator S where we recover a clear juice which is transported for storage and treatment later by line 1c to a tank (not shown).
  • Sludge separated from the juice J1 in the separator S are optionally recycled in the fresh grating Ro by a pipe 4.
  • the R1 rasp, partially exhausted, from the first press P1 is routed through a pipe 2 provided with a means of advancing the grate R1 to the feed chute G2 of the press P2 where the R1 is pressed again.
  • the J2 juice extracted in the P2 press is routed through line 2a in a tank B2 and then from tank B2 by a line 2b fitted with a pump, possibly through a heater H to bring the juice J2 to a temperature of 60-80 ° C, to be mixed with fresh grating Ro.
  • the partially spent rasp R2 produced in the P2 press is routed through a pipe 3 provided with a means of advancement (pump) up to the feed chute G3 of the press P3.
  • J3 juice extracted in the press P3 is conveyed by a line 3a in a tank B3, then from tank B3 via line 3b to line 2 to be mixed with the rasp R1 from the P1 press and feeding the P2 press.
  • the grating R3 from the P3 press is conveyed, for example by a conveyor tape to a storage location.
  • Water at a temperature of 60 ° C. is introduced by via a line 5 in line 3 to be mixed with the R2 grater from the P2 press.
  • Sodium bisulfite is introduced via line 6 into the tray B3 to be mixed with the J3 juice from the P3 press and recycled in the R1 grating.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Non-Alcoholic Beverages (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)
  • Preparation Of Fruits And Vegetables (AREA)

Abstract

Sugar beet or chicory is grated to form particles 1.5 - 4 mm and supplied to the first of a series of presses. Apart from the first two presses and the last press, the juice extracted from each presses is returned to the inlet of the preceding press. Water is supplied to the inlet of the last press. Sugar juice is collected from the first press and waste material from the last press. An Independent claim is included for an apparatus as above. Preferred Features: There are 2- 5 presses. The first press operates at 30 - 60 degrees C and the second press at 60 - 80 degrees C. Anit-oxidant is added to the juice produced by the last press.

Description

La présente invention concerne d'une manière générale un procédé et une unité d'extraction d'un jus sucré à partir de betteraves sucrières ou de chicorée, et plus particulièrement un procédé et une unité d'extraction dans lesquels on utilise une batterie de presses reliées en série.The present invention relates generally to a process and unit for extracting a sweet juice from beets sugar or chicory, and more particularly a process and a unit extraction in which a battery of presses connected in series.

Les procédés classiques de diffusion de l'art antérieur emploient des extracteurs dans lesquels on fait passer à contre-courant des cossettes de betteraves sucrières et un solvant d'extraction à haute température tel que de l'eau chaude, le sucre étant extrait par diffusion sans qu'il y ait pressage des cossettes.The conventional methods of diffusion of the prior art employ extractors in which the cossettes are passed against the current sugar beets and a high temperature extraction solvent such as than hot water, the sugar being extracted by diffusion without there being pressing of the pods.

Pour obtenir une extraction convenable le temps de contact doit être relativement long, ce qui nécessite des extracteurs de grande longueur et de maintenir le solvant d'extraction tel que l'eau à une température élevée sur la totalité de la zone d'extraction; par exemple à une température de l'ordre de 70°C.To obtain a suitable extraction, the contact time must be relatively long, which requires large extractors length and maintain the extraction solvent such as water at a high temperature over the entire extraction area; for example at a temperature of the order of 70 ° C.

Ces exigences font que les coûts d'infrastructure et les coûts d'exploitation, en particulier en ce qui concerne le bilan énergétique, sont élevés.These requirements mean that infrastructure costs and costs , in particular with regard to the energy balance, are high.

En outre, ces procédés classiques se traduisent par un rejet important de CO2 dans l'atmosphère, du fait de l'épuration calcocarbonique classique du jus sucré obtenu.In addition, these conventional processes result in a significant release of CO 2 into the atmosphere, due to the conventional calcocarbon purification of the sweet juice obtained.

La présente invention a donc pour objet de fournir un procédé d'extraction d'un jus sucré à partir de betteraves sucrières ou de chicorée nécessitant une infrastructure moins coûteuse, un coût énergique moindre et qui se traduit par une absence de rejet de CO2 dans l'atmosphère au niveau de l'épuration.The present invention therefore aims to provide a process for extracting a sweet juice from sugar beets or chicory requiring a less expensive infrastructure, a lower energy cost and which results in an absence of CO 2 release in the atmosphere at the level of purification.

En outre, le procédé de l'invention permet l'obtention d'un jus sucré de meilleure qualité que les procédés de diffusion de l'art antérieur car nécessitant de plus faibles températures, l'oxydation réduite de la matière première évite la mise en solution de produits non sucrés indésirables et limite les développements microbiens avec pour conséquence des teneurs très réduites en acides organiques dans les jus sucrés obtenus.In addition, the process of the invention makes it possible to obtain a juice better quality than the diffusion methods of the prior art because requiring lower temperatures, the reduced oxidation of the raw material avoids dissolving unsweetened products undesirable and limits microbial development with for consequence of the very reduced levels of organic acids in juices sweets obtained.

L'invention concerne également une unité de production d'un jus sucré mettant en oeuvre le procédé ci-dessus.The invention also relates to a unit for producing a juice. sweet implementing the above process.

On atteint les buts ci-dessus selon l'invention au moyen d'un procédé d'extraction d'un jus sucré à partir de betteraves sucrières ou de chicorée, comprenant le traitement successif d'une râpure de betteraves sucrières ou de chicorée dans une batterie de plusieurs presses en série, le jus sucré obtenu par le pressage dans chacune des presses étant recyclé avec la râpure alimentant la presse immédiatement précédente, et une quantité d'eau étant introduite au moins dans la râpure alimentant la dernière presse.The above objects are achieved according to the invention by means of a process for extracting a sweet juice from sugar beets or chicory, including the successive treatment of a beet rasp sugar or chicory in a battery of several presses in series, the sweet juice obtained by pressing in each press being recycled with the grating feeding the immediately preceding press, and a quantity of water being introduced at least into the grating supplying the last press.

Plus précisément, le procédé selon l'invention d'extraction d'un jus sucré à partir de betteraves sucrières ou de chicorée comprend :

  • a) le râpage des betteraves ou de la chicorée en une râpure fraíche (Ro) dont les particules ont une dimension moyenne de 1,5 à 4 mm;
  • b) l'introduction de la râpure fraíche (Ro) dans une première presse (P1) d'un ensemble de n presses (Pi, i=1 à n) agencées en série de telle sorte que chacune des presses successives (Pi de rang i), autres que la première presse (P1), et jusqu'à la dernière presse (Pn) de rang n, soit alimentée par une râpure partiellement épuisée (Ri-1) provenant de la presse (Pi-1) de rang immédiatement inférieur (i-1);
  • c) la récupération à la sortie de chacune des presses (Pi) d'un jus sucré (Ji);
  • d) l'introduction du jus sucré (Ji) issu d'une presse d'un rang donné i dans la râpure (Ri-2) issue de la presse de rang i-2 et la râpure fraíche (Ro) pour le jus sucré issu de la deuxième presse P2 de rang 2;
  • e) l'introduction d'eau au moins dans la râpure partiellement épuisée (Rn-1) issue de la presse (Pn-1) de rang n-1;
  • f) la récupération de la râpure épuisée (Rn) issue de la dernière presse de rang n; et
  • h) la récupération du jus sucré (J1) issu de la première presse (P1).
    • More specifically, the method according to the invention for extracting a sweet juice from sugar beets or chicory comprises:
  • a) grating the beets or chicory into a fresh grate (Ro) whose particles have an average size of 1.5 to 4 mm;
  • b) the introduction of the fresh grating (Ro) in a first press (P1) of a set of n presses (Pi, i = 1 to n) arranged in series so that each of the successive presses (Pi of row i), other than the first press (P1), and up to the last press (Pn) of row n, is fed by a partially exhausted grating (Ri-1) coming from the press (Pi-1) of row immediately lower (i-1);
  • c) recovering at the outlet of each of the presses (Pi) a sweet juice (Ji);
  • d) introduction of the sweet juice (Ji) from a press of a given rank i into the rasp (Ri-2) from the press of rank i-2 and the fresh rasp (Ro) for the sweet juice from the second P2 row 2 press;
  • e) the introduction of water at least into the partially exhausted grating (R n-1 ) from the press (Pn-1) of rank n-1;
  • f) recovering the exhausted grating (Rn) from the last row n press; and
  • h) recovering the sweet juice (J1) from the first press (P1).

    • La suite de la description se réfère aux figures annexées qui représentent respectivement :

  • Figure 1 - un schéma de principe du procédé de l'invention; et
  • Figure 2 - un schéma d'une unité de production selon l'invention, comportant une batterie de 3 presses.
    • The following description refers to the appended figures which represent respectively:
  • Figure 1 - a block diagram of the method of the invention; and
  • Figure 2 - a diagram of a production unit according to the invention, comprising a battery of 3 presses.

    • En se référant à la figure 1, le procédé d'extraction d'un jus sucré à partir de betteraves sucrières ou de chicorée comprend une batterie de n presses Pi, i=1 à n agencées en série recevant une râpure Ro, Ri (i=1 à n-1) et fournissant par pressage de la râpure d'alimentation un jus sucré Ji, i=1 à n.Referring to Figure 1, the process of extracting a sweet juice from sugar beets or chicory includes a battery of n presses Pi, i = 1 to n arranged in series receiving a rasp Ro, Ri (i = 1 to n-1) and supplying by pressing the feed grater a sweet juice Ji, i = 1 to n.

    Plus précisément, la première presse P1 est alimentée de préférence par une goulotte verticale d'alimentation évasée, de taille suffisante pour permettre un bon gavage de la presse et un équilibre aussi parfait que possible entre la concentration en sucre de la phase cellulosique et de la phase liquide (comme d'ailleurs les presses ultérieures) avec de la râpure fraíche Ro de betteraves sucrières ou de chicorée. L'utilisation d'une râpure, c'est-à-dire d'une matière première betterave ou chicorée, réduite en particules de taille moyenne de 1,5 à 4 mm, contrairement aux cossettes habituellement utilisées, favorise l'extraction du sucre des cellules par opération de lessivage/pressage.More precisely, the first press P1 is supplied with preferably by a vertical flared feed chute, size sufficient to allow a good force-feeding of the press and also a balance perfect as possible between the sugar concentration of the phase cellulosic and liquid phase (like presses later) with fresh Ro grating from sugar beets or chicory. The use of a grater, i.e. a raw material beet or chicory, reduced to medium-sized particles from 1.5 to 4 mm, unlike the commonly used caps, favors sugar extraction from cells by leaching / pressing operation.

    La râpure pressée dans la presse P1 et partiellement épuisée R1 est introduite, comme précédemment, par une goulotte verticale dans la presse P2 de rang 2.The rasp pressed in the P1 press and partially exhausted R1 is introduced, as before, by a vertical chute into the P2 press of row 2.

    La râpure partiellement épuisée issue de la presse P2 de rang 2 est elle-même introduite dans la presse de rang immédiatement supérieur et ainsi de suite jusqu'à la dernière presse Pn de la batterie à la sortie de laquelle on récupère une râpure Rn totalement épuisée en vue de son stockage et de sa transformation en aliment pour bétail.The partially exhausted rasp from the P2 row 2 press is itself introduced in the press of immediately higher rank and so on until the last press Pn of the battery at the outlet of which we recover a completely exhausted Rn rasp for its storage and its transformation into animal feed.

    Le jus sucré J1 issu de la première presse est récupéré, épuré et traité de manière classique. Toutefois, avec le procédé de l'invention, il est possible d'utiliser une épuration simplifiée du jus récupéré J1 par coagulation/floculation avec une très petite quantité de chaux (1 à 3 g/l), au lieu de l'épuration calcocarbonique classique. Le jus traité est alors décanté et le jus clair obtenu est, comme cela est classique, sulfité puis filtré. Le cas échéant, les boues extraites du séparateur ou décanteur, de nature très visqueuse, sont filtrées, par exemple au moyen d'un filtre à précouche avec raclage par couteau à avance micrométrique et désucrage du gâteau par pulvérisation d'une faible quantité d'eau chaude et réintroduites dans la première presse P1 avec la râpure fraíche Ro.The sweet juice J1 from the first press is recovered, purified and treated in a conventional manner. However, with the method of the invention, it it is possible to use a simplified purification of the juice recovered J1 by coagulation / flocculation with a very small amount of lime (1 to 3 g / l), instead of conventional calcocarbon purification. The processed juice is then decanted and the clear juice obtained is, as is conventional, sulfited then filtered. Where appropriate, the sludge extracted from the separator or decanter, from very viscous in nature, are filtered, for example by means of a precoat with scraping by micrometric advance knife and sugar removal cake by spraying a small amount of hot water and reintroduced into the first press P1 with the fresh grating Ro.

    On peut également, pour la séparation des boues, utiliser des filtres sous vide avec média filtrant cellulosique en rouleau, récupérable ou non.It is also possible, for the separation of sludge, to use vacuum filters with rollable cellulosic filter media or not.

    Comme le montre la figure 1, les jus Ji (i=2 à n) issus des presses de rang supérieur Pi (i=2 à n) sont recyclés avec la râpure fraíche pour la presse P2 de rang 2, la râpure R1 issue de la presse P1 pour le jus J3 issu de la presse P3 et ainsi de suite jusqu'à la dernière presse Pn. En d'autres termes, le jus Ji d'une presse Pi de rang i quelconque est recyclé dans la râpure Ri-2 issue de la presse Pi-2 de rang i-2, à l'exception du jus J1 de la première presse P1.As shown in Figure 1, the juices Ji (i = 2 to n) from the presses of higher rank Pi (i = 2 to n) are recycled with the fresh grating for the press P2 of row 2, the rasp R1 from the press P1 for the juice J3 from press P3 and so on until the last press Pn. In others terms, the juice Ji of a press Pi of any rank i is recycled in the Ri-2 rasp from the Pi-2 press of rank i-2, except for the J1 juice from the first press P1.

    De préférence, au moins le jus J2 issu de la presse P2 de rang 2 et recyclé dans la râpure fraíche Ro est réchauffé au moyen d'un réchauffeur à une température de 60 à 80°C, suivant les conditions climatiques extérieures, avant d'être mélangé à la râpure fraíche Ro afin d'obtenir un mélange d'alimentation de la première presse P1 à une température de 20 à 40°C. Cet ajout de liquide à haute température provoque un effet de pasteurisation de la surface de la râpure fraíche Ro.Preferably, at least the juice J2 from the press P2 of rank 2 and recycled into fresh grating Ro is heated by means of a heater at a temperature of 60 to 80 ° C, depending on the climatic conditions outside, before being mixed with the fresh grating Ro to obtain a feed mixture of the first press P1 at a temperature of 20 to 40 ° C. This addition of liquid at high temperature causes a pasteurization of the surface of the fresh grating Ro.

    De préférence encore, l'extraction dans les presses de la batterie se fera à une température comprise entre 30° et 60°C, et si nécessaire on peut également réchauffer les jus issus des presses de rangs supérieurs au moyen de réchauffeurs.Preferably also, the extraction in the presses of the battery will be done at a temperature between 30 ° and 60 ° C, and if necessary can also reheat juices from presses of rows higher than means of heaters.

    Les températures de pressage de 30-60°C sont beaucoup plus basses que les températures de diffusion utilisées avec les unités d'extraction classiques, ce qui, ajouté à un temps d'extraction réduit et à une absence d'oxydation, limite la coloration des jus extraits.The pressing temperatures of 30-60 ° C are much higher lower than the diffusion temperatures used with the units conventional extraction, which, added to a reduced extraction time and an absence of oxidation, limits the coloring of the extracted juices.

    Une quantité appropriée d'eau, éventuellement chauffée à la température voulue, ajoutée en amont de la dernière presse Pn, est généralement comprise entre 20 et 50% en poids par rapport au poids total de râpure fraíche Ro traitée. La quantité d'eau variera bien évidemment en fonction de l'extraction recherchée et du nombre de presses de la batterie.An appropriate amount of water, possibly heated to the desired temperature, added upstream of the last Pn press, is generally between 20 and 50% by weight relative to the total weight of freshly grated Ro processed. The amount of water will obviously vary in depending on the extraction sought and the number of presses in the battery.

    De préférence, la batterie comprendra de 2 à 5 presses, mieux de 3 à 4 presses.Preferably, the battery will include from 2 to 5 presses, better 3 to 4 presses.

    Pour les presses du procédé de l'invention, on peut utiliser des presses de type bi-vis classiques, telles que, par exemple, les presses développées par la Société BABBINI.For the presses of the process of the invention, it is possible to use conventional twin-screw presses, such as, for example, presses developed by the BABBINI Company.

    Avec le procédé de l'invention, le taux d'extraction de chaque presse exprimé en pourcent de sucre extrait dans le jus de pressage par rapport au sucre contenu dans le mélange "râpure + jus ou eau" introduit dans la presse se situe entre 50 et 80%.With the process of the invention, the extraction rate of each press expressed as a percentage of sugar extracted in the pressing juice by compared to the sugar contained in the mixture "grating + juice or water" introduced in the press is between 50 and 80%.

    Le taux d'extraction total de la batterie (sucre extrait/sucre total contenu dans la râpure fraíche) se situe entre 94 et 98,5% et dépend bien évidemment du nombre de presses et de la quantité d'eau ajoutée avant la dernière presse.Total battery extraction rate (extracted sugar / total sugar contained in fresh grating) is between 94 and 98.5% and depends well obviously the number of presses and the amount of water added before the last press.

    On peut également ajouter dans les jus de pressage, de préférence dans le jus de pressage Jn de la dernière presse Pn de rang n ou l'eau introduite dans la râpure Rn-1 issue de la presse Pn-1 de rang n-1, un agent anti-oxydant tel que du bisulfite de sodium afin d'éviter les oxydations et les développements microbiens.It is also possible to add in the pressing juices, preferably in the pressing juice Jn of the last press Pn of row n or the water introduced into the rasp R n-1 from the press Pn-1 of row n-1 , an antioxidant such as sodium bisulfite to prevent oxidation and microbial growth.

    Le jus sucré récupéré J1, après évaporation et cristallisation classiques, permet l'obtention d'un sucre de qualité CEE n°2 ou de qualité légèrement inférieure suivant la qualité de la matière première dans le cas d'une râpure de betteraves. Dans le cas d'une râpure de chicorée, le jus clair obtenu est éventuellement décoloré, préconcentré et utilisé pour en extraire des composés sucrés et des dérivés de l'insuline.The sweet juice recovered J1, after evaporation and crystallization conventional, allows to obtain a quality sugar EEC n ° 2 or quality slightly lower depending on the quality of the raw material in the case a grated beetroot. In the case of a chicory grater, the juice clear obtained is possibly discolored, preconcentrated and used to extract sweet compounds and insulin derivatives.

    Le procédé de l'invention a pour avantages :

    • une diminution notable des investissements nécessaires à l'épuration des jus et de la quantité de chaux nécessaire à cette épuration, ce qui se traduit par une absence de rejet de CO2 dans l'atmosphère au niveau de l'épuration;
    • l'obtention d'un jus sucré de meilleure qualité que les jus de diffusion classiques, car l'extraction par pressage se fait à plus basse température avec une oxydation très réduite de la matière première, évite la mise en solution de certains sucres, limite les développements microbiens et une prise de coloration importante du jus au cours de la phase d'extraction;
    • enfin, l'utilisation de températures plus basses améliore le bilan énergétique du procédé.
    The process of the invention has the advantages:
    • a significant reduction in the investments necessary for the purification of the juices and in the quantity of lime necessary for this purification, which results in an absence of release of CO 2 into the atmosphere at the level of the purification;
    • obtaining a sugar juice of better quality than conventional diffusion juices, since extraction by pressing is carried out at a lower temperature with very reduced oxidation of the raw material, avoids the dissolution of certain sugars, limit microbial developments and significant coloration of the juice during the extraction phase;
    • finally, the use of lower temperatures improves the energy balance of the process.

    Le procédé de l'invention est particulièrement adapté aux sucreries de petite taille pouvant traiter jusqu'à 3000 tonnes/jour de râpures de betteraves ou de chicorée.The process of the invention is particularly suitable for small sweets that can process up to 3000 tonnes / day of grated beets or chicory.

    Exemple : Example :

    On a représenté, à la figure 2, une unité d'extraction selon l'invention, comprenant une batterie de 3 presses de type bi-vis P1, P2, P3.FIG. 2 shows an extraction unit according to the invention, comprising a battery of 3 twin-screw presses P1, P2, P3.

    La râpure fraíche Ro est introduite dans la première presse P1 par la goulotte verticale G1 où elle est pressée. Le jus sucré J1 est acheminé depuis la presse P1 par une conduite 1a jusqu'à un bac B1, puis du bac B1 par une conduite 1b munie d'une pompe jusqu'à un séparateur S où on récupère un jus clair qui est acheminé pour stockage et traitement ultérieur par la conduite 1c jusqu'à une cuve (non représentée). Les boues séparées du jus J1 dans le séparateur S sont éventuellement recyclées dans la râpure fraíche Ro par une conduite 4.The fresh Ro grating is introduced in the first P1 press by the vertical chute G1 where it is pressed. J1 sweet juice is routed from the press P1 by a line 1a to a tank B1, then from tank B1 via line 1b fitted with a pump to a separator S where we recover a clear juice which is transported for storage and treatment later by line 1c to a tank (not shown). Sludge separated from the juice J1 in the separator S are optionally recycled in the fresh grating Ro by a pipe 4.

    La râpure R1, partiellement épuisée, issue de la première presse P1 est acheminée par une conduite 2 munie d'un moyen d'avancement de la râpure R1 jusqu'à la goulotte d'alimentation G2 de la presse P2 où la râpure R1 est à nouveau pressée. Le jus J2 extrait dans la presse P2 est acheminé par la conduite 2a dans un bac B2 puis du bac B2 par une conduite 2b munie d'une pompe, éventuellement à travers un réchauffeur H pour porter le jus J2 à une température de 60-80°C, pour être mélangé avec la râpure fraíche Ro.The R1 rasp, partially exhausted, from the first press P1 is routed through a pipe 2 provided with a means of advancing the grate R1 to the feed chute G2 of the press P2 where the R1 is pressed again. The J2 juice extracted in the P2 press is routed through line 2a in a tank B2 and then from tank B2 by a line 2b fitted with a pump, possibly through a heater H to bring the juice J2 to a temperature of 60-80 ° C, to be mixed with fresh grating Ro.

    La râpure partiellement épuisée R2 produite dans la presse P2 est acheminée par une conduite 3 munie d'un moyen d'avancement (pompe) jusque dans la goulotte d'alimentation G3 de la presse P3. Le jus J3 extrait dans la presse P3 est acheminé par une conduite 3a dans un bac B3, puis du bac B3 par une conduite 3b jusque dans la conduite 2 pour être mélangé avec la râpure R1 issue de la presse P1 et alimentant la presse P2. La râpure R3 issue de la presse P3 est acheminée, par exemple par un convoyeur à bande jusqu'à un lieu de stockage.The partially spent rasp R2 produced in the P2 press is routed through a pipe 3 provided with a means of advancement (pump) up to the feed chute G3 of the press P3. J3 juice extracted in the press P3 is conveyed by a line 3a in a tank B3, then from tank B3 via line 3b to line 2 to be mixed with the rasp R1 from the P1 press and feeding the P2 press. The grating R3 from the P3 press is conveyed, for example by a conveyor tape to a storage location.

    De l'eau à une température de 60°C est introduite par l'intermédiaire d'une conduite 5 dans la conduite 3 pour être mélangée avec la râpure R2 issue de la presse P2.Water at a temperature of 60 ° C. is introduced by via a line 5 in line 3 to be mixed with the R2 grater from the P2 press.

    Du bisulfite de sodium est introduit par une conduite 6 dans le bac B3 pour être mélangé avec le jus J3 issu de la presse P3 et recyclé dans la râpure R1.Sodium bisulfite is introduced via line 6 into the tray B3 to be mixed with the J3 juice from the P3 press and recycled in the R1 grating.

    On a fait fonctionner l'installation décrite ci-dessus dans les conditions suivantes : Débit-massique de râpure fraíche Ro 1400 kg/heure Débit-massique J1 1660 kg/heure Débit-massique R1 500 kg/heure Débit-massique J2 730 kg/heure Débit-massique R2 400 kg/heure Débit-massique J3 630 kg/heure Débit-massique R3 260 kg/heure Débit-massique eau 500 kg/heure Débit-massique bisulfite de Na 20 kg/heure (solution à 3% en poids)

  • Températures mélanges dans les presses : de 25 à 40°C
  • Pureté du jus extrait J1 : 85,1%
  • Pureté du jus épuré : 95%
  • Coloration du jus épuré : 800 unités ICUMSA
  • Teneur en sucre de la râpure fraíche Ro : 15% en poids
  • Teneur en sucre de R3 : 0,7% en poids.
    • The installation described above was operated under the following conditions: Mass flow rate of fresh Ro 1400 kg / hour Mass flow J1 1660 kg / hour Mass flow R1 500 kg / hour Mass flow J2 730 kg / hour Mass flow R2 400 kg / hour Mass flow J3 630 kg / hour Mass flow R3 260 kg / hour Water mass flow 500 kg / hour Mass flow bisulfite of Na 20 kg / hour (3% by weight solution)
  • Mixing temperatures in presses: 25 to 40 ° C
  • Purity of juice extracted D1: 85.1%
  • Purity of purified juice: 95%
  • Coloring of purified juice: 800 ICUMSA units
  • Sugar content of fresh Ro cheese: 15% by weight
  • Sugar content of R3: 0.7% by weight.

    • Claims (14)

    Procédé d'extraction d'un jus sucré à partir de betteraves sucrières ou de chicorée, caractérisé en ce qu'il comprend : a) le râpage des betteraves ou de la chicorée en une râpure fraíche (Ro) dont les particules ont une dimension moyenne allant de 1,5 à 4 mm; b) l'introduction de la râpure fraíche (Ro) dans une première presse P1 d'une batterie de n presses (Pi, i=1 à n) agencées en série de telle sorte que chacune des presses successives (Pi) de rang i supérieur à 1 jusqu'à la dernière presse (Pn) et à l'exception de la première presse (P1) soient alimentées par une râpure partiellement épuisée (Ri) provenant de la presse de rang immédiatement inférieur (i-1); c) la récupération à la sortie de chacune des presses (Pi, i=1 à n) d'un jus sucré (Ji, i=1 à n); d) l'introduction du jus sucré issu d'une presse d'un rang donné i dans la râpure issue de la presse de rang i-2 et la râpure fraíche pour le jus sucré issu de la deuxième presse (P2) de rang i=2; e) l'introduction d'eau au moins dans la râpure partiellement épuisée issue de la presse (Pn-1) de rang n-1; f) la récupération de la râpure épuisée issue de la presse de rang n; et g) la récupération du jus sucré (J1) issu de la première presse (P1). Process for extracting a sweet juice from sugar beets or chicory, characterized in that it comprises: a) grating the beets or chicory into a fresh grate (Ro) whose particles have an average size ranging from 1.5 to 4 mm; b) the introduction of the fresh grating (Ro) in a first press P1 of a battery of n presses (Pi, i = 1 to n) arranged in series so that each of the successive presses (Pi) of rank i greater than 1 until the last press (Pn) and with the exception of the first press (P1) are fed by a partially exhausted rasp (Ri) coming from the press of immediately lower rank (i-1); c) recovery at the outlet of each of the presses (Pi, i = 1 to n) of a sweet juice (Ji, i = 1 to n); d) the introduction of the sweet juice from a press of a given row i into the grater from the press of row i-2 and the fresh grater for the sweet juice from the second press (P2) of row i = 2; e) the introduction of water at least into the partially exhausted grating from the press (Pn-1) of rank n-1; f) recovering the exhausted grating from the row n press; and g) recovering the sweet juice (J1) from the first press (P1). Procédé selon la revendication 1, caractérisé en ce que le nombre de presse n varie de 2 à 5.Method according to claim 1, characterized in that the number of press n varies from 2 to 5. Procédé selon la revendication 1 ou 2, caractérisé en ce que la quantité d'eau introduite dans la râpure issue de la presse (Pn-1) de rang n-1 représente 20 à 50% en poids du poids total de râpure fraíche traitée.Method according to claim 1 or 2, characterized in that than the quantity of water introduced into the grater from the press (Pn-1) of rank n-1 represents 20 to 50% by weight of the total weight of grating fresh processed. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le pressage de la râpure fraíche (Ro) dans la première presse (P1) s'effectue à une température de 30 à 60°C.Method according to any of the claims previous, characterized in that the pressing of the fresh grating (Ro) in the first press (P1) is carried out at a temperature of 30 to 60 ° C. Procédé selon l'une quelconque des revendications 1 à 4, caractérisé en ce qu'au moins le jus (J2) issu de la seconde presse (P2) est réchauffé à une température de 60 à 80°C avant d'être ajouté à la râpure fraíche (Ro).Process according to any one of Claims 1 to 4, characterized in that at least the juice (J2) from the second press (P2) is heated to a temperature of 60 to 80 ° C before being added to the fresh grating (Ro). Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce qu'un agent anti-oxydant est ajouté au jus (Jn) issu de la dernière presse (Pn) de rang n.Method according to any of the claims above, characterized in that an antioxidant is added to the juice (Jn) from the last press (Pn) of rank n. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le jus sucré (J1) issu de la première presse (P1) est soumis à une étape de séparation des boues pour récupérer un jus sucré clair, les boues séparées étant soit éliminées, soit recyclées dans la râpure fraíche (Ro) d'alimentation de la première presse (P1).Method according to any of the claims above, characterized in that the sweet juice (J1) from the first press (P1) is subjected to a sludge separation step to recover a clear sweet juice, the separated sludge being either eliminated, either recycled in the fresh feed grater (Ro) of the first press (P1). Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le nombre n de presses est au moins égal à 3.Method according to any one of the preceding claims, characterized in that the number n of presses is at least equal to 3. Unité de production d'un jus sucré à partir de râpures de betteraves sucrières ou de chicorées, lesdites râpures étant constituées de particules ayant une dimension moyenne de 1,5 à 4 mm, caractérisée en ce qu'il comprend : un ensemble comprenant n presses (Pi, i=1 à n) reliées en série; des moyens pour acheminer et introduire dans chaque presse Pi de rang i, une râpure (Ri-1) partiellement épuisée provenant de la presse de rang i-1 immédiatement inférieur, à l'exception de la première presse (P1) qui est alimentée avec une râpure fraíche (Ro); des moyens pour acheminer et introduire un jus sucré (Ji, i=1 à n) issu de chacune des presses de rang i supérieur à 1 dans la râpure partiellement épuisée issue de chacune des presses de rang i-2, respectivement et la râpure fraíche (Ro) pour la presse de rang i=2; un moyen pour introduire de l'eau dans la râpure (Rn-1) issue de la presse (Pn-1) de rang n-1; un moyen pour récupérer le jus sucré (J1) issu de la première presse (P1) de la série; et un moyen pour acheminer la râpure épuisée (Rn) issue de la dernière presse (Pn) de rang n vers une décharge. Unit for producing a sweet juice from sugar beet or chicory grates, said grates consisting of particles having an average size of 1.5 to 4 mm, characterized in that it comprises: an assembly comprising n presses (Pi, i = 1 to n) connected in series; means for conveying and introducing into each press Pi of rank i, a partially exhausted rasp (Ri-1) coming from the press of rank i-1 immediately lower, with the exception of the first press (P1) which is supplied with a fresh grate (Ro); means for conveying and introducing a sweet juice (Ji, i = 1 to n) from each of the presses of rank i greater than 1 into the partially exhausted rasp from each of the presses of rank i-2, respectively and the fresh rasp (Ro) for the press of row i = 2; means for introducing water into the grating (Rn-1) from the press (Pn-1) of rank n-1; means for recovering the sweet juice (J1) from the first press (P1) of the series; and means for conveying the spent rasp (Rn) from the last press (Pn) of rank n to a landfill. Unité d'extraction selon la revendication 9, caractérisée en ce qu'elle comprend un séparateur (S) recevant le jus sucré issu de la première presse (P1) pour en éliminer les boues.Extraction unit according to claim 9, characterized in that it comprises a separator (S) receiving the sweet juice from the first press (P1) to remove the sludge. Unité d'extraction selon la revendication 10, caractérisée en ce qu'elle comprend un moyen pour recycler les boues séparées par le séparateur (S) avec la râpure fraíche (Ro) introduite dans la première presse (P1).Extraction unit according to claim 10, characterized in that it includes means for recycling the sludge separated by the separator (S) with the fresh grating (Ro) introduced into the first press (P1). Unité d'extraction selon l'une quelconque des revendications 9 à 11, caractérisée en ce qu'elle comprend un moyen éventuel (H) pour réchauffer le jus sucré (J2) issu de la presse (P2) de rang 2 à une température de 60 à 80°C.Extraction unit according to any one of Claims 9 to 11, characterized in that it comprises means optional (H) to heat the sweet juice (J2) from the press (P2) of row 2 at a temperature of 60 to 80 ° C. Unité d'extraction selon l'une quelconque des revendications 9 à 12, caractérisée en ce qu'elle comprend un moyen pour introduire un agent anti-oxydant dans le jus sucré (Jn) issu de la dernière presse (Pn) de rang n.Extraction unit according to any one of Claims 9 to 12, characterized in that it comprises means to introduce an antioxidant agent in the sweet juice (Jn) from the last press (Pn) of row n. Unité d'extraction selon l'une quelconque des revendications 9 à 13, caractérisée en ce que le nombre n de presses est au moins égal à 3.Extraction unit according to any one of the claims 9 to 13, characterized in that the number n of presses is at less than 3.
    EP00400130A 1999-01-21 2000-01-19 Process and unit for extracting a sugar juice from beet or chicory Expired - Lifetime EP1022342B1 (en)

    Applications Claiming Priority (2)

    Application Number Priority Date Filing Date Title
    FR9900652 1999-01-21
    FR9900652A FR2788785B1 (en) 1999-01-21 1999-01-21 PROCESS AND UNIT FOR EXTRACTING SUGAR JUICE FROM BEET OR CHICORE

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    EP1022342B1 EP1022342B1 (en) 2004-07-14

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    AT (1) ATE271136T1 (en)
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    Cited By (4)

    * Cited by examiner, † Cited by third party
    Publication number Priority date Publication date Assignee Title
    FR2839073A1 (en) * 2002-04-26 2003-10-31 Sucre Rech & Dev Production of an inulin solution comprises treating a chicory root extract with a coagulant and then a flocculant
    EP1063302B1 (en) * 1999-06-25 2008-04-16 Maguin S.A. Process for extracting sugar syrup
    FR2928817A1 (en) * 2008-03-19 2009-09-25 Ecopsi Soc Par Actions Simplif PROCESS AND UNIT FOR PRODUCING BETTRAVES AND SUGAR JUICE DRECHES FROM BETTRAVES
    WO2014096656A1 (en) 2012-12-18 2014-06-26 Lesaffre Et Compagnie Process for purifying beet juice

    Families Citing this family (1)

    * Cited by examiner, † Cited by third party
    Publication number Priority date Publication date Assignee Title
    DE102014006046A1 (en) * 2014-04-24 2015-10-29 Richard Hartinger Method and device for producing a vegetable sweetener

    Citations (4)

    * Cited by examiner, † Cited by third party
    Publication number Priority date Publication date Assignee Title
    DE736734C (en) * 1939-07-02 1943-06-25 Fraembs & Freudenberg Process for juicing sugar beets
    FR2489840A1 (en) * 1980-09-05 1982-03-12 Ital Ind Degli Zuccheri PROCESS AND PLANT FOR THE EXTRACTION OF BEET SUGAR AND PRODUCTS OBTAINED BY THIS PROCESS
    FR2502909A1 (en) * 1981-04-03 1982-10-08 Alsthom Atlantique PROCESS FOR THE EXTRACTION OF JUICE FROM TUBERS, ESPECIALLY TOPINAMBOURS AND INSTALLATION IMPLEMENTING THE PROCESS
    WO1990010719A2 (en) * 1989-03-10 1990-09-20 Sugana Zucker-Gesellschaft M.B.H. Mulitistage process for extracting sugar from sugar beet and special raw sugar obtained

    Patent Citations (4)

    * Cited by examiner, † Cited by third party
    Publication number Priority date Publication date Assignee Title
    DE736734C (en) * 1939-07-02 1943-06-25 Fraembs & Freudenberg Process for juicing sugar beets
    FR2489840A1 (en) * 1980-09-05 1982-03-12 Ital Ind Degli Zuccheri PROCESS AND PLANT FOR THE EXTRACTION OF BEET SUGAR AND PRODUCTS OBTAINED BY THIS PROCESS
    FR2502909A1 (en) * 1981-04-03 1982-10-08 Alsthom Atlantique PROCESS FOR THE EXTRACTION OF JUICE FROM TUBERS, ESPECIALLY TOPINAMBOURS AND INSTALLATION IMPLEMENTING THE PROCESS
    WO1990010719A2 (en) * 1989-03-10 1990-09-20 Sugana Zucker-Gesellschaft M.B.H. Mulitistage process for extracting sugar from sugar beet and special raw sugar obtained

    Cited By (7)

    * Cited by examiner, † Cited by third party
    Publication number Priority date Publication date Assignee Title
    EP1063302B1 (en) * 1999-06-25 2008-04-16 Maguin S.A. Process for extracting sugar syrup
    FR2839073A1 (en) * 2002-04-26 2003-10-31 Sucre Rech & Dev Production of an inulin solution comprises treating a chicory root extract with a coagulant and then a flocculant
    FR2928817A1 (en) * 2008-03-19 2009-09-25 Ecopsi Soc Par Actions Simplif PROCESS AND UNIT FOR PRODUCING BETTRAVES AND SUGAR JUICE DRECHES FROM BETTRAVES
    WO2009125088A2 (en) * 2008-03-19 2009-10-15 Ecopsi Beet processing process and unit
    WO2009125088A3 (en) * 2008-03-19 2011-12-01 Lesaffre Et Compagnie Beet processing method
    US9326534B2 (en) 2008-03-19 2016-05-03 Lesaffre Et Comopagnie Beet processing process and unit
    WO2014096656A1 (en) 2012-12-18 2014-06-26 Lesaffre Et Compagnie Process for purifying beet juice

    Also Published As

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    EP1022342B1 (en) 2004-07-14
    DE60012054D1 (en) 2004-08-19
    FR2788785B1 (en) 2001-04-06
    FR2788785A1 (en) 2000-07-28
    DE60012054T2 (en) 2005-08-25
    ATE271136T1 (en) 2004-07-15
    ES2225033T3 (en) 2005-03-16

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