EP0629707A2 - Process for softening a sugar containing juice such as molasses and the application thereof to a process for the recovery of the sugars contained in this juice - Google Patents

Process for softening a sugar containing juice such as molasses and the application thereof to a process for the recovery of the sugars contained in this juice Download PDF

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Publication number
EP0629707A2
EP0629707A2 EP94401313A EP94401313A EP0629707A2 EP 0629707 A2 EP0629707 A2 EP 0629707A2 EP 94401313 A EP94401313 A EP 94401313A EP 94401313 A EP94401313 A EP 94401313A EP 0629707 A2 EP0629707 A2 EP 0629707A2
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EP
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Prior art keywords
ions
resin
sugars
liquid effluent
sweet juice
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EP94401313A
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German (de)
French (fr)
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EP0629707B1 (en
EP0629707A3 (en
Inventor
Xavier Lancrenon
Michael Saska
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Applexion SAS
Louisiana State University and Agricultural and Mechanical College
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Applexion SAS
Louisiana State University and Agricultural and Mechanical College
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    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B35/00—Extraction of sucrose from molasses
    • C13B35/02—Extraction of sucrose from molasses by chemical means
    • C13B35/06—Extraction of sucrose from molasses by chemical means using ion exchange
    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B20/00—Purification of sugar juices
    • C13B20/14—Purification of sugar juices using ion-exchange materials
    • C13B20/144—Purification of sugar juices using ion-exchange materials using only cationic ion-exchange material

Definitions

  • the subject of the present invention is a process for softening a sweet juice such as a candy molasses and its use in a process for recovering the sugars contained in this sweet juice.
  • the sugar cane or sugar beet industry produces significant amounts of non-crystallizable sweet juice known as candy molasses. Since this molasses has a non-negligible sugar content, it is usual to subject it to an appropriate treatment in order to extract the major part of the sugars which it contains. This treatment consists in particular in subjecting the molasses to an ion exclusion chromatography using a fixed support constituted by a strong cationic resin, in the Na+ and / or K+ form.
  • the sugar molasses contains significant quantities of dissolved calcium and / or magnesium salts, the said resin becomes charged with Ca2+ and / or Mg2+ ions during the chromatography operation and sees this makes its separation power decrease relatively quickly. This requires the periodic interruption of the chromatography operation to regenerate the cationic resin, which implies the consumption of a regeneration reagent and a decrease in productivity.
  • the regeneration step of the process according to the invention makes astute use of one of the liquid effluents available in a sugar refinery installation, namely the so-called raffinate fraction generated during the separation by chromatography of the sugars from a sweetened sweetened juice loaded with Na+ and / or K+ ions, a fraction which was usually purely and simply rejected out of this installation.
  • raffinate fraction generated during the separation by chromatography of the sugars from a sweetened sweetened juice loaded with Na+ and / or K+ ions
  • the liquid effluent (raffinate) used in step (b) advantageously consists of that produced during the separation by chromatography of the sugars from the sweetened sweet juice obtained in step (a).
  • the invention it is also advantageous to concentrate the liquid effluent (raffinate) before its implementation in step (b), since the degree of regeneration is all the higher as the concentration of Na ions + and / or K+ of this effluent is higher. It is also advantageous according to the invention, that before bringing said resin into contact with said liquid effluent in step (b), Na+ and / or K+ ions are added to said effluent, which will further improve regeneration.
  • the cation exchange resin used in step (a) will preferably be a strong cationic resin in the Na+ and / or K+ form and that the chromatography producing the liquid effluent (raffinate) used in step (b) is preferably carried out on a strong cationic resin in the Na+ and / or K+ form with elution with water.
  • a strong cationic resin it is possible to choose in particular any resin comprising a polymer matrix, for example of the polystyrene or polyacrylate type, crosslinked by a crosslinking agent such as divinylbenzene, matrix on which are grafted cation exchange groups, such as acid groups. strongly acid sulfonic. Particular preference is given to IR 200 resin (trademark of a resin sold by Rohm and Haas).
  • the present invention further extends to sweetened sweet juice as obtained by the softening process described above.
  • said first liquid effluent (raffinate) is preferably concentrated before its use in step (iii), that Na+ and / or K+ ions may be added to said first liquid effluent before the use of the latter in step (iii), that the cation exchange resin used in step (i) is preferably a strong cationic resin in the Na+ and / or K+ form and that the chromatography used in step (ii) is preferably carried out on a strong cationic resin in the Na+ and / or K+ form with elution with water.
  • a strong cationic resin use can be made of those already mentioned above in connection with the softening process.
  • the present invention further extends to the liquid effluent enriched in sugars as obtained by the recovery process described above.
  • the installation shown by way of example in this figure comprises, in a manner known per se, two softening units 1, 2 each consisting of a column filled with a strong cationic resin, in the form Na+ and / or K +, for example the IR®200 resin sold by Rohm and Haas. These columns are each provided, at their upper part, with a conduit 3,4 for supplying candy molasses (aqueous sweet juice) previously clarified and diluted with deionized water.
  • the clarification can be carried out by any known method, for example by implementing the clarification process described in US-A-5 110 363. As for dilution, it is carried out so that the dry matter content of the molasses after dilution or preferably of the order of 10 to 70% by weight.
  • the molasses thus clarified and diluted essentially comprises sugars, mineral salts of sodium, potassium, calcium and optionally magnesium and colorings.
  • Each softening column 1, 2 is further provided, at its lower part, with a conduit 5,6 for softened molasses outlet, the conduits 5,6 both leading to a three-way valve 7 from which a conduit 8, the free end of which opens out at the top of a chromatography column 9.
  • a circulation pump 10, 11 can be provided on each conduit 5.6.
  • Each column 1,2 is finally provided, at its upper part, with a conduit 12, 13 for supplying resin regeneration liquid and, at its lower part, with a conduit 12 a , 13 a for outlet from spent regeneration liquid carrying respectively a shut-off valve 12 b , 13 b .
  • the chromatography column 9 is of the type comprising a fixed support constituted by a strong cationic resin, in the Na+ and / or K+ form, the elution liquid being of the water brought into the upper part of the column by a pipe 14.
  • This same column 9 also comprises, at its lower part, a pipe 15 for extracting a liquid effluent (raffinate) rich in sugars and a pipe 16 d extraction of a liquid effluent poor in sugars.
  • the concentration unit can be constituted by an evaporator operating under reduced pressure. It may, for example, be a simple or multiple effect falling-stream evaporator, well known in the art considered.
  • the outlet 22 ensures the evacuation of the condensates formed during the evaporation.
  • valve 7 is positioned to communicate the conduit 8 with the conduits 5 and 6, the pumps 10, 11, 18 and 24 are in operation, the pump 27 is stopped and the valves 12 b , 13 b and 28 are closed.
  • the clarified and diluted molasses (10 to 70% by weight of dry matter) is brought through conduits 3 and 4 into columns 1 and 2 where it undergoes a cation exchange, the Na+ and / or K+ ions of the resin arranged in these columns being progressively replaced by the Ca2+ and / or Mg2+ ions present in the molasses.
  • molasses is enriched in Na / and / or K+ ions and is depleted in Ca2+ and / or Mg2+ ions, while the resin is enriched in Ca2+ and / or Mg2+ ions and s 'depleted in Na+ and / or K+ ions.
  • the molasses from the columns 1,2 is then brought via the conduits 5,6, the pumps 10, 11, the valve 7 and the conduit 8 in the chromatography column 9.
  • the molasses is subjected to a separation there under the effect resin and water supplied via line 14 as an eluent.
  • the first eluted fractions (constituting the raffinate) poor in sugars and rich in sodium and / or potassium salts and dyes, are extracted via line 16 and poured into tank 20.
  • the following fractions, poor in sodium salts and / or potassium and rich in sugars are extracted via line 15.
  • the raffinate recovered in the tank 20 is brought via the conduit 19, the pump 18 and the pipe 17 into the evaporation unit 21.
  • the concentrated raffinate (preferably at 10-70% by weight of dry matter ) produced in this unit 21 is extracted from the latter by the conduit 23 and the pump 24 and poured into the tank 25.
  • the ion-exchange resin of one of the columns 1 and 2 is regenerated, for example the resin of column 1.
  • the supply of molasses to be softened is stopped, the pump 10 is stopped, valve 7 is positioned to communicate conduit 8 only with conduit 6, valve 12b is open, valve 28 is positioned to communicate conduit 26 only with conduit 29 and pump 27 is brought into operation.
  • the concentrated raffinate from tank 25 is brought via conduits 26, 29 and 12 to column 1 where said concentrated raffinate, rich in Na+ and / or K+ ions, will pass through the resin contained in the column 1 and regenerate it, the Na+ and / or K+ ions of said concentrated raffinate progressively replacing the Ca2+ and / or Mg2+ ions of the resin.
  • the concentrated raffinate which, during its passage through the resin, is enriched in Ca2+ and / or Mg2+ ions is then evacuated via line 12 a .
  • the second and third cycles are then repeated at regular time intervals.
  • the flow of clarified and diluted molasses (10 to 70% by weight of dry matter) through each column 1,2 may be of the order 0.1 to 5 times the volume of the resin bed / hour and that during the regeneration operation, the flow rate of regeneration liquid (concentrated raffinate present in the tank 25 and containing 10 to 70% by weight of dry matter) through each column 1.2 may be of the order of 0.1 to 5 times the volume of the resin bed / hour.
  • these flow rates will be chosen according to the dry matter content of the liquid used.
  • the higher the dry matter content of the molasses the lower the molasses flow rate through the columns 1,2 will be for the softening operation.
  • the higher the dry matter content of the regeneration liquid (concentrated raffinate) the lower the flow rate of this liquid through the columns 1,2.
  • the temperature of the regeneration liquid will be adjusted so as to have a liquid having a viscosity suitable for the regeneration operations; this may be in the range of 20 to 70 ° C depending on the dry matter content.
  • Na+ and / or K+ ions in the form of NaCl and / or KCl for example
  • the concentrated raffinate for example at the level of tank 25.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Saccharide Compounds (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)
  • Non-Alcoholic Beverages (AREA)
  • Treatment Of Water By Ion Exchange (AREA)

Abstract

The invention relates to a process for softening an aqueous sugar (sugar cane) juice containing sugars and Ca<2+> and/or Mg<2+> ions, such as a sugar refinery molasses, by means of a cation-exchange resin, in the Na<+> and/or K<+> form, and for regenerating the said resin, which comprises: (a) a softening stage consisting in bringing the said sugar juice into contact with the said cation-exchange resin, in the Na<+> and/or K<+> form, in order to obtain, on the one hand, a softened sugar juice depleted in Ca<2+> and/or Mg<2+> ions and loaded with Na<+> and/or K<+> ions and, on the other hand, a cation-exchange resin loaded with Ca<2+> and/or Mg<2+> ions, and (b) a stage for regeneration of the latter resin, characterised in that the regeneration stage (b) consists in bringing the said resin into contact with a liquid effluent produced during the separation by chromatography of the sugars of a softened aqueous sugar juice containing sugars and Na<+> and/or K<+> ions, this liquid effluent containing the greater part of the Na<+> and/or K<+> ions initially present in the softened sugar juice.

Description

La présente invention a pour objet un procédé d'adoucissement d'un jus sucré tel qu'une mélasse de sucrerie et son utilisation dans un procédé de récupération des sucres contenus dans ce jus sucré.The subject of the present invention is a process for softening a sweet juice such as a candy molasses and its use in a process for recovering the sugars contained in this sweet juice.

L'industrie sucrière de la canne à sucre ou de la betterave sucrière produit des quantités importantes de jus sucré non cristallisable désigné sous le nom de mélasse de sucrerie. Cette mélasse présentant une teneur en sucres non négligeables, il est usuel de la soumettre à un traitement approprié pour en extraire la majeure partie des sucres qu'elle contient. Ce traitement consiste notamment à soumettre la mélasse à une chromatographie d'exclusion d'ions faisant appel à un support fixe constitué par une résine cationique forte, sous la forme Na⁺ et/ou K⁺. Toutefois, étant donné que la mélasse de sucrerie contient des quantités non négligeables de sels de calcium et/ou de magnésium dissous, ladite résine se charge en ions Ca²⁺ et/ou Mg²⁺ au cours de l'opération de chromatographie et voit de ce fait son pouvoir de séparation diminuer relativement rapidement. Ceci nécessite l'interruption périodique de l'opération de chromatographie pour régénérer la résine cationique, ce qui implique la consommation d'un réactif de régénération et une baisse de productivité.The sugar cane or sugar beet industry produces significant amounts of non-crystallizable sweet juice known as candy molasses. Since this molasses has a non-negligible sugar content, it is usual to subject it to an appropriate treatment in order to extract the major part of the sugars which it contains. This treatment consists in particular in subjecting the molasses to an ion exclusion chromatography using a fixed support constituted by a strong cationic resin, in the Na⁺ and / or K⁺ form. However, since the sugar molasses contains significant quantities of dissolved calcium and / or magnesium salts, the said resin becomes charged with Ca²⁺ and / or Mg²⁺ ions during the chromatography operation and sees this makes its separation power decrease relatively quickly. This requires the periodic interruption of the chromatography operation to regenerate the cationic resin, which implies the consumption of a regeneration reagent and a decrease in productivity.

Il a donc été proposé d'éliminer, par échange d'ions sur une résine cationique, sous la forme Na⁺ et/ou K⁺, les sels de calcium et/ou de magnésium dissous dans la mélasse avant la chromatographie de cette dernière. Etant donné qu'au cours de cet échange d'ions, les ions Na⁺ et/ou K⁺ de la résine cationique sont progressivement remplacés par les ions Ca²⁺ et/ou Mg²⁺ de la mélasse, il y a lieu de périodiquement régénérer ladite résine, ce qui est habituellement réalisé au moyen d'une solution aqueuse de NaCl. Cette technique de régénération présente essentiellement deux inconvénients : elle nécessite la consommation d'un réactif de régénération (NaCl) et elle produit des eaux usées contenant du sucre perdu. Ce système de régénération par une solution aqueuse de NaCl n'est donc pas satisfaisant sur le plan économique.It has therefore been proposed to eliminate, by ion exchange on a cationic resin, in the Na⁺ and / or K⁺ form, the calcium and / or magnesium salts dissolved in the molasses before the chromatography of the latter. Since during this ion exchange, the Na⁺ and / or K⁺ ions of the cationic resin are gradually replaced by the Ca²⁺ and / or Mg²⁺ ions of the molasses, it is necessary to periodically regenerate said resin, which is usually carried out using an aqueous NaCl solution. This regeneration technique essentially has two drawbacks: it requires the consumption of a regeneration reagent (NaCl) and it produces waste water containing lost sugar. This regeneration system with an aqueous NaCl solution is therefore not economically satisfactory.

Le but de la présente invention est donc de proposer un procédé d'adoucissement n'ayant pas les inconvénients susmentionnés. Il est ainsi proposé selon l'invention, un procédé d'adoucissement au moyen d'une résine échangeuse de cations, sous la forme Na⁺ et/ou K⁺, d'un jus sucré aqueux contenant des sucres et des ions Ca²⁺ et/ou Mg²⁺ tel qu'une mélasse de sucrerie, et de régénération de ladite résine, ce procédé comprenant :

  • (a) une étape d'adoucissement consistant à amener ledit jus sucré en contact avec ladite résine échangeuse de cations sous la forme Na⁺ et/ou K⁺, pour obtenir d'une part un jus sucré adouci appauvri en ions Ca²⁺ et/ou Mg²⁺ et chargé en ions Na⁺ et/ou K⁺ et d'autre part, une résine échangeuse de cations, chargée en ions Ca²⁺ et/ou Mg²⁺, et
  • (b) une étape de régénération de cette dernière résine,

caractérisé en ce que l'étape de régénération (b) consiste à amener ladite résine en contact avec un effluent liquide (appelé raffinat) produit lors de la séparation par chromatographie des sucres d'un jus sucré aqueux adouci contenant des sucres et des ions Na⁺ et/ou K⁺, cet effluent liquide contenant la majeure partie des ions Na⁺ et/ou K⁺ initialement présents dans le jus sucré aqueux adouci.The object of the present invention is therefore to propose a softening process which does not have the abovementioned drawbacks. It is thus proposed according to the invention, a method of softening by means of a cation exchange resin, in the form Na⁺ and / or K⁺, of an aqueous sweet juice containing sugars and Ca²⁺ and / or Mg²⁺ ions such as a sugar molasses, and of regeneration of said resin, this process comprising:
  • (a) a softening step consisting in bringing said sweet juice into contact with said cation exchange resin in the Na⁺ and / or K⁺ form, in order to obtain, on the one hand, a sweetened sweet juice depleted in Ca²⁺ ions and / or Mg²⁺ and charged with Na⁺ and / or K⁺ ions and on the other hand, a cation exchange resin, charged with Ca²⁺ and / or Mg²⁺ ions, and
  • (b) a step of regenerating this latter resin,

characterized in that the regeneration step (b) consists in bringing said resin into contact with a liquid effluent (called raffinate) produced during the separation by chromatography of the sugars from a sweetened aqueous sweet juice containing sugars and Na ions ⁺ and / or K⁺, this liquid effluent containing the major part of the Na⁺ and / or K⁺ ions initially present in the sweetened aqueous sweet juice.

Comme on le comprendra aisément, l'étape de régénération du procédé selon l'invention fait une utilisation astucieuse de l'un des effluents liquides disponibles dans une installation de sucrerie, à savoir la fraction dite raffinat générée au cours de la séparation par chromatographie des sucres d'un jus sucré adouci et chargé en ions Na⁺ et/ou K⁺, fraction qui était habituellement purement et simplement rejetée hors de cette installation. Il n'y a donc pas apport de réactif de régénération extérieur et, partant, économie par rapport au système de régénération antérieurement connu ; par ailleurs, les pertes en sucres sont moindres par rapport au système connu.As will be readily understood, the regeneration step of the process according to the invention makes astute use of one of the liquid effluents available in a sugar refinery installation, namely the so-called raffinate fraction generated during the separation by chromatography of the sugars from a sweetened sweetened juice loaded with Na⁺ and / or K⁺ ions, a fraction which was usually purely and simply rejected out of this installation. There is therefore no addition of external regeneration reagent and, therefore, economy compared to the previously known regeneration system; moreover, the sugar losses are lower compared to the known system.

L'effluent liquide (raffinat) mis en oeuvre à l'étape (b) est avantageusement constitué par celui produit lors de la séparation par chromatographie des sucres du jus sucré adouci obtenu à l'étape (a).The liquid effluent (raffinate) used in step (b) advantageously consists of that produced during the separation by chromatography of the sugars from the sweetened sweet juice obtained in step (a).

Selon l'invention, il est par ailleurs avantageux de concentrer l'effluent liquide (raffinat) avant sa mise en oeuvre à l'étape (b), puisque le degré de la régénération est d'autant plus élevé que la concentration en ions Na⁺ et/ou K⁺ de cet effluent est plus élevée. Il est également avantageux selon l'invention, qu'avant d'amener ladite résine en contact avec ledit effluent liquide à l'étape (b), des ions Na⁺ et/ou K⁺ soient ajoutés audit effluent, ce qui améliorera encore la régénération.According to the invention, it is also advantageous to concentrate the liquid effluent (raffinate) before its implementation in step (b), since the degree of regeneration is all the higher as the concentration of Na ions ⁺ and / or K⁺ of this effluent is higher. It is also advantageous according to the invention, that before bringing said resin into contact with said liquid effluent in step (b), Na⁺ and / or K⁺ ions are added to said effluent, which will further improve regeneration.

On ajoutera que la résine échangeuse de cations mise en oeuvre à l'étape (a) sera de préférence une résine cationique forte sous la forme Na⁺ et/ou K⁺ et que la chromatographie produisant l'effluent liquide (raffinat) mis en oeuvre à l'étape (b) est de préférence réalisée sur une résine cationique forte sous la forme Na⁺ et/ou K⁺ avec élution par l'eau. A titre de résine cationique forte, on pourra choisir notamment toute résine comprenant une matrice polymère par exemple du type polystyrène ou polyacrylate, réticulé par un réticulant tel que le divinylbenzène, matrice sur laquelle sont greffés des groupes échangeurs de cations, tels que des groupes acide sulfonique fortement acides. Une préférence toute particulière est donnée à la résine IR 200 (marque de fabrique d'une résine commercialisée par Rohm et Haas).It will be added that the cation exchange resin used in step (a) will preferably be a strong cationic resin in the Na⁺ and / or K⁺ form and that the chromatography producing the liquid effluent (raffinate) used in step (b) is preferably carried out on a strong cationic resin in the Na⁺ and / or K⁺ form with elution with water. As a strong cationic resin, it is possible to choose in particular any resin comprising a polymer matrix, for example of the polystyrene or polyacrylate type, crosslinked by a crosslinking agent such as divinylbenzene, matrix on which are grafted cation exchange groups, such as acid groups. strongly acid sulfonic. Particular preference is given to IR 200 resin (trademark of a resin sold by Rohm and Haas).

La présente invention s'étend en outre au jus sucré adouci tel qu'obtenu par le procédé d'adoucissement décrit ci-dessus.The present invention further extends to sweetened sweet juice as obtained by the softening process described above.

Elle s'étend par ailleurs à un procédé de récupération des sucres contenus dans un jus sucré aqueux contenant essentiellement des sucres, des ions Ca²⁺ et/ou Mg²⁺ et des colorants, tel qu'une mélasse de sucrerie, qui comprend :

  • (i) une étape d'adoucissement consistant à amener ledit jus sucré aqueux en contact avec une résine échangeuse de cations, sous la forme Na⁺et/ou K⁺, pour obtenir d'une part un jus sucré adouci appauvri en ions Ca²⁺ et/ou Mg²⁺ et chargé en ions Na⁺ et/ou K⁺ et d'autre part, une résine échangeuse de cations, chargée en ions Ca²⁺ et/ou Mg²⁺, et
  • (ii) une étape de séparation des sucres consistant à soumettre le jus sucré adouci produit à l'étape (i) à une chromatographie pour obtenir un premier effluent liquide (raffinat) enrichi en ions Na⁺ et/ou K⁺ et appauvri en sucres, et un second effluent liquide enrichi en sucres et appauvri en ions Na²⁺ et/ou K⁺,

ce procédé étant caractérisé en ce qu'il comprend en outre :
   (iii) une étape de régénération consistant à amener la résine échangeuse de cations, chargée en ions Ca²⁺ et/ou Mg²⁺ obtenue à l'étape (i) en contact avec ledit premier effluent liquide (raffinat) produit à l'étape (ii) pour obtenir d'une part, un effluent liquide enrichi en ions Ca²⁺ et/ou Mg²⁺ et d'autre part, une résine échangeuse de cations régénérée sous la forme Na⁺ et/ou K⁺.It also extends to a process for recovering the sugars contained in an aqueous sweet juice essentially containing sugars, Ca²⁺ and / or Mg²⁺ ions and dyes, such as a sugar molasses, which comprises:
  • (i) a softening step consisting in bringing said aqueous sweet juice into contact with a cation exchange resin, in the form Na⁺ e t / or K⁺, to obtain on the one hand a sweetened sweet juice depleted in Ca² ions ⁺ and / or Mg²⁺ and charged with Na⁺ and / or K⁺ ions and on the other hand, a cation exchange resin, charged with Ca²⁺ and / or Mg²⁺ ions, and
  • (ii) a sugar separation step consisting in subjecting the sweetened sweet juice produced in step (i) to chromatography to obtain a first liquid effluent (raffinate) enriched in Na⁺ and / or K⁺ ions and depleted in sugars , and a second liquid effluent enriched in sugars and depleted in Na²⁺ and / or K⁺ ions,

this process being characterized in that it further comprises:
(iii) a regeneration step consisting in bringing the cation exchange resin, charged with Ca²⁺ and / or Mg²⁺ ions obtained in step (i) in contact with said first liquid effluent (raffinate) produced in step ( ii) to obtain on the one hand, a liquid effluent enriched in Ca² en and / or Mg²⁺ ions and on the other hand, a cation exchange resin regenerated in the Na⁺ and / or K⁺ form.

On notera que ledit premier effluent liquide (raffinat) est de préférence concentré avant sa mise en oeuvre à l'étape (iii), que des ions Na⁺ et/ou K⁺ pourront être ajoutés audit premier effluent liquide avant la mise en oeuvre de ce dernier à l'étape (iii), que la résine échangeuse de cations mise en oeuvre à l'étape (i) est de préférence une résine cationique forte sous la forme Na⁺ et/ou K⁺ et que la chromatographie mise en oeuvre à l'étape (ii) est de préférence réalisée sur une résine cationique forte sous la forme Na⁺ et/ou K⁺ avec élution par l'eau. A titre de résine cationique forte, utilisation peut être faite de celles déjà mentionnées ci-dessus à propos du procédé d'adoucissement.It will be noted that said first liquid effluent (raffinate) is preferably concentrated before its use in step (iii), that Na⁺ and / or K⁺ ions may be added to said first liquid effluent before the use of the latter in step (iii), that the cation exchange resin used in step (i) is preferably a strong cationic resin in the Na⁺ and / or K⁺ form and that the chromatography used in step (ii) is preferably carried out on a strong cationic resin in the Na⁺ and / or K⁺ form with elution with water. As a strong cationic resin, use can be made of those already mentioned above in connection with the softening process.

La présente invention s'étend encore à l'effluent liquide enrichi en sucres tel qu'obtenu par le procédé de récupération décrit ci-dessus.The present invention further extends to the liquid effluent enriched in sugars as obtained by the recovery process described above.

La présente invention a enfin pour objet une installation pour la mise en oeuvre du procédé de régénération des sucres décrit ci-dessus ; cette installation comprend :

  • au moins une unité d'adoucissement contenant une résine échangeuse de cations, sous la forme Na⁺ et/ou K⁺, et comportant des moyens d'amenée de jus sucré aqueux à adoucir, des moyens d'amenée de liquide de régénération, des moyens d'extraction de jus sucré aqueux adouci et des moyens d'extraction de liquide de régénération usé, et
  • au moins une unité de chromatographie comportant des moyens d'amenée d'éluant, des moyens d'amenée de jus sucré aqueux adouci produit dans l'unité d'adoucissement et des moyens d'extraction d'un effluent liquide enrichi en ions Na⁺ et/ou K⁺ et appauvri en sucres (raffinat),

et elle se caractérise en ce qu'elle comprend en outre des moyens de liaison pour relier lesdits moyens d'amenée de liquide de régénération aux moyens d'extraction de l'unité de chromatographie, étant précisé que lesdits moyens de liaison peuvent, si on le souhaite, comprendre une unité de concentration dudit effluent liquide (raffinat) extrait par ces moyens d'extraction.The present invention finally relates to an installation for implementing the sugar regeneration process described above; this installation includes:
  • at least one softening unit containing a cation exchange resin, in the Na⁺ and / or K⁺ form, and comprising means for supplying aqueous sweet juice to be softened, means for supplying regeneration liquid, means for extracting sweetened aqueous sweet juice and means for extracting spent regeneration liquid, and
  • at least one chromatography unit comprising means for supplying eluent, means for supplying sweetened aqueous sweet juice produced in the softening unit and means for extracting a liquid effluent enriched in Na⁺ ions and / or K⁺ and depleted in sugars (raffinate),

and it is characterized in that it further comprises connection means for connecting said means for supplying regeneration liquid to the extraction means for the chromatography unit, it being specified that said connection means can, if one wish, to understand a unit of concentration of said liquid effluent (raffinate) extracted by these extraction means.

D'autres buts et avantages de la présente invention apparaîtront à la lecture de la description suivante faite en regard du dessin annexé dont la figure unique est un schéma de principe d'un mode de réalisation d'une installation de récupération des sucres d'une mélasse de sucrerie.Other objects and advantages of the present invention will appear on reading the following description made with reference to the appended drawing, the single figure of which is a block diagram of an embodiment of an installation for recovering sugars from a candy molasses.

L'installation représentée à titre d'exemple sur cette figure comprend d'une manière connue en soi deux unités d'adoucissement 1,2 constituées chacune par une colonne remplie d'une résine cationique forte, sous la forme Na⁺ et/ou K⁺, par exemple la résine IR®200 commercialisée par Rohm et Haas. Ces colonnes sont pourvues chacune, à leur partie haute, d'un conduit 3,4 d'amenée de mélasse de sucrerie (jus sucré aqueux) préalablement clarifiée et diluée par de l'eau désionisée. La clarification peut être effectuée par toute méthode connue, par exemple par mise en oeuvre du procédé de clarification décrit dans US-A-5 110 363. Quant à la dilution, elle est réalisée pour que la teneur en matière sèche de la mélasse après dilution soit de préférence de l'ordre de 10 à 70 % en poids. La mélasse ainsi clarifiée et diluée comprend essentiellement des sucres, des sels minéraux de sodium, de potassium, de calcium et éventuellement de magnésium et des colorants.The installation shown by way of example in this figure comprises, in a manner known per se, two softening units 1, 2 each consisting of a column filled with a strong cationic resin, in the form Na⁺ and / or K ⁺, for example the IR®200 resin sold by Rohm and Haas. These columns are each provided, at their upper part, with a conduit 3,4 for supplying candy molasses (aqueous sweet juice) previously clarified and diluted with deionized water. The clarification can be carried out by any known method, for example by implementing the clarification process described in US-A-5 110 363. As for dilution, it is carried out so that the dry matter content of the molasses after dilution or preferably of the order of 10 to 70% by weight. The molasses thus clarified and diluted essentially comprises sugars, mineral salts of sodium, potassium, calcium and optionally magnesium and colorings.

Chaque colonne d'adoucissement 1,2 est en outre pourvue, à sa partie basse, d'un conduit 5,6 de sortie de mélasse adoucie, les conduits 5,6 aboutissant tous deux à une vanne trois voies 7 d'où part un conduit 8 dont l'extrémité libre débouche à la partie supérieure d'une colonne de chromatographie 9. Si nécessaire, on peut prévoir une pompe de circulation 10, 11 sur chaque conduit 5,6. Chaque colonne 1,2 est enfin pourvue, à sa partie supérieure, d'un conduit 12, 13 d'amenée de liquide de régénération de la résine et, à sa partie inférieure, d'un conduit 12a, 13a de sortie de liquide de régénération usé portant respectivement une vanne de sectionnement 12b, 13b.Each softening column 1, 2 is further provided, at its lower part, with a conduit 5,6 for softened molasses outlet, the conduits 5,6 both leading to a three-way valve 7 from which a conduit 8, the free end of which opens out at the top of a chromatography column 9. If necessary, a circulation pump 10, 11 can be provided on each conduit 5.6. Each column 1,2 is finally provided, at its upper part, with a conduit 12, 13 for supplying resin regeneration liquid and, at its lower part, with a conduit 12 a , 13 a for outlet from spent regeneration liquid carrying respectively a shut-off valve 12 b , 13 b .

La colonne de chromatographie 9 est du type comprenant un support fixe constitué par une résine cationique forte, sous la forme Na⁺ et/ou K⁺, le liquide d'élution étant de l'eau amenée en partie haute de la colonne par un conduit 14. Cette même colonne 9 comporte en outre, à sa partie inférieure, un conduit 15 d'extraction d'un effluent liquide (raffinat) riche en sucres et un conduit 16 d'extraction d'un effluent liquide pauvre en sucres.The chromatography column 9 is of the type comprising a fixed support constituted by a strong cationic resin, in the Na⁺ and / or K⁺ form, the elution liquid being of the water brought into the upper part of the column by a pipe 14. This same column 9 also comprises, at its lower part, a pipe 15 for extracting a liquid effluent (raffinate) rich in sugars and a pipe 16 d extraction of a liquid effluent poor in sugars.

Conformément à l'invention, l'installation qui vient d'être décrite comprend en outre des moyens pour alimenter les conduits 12, 13 en raffinat (liquide de régénération) issu du conduit d'extraction 16. Ces moyens comprennent :

  • a) une tuyauterie 17 dont l'une des extrémités est reliée au refoulement d'une pompe 18 de mise en circulation dont l'aspiration est reliée à un conduit 19 dont l'extrémité libre s'étend jusqu'au voisinage du fond d'une cuve 20 dans laquelle débouche d'extrémité libre du conduit d'extraction 16 ;
  • b) une unité de concentration 21 pourvue d'une arrivée de liquide à concentrer reliée à la tuyauterie 17, d'une sortie 22 d'eau séparée au cours de la concentration et d'une sortie 23 de liquide concentré pourvue d'une pompe 24 d'extraction ;
  • c) une cuve 25 dans laquelle débouche la sortie 23 ; et
  • d) une tuyauterie 26 portant une pompe 27 de mise en circulation, l'une des extrémités de cette tuyauterie étant située au voisinage du fond de la cuve 25 et l'autre extrémité aboutissant à une vanne trois voies 28 de laquelle partent un conduit 29 relié au conduit 12 et un conduit 30 relié au conduit 13.
According to the invention, the installation which has just been described further comprises means for supplying the conduits 12, 13 with raffinate (regeneration liquid) coming from the extraction conduit 16. These means include:
  • a) a pipe 17, one end of which is connected to the discharge of a circulation pump 18, the suction of which is connected to a duct 19, the free end of which extends as far as the bottom of a tank 20 into which opens the free end of the extraction duct 16;
  • b) a concentration unit 21 provided with an inlet for concentrating liquid connected to the piping 17, an outlet 22 for separate water during the concentration and an outlet 23 for concentrated liquid provided with a pump 24 extraction;
  • c) a tank 25 into which the outlet 23 opens; and
  • d) a pipe 26 carrying a circulation pump 27, one end of this pipe being located near the bottom of the tank 25 and the other end leading to a three-way valve 28 from which a conduit 29 connected to conduit 12 and a conduit 30 connected to conduit 13.

L'unité de concentration peut être constituée par un évaporateur fonctionnant sous pression réduite. Il peut s'agir par exemple d'un évaporateur à flot tombant simple ou multiple effet, bien connu de la technique considérée. Dans ce cas, la sortie 22 assure l'évacuation des condensats formés au cours de l'évaporation.The concentration unit can be constituted by an evaporator operating under reduced pressure. It may, for example, be a simple or multiple effect falling-stream evaporator, well known in the art considered. In this case, the outlet 22 ensures the evacuation of the condensates formed during the evaporation.

Cette installation fonctionne de la manière suivante.This installation works as follows.

Au cours d'un premier cycle, la vanne 7 est positionnée pour faire communiquer le conduit 8 avec les conduits 5 et 6, les pompes 10, 11, 18 et 24 sont en fonctionnement, la pompe 27 est à l'arrêt et les vannes 12b, 13b et 28 sont fermées.During a first cycle, the valve 7 is positioned to communicate the conduit 8 with the conduits 5 and 6, the pumps 10, 11, 18 and 24 are in operation, the pump 27 is stopped and the valves 12 b , 13 b and 28 are closed.

La mélasse clarifiée et diluée (10 à 70 % en poids de matière sèche) est amenée par les conduits 3 et 4 dans les colonnes 1 et 2 où elle subit un échange de cations, les ions Na⁺ et/ou K⁺ de la résine disposée dans ces colonnes étant progressivement remplacés par les ions Ca²⁺ et/ou Mg²⁺ présents dans la mélasse. De ce fait, la mélasse s'enrichit en ions Na⁺ et/ou K⁺ et s'appauvrit en ions Ca²⁺ et/ou Mg²⁺, alors que la résine s'enrichit en ions Ca²⁺ et/ou Mg²⁺ et s'appauvrit en ions Na⁺ et/ou K⁺.The clarified and diluted molasses (10 to 70% by weight of dry matter) is brought through conduits 3 and 4 into columns 1 and 2 where it undergoes a cation exchange, the Na⁺ and / or K⁺ ions of the resin arranged in these columns being progressively replaced by the Ca²⁺ and / or Mg²⁺ ions present in the molasses. As a result, molasses is enriched in Na / and / or K⁺ ions and is depleted in Ca²⁺ and / or Mg²⁺ ions, while the resin is enriched in Ca²⁺ and / or Mg²⁺ ions and s 'depleted in Na⁺ and / or K⁺ ions.

La mélasse issue des colonnes 1,2 est ensuite amenée via les conduits 5,6, les pompes 10, 11, la vanne 7 et le conduit 8 dans la colonne de chromatographie 9. La mélasse y est soumise à une séparation sous l'effet de la résine et de l'eau amenée par le conduit 14 à titre d'éluant.The molasses from the columns 1,2 is then brought via the conduits 5,6, the pumps 10, 11, the valve 7 and the conduit 8 in the chromatography column 9. The molasses is subjected to a separation there under the effect resin and water supplied via line 14 as an eluent.

Les premières fractions éluées (constituant le raffinat) pauvres en sucres et riches en sels de sodium et/ou de potassium et en colorants, sont extraites par le conduit 16 et déversées dans la cuve 20. Les fractions suivantes, pauvres en sels de sodium et/ou potassium et riches en sucres sont extraites par le conduit 15.The first eluted fractions (constituting the raffinate) poor in sugars and rich in sodium and / or potassium salts and dyes, are extracted via line 16 and poured into tank 20. The following fractions, poor in sodium salts and / or potassium and rich in sugars are extracted via line 15.

Simultanément ou ultérieurement, le raffinat récupéré dans la cuve 20 est amené via le conduit 19, la pompe 18 et la tuyauterie 17 dans l'unité d'évaporation 21. Le raffinat concentré (de préférence à 10-70 % en poids de matière sèche) produit dans cette unité 21 est extrait de cette dernière par le conduit 23 et la pompe 24 et déversé dans la cuve 25.Simultaneously or later, the raffinate recovered in the tank 20 is brought via the conduit 19, the pump 18 and the pipe 17 into the evaporation unit 21. The concentrated raffinate (preferably at 10-70% by weight of dry matter ) produced in this unit 21 is extracted from the latter by the conduit 23 and the pump 24 and poured into the tank 25.

Au cours d'un deuxième cycle, la résine échangeuse d'ions de l'une des colonnes 1 et 2 est régénérée, par exemple la résine de la colonne 1. A cet effet, on arrête l'alimentation en mélasse à adoucir, la pompe 10 est arrêtée, la vanne 7 est positionnée pour faire communiquer le conduit 8 uniquement avec le conduit 6, la vanne 12b est ouverte, la vanne 28 est positionnée pour faire communiquer le conduit 26 uniquement avec le conduit 29 et la pompe 27 est amenée en fonctionnement.During a second cycle, the ion-exchange resin of one of the columns 1 and 2 is regenerated, for example the resin of column 1. To this end, the supply of molasses to be softened is stopped, the pump 10 is stopped, valve 7 is positioned to communicate conduit 8 only with conduit 6, valve 12b is open, valve 28 is positioned to communicate conduit 26 only with conduit 29 and pump 27 is brought into operation.

Dans ces conditions, le raffinat concentré de la cuve 25 est amené via les conduits 26, 29 et 12 jusqu'à la colonne 1 où ledit raffinat concentré, riche en ions Na⁺ et/ou K⁺, va traverser la résine contenue dans la colonne 1 et la régénérer, les ions Na⁺ et/ou K⁺ dudit raffinat concentré remplaçant progressivement les ions Ca²⁺ et/ou Mg²⁺ de la résine. Le raffinat concentré qui au cours de son passage à travers la résine s'est enrichi en ions Ca²⁺ et/ou Mg²⁺ est ensuite évacué par le conduit 12a.Under these conditions, the concentrated raffinate from tank 25 is brought via conduits 26, 29 and 12 to column 1 where said concentrated raffinate, rich in Na⁺ and / or K⁺ ions, will pass through the resin contained in the column 1 and regenerate it, the Na⁺ and / or K⁺ ions of said concentrated raffinate progressively replacing the Ca²⁺ and / or Mg²⁺ ions of the resin. The concentrated raffinate which, during its passage through the resin, is enriched in Ca²⁺ and / or Mg²⁺ ions is then evacuated via line 12 a .

Une fois la régénération terminée, on procède, au cours d'un troisième cycle, à la régénération de la résine de la colonne 2 tout en reprenant les opérations d'adoucissement dans la colonne 1. Ceci implique l'arrêt de l'alimentation en mélasse de la colonne 2, l'ouverture de la vanne 13b, la mise en communication du conduit 26 avec le conduit 30 par réglage approprié de la position de la vanne 28, la mise en communication du conduit 8 avec le conduit 5 par réglage approprié de la position de la vanne 7 et la reprise de l'alimentation en mélasse de la colonne 1.Once the regeneration is complete, we proceed, during a third cycle, to the regeneration of the resin in column 2 while resuming the softening operations in column 1. This involves stopping the supply of molasses in column 2, the opening of valve 13b , the communication of conduit 26 with conduit 30 by appropriate adjustment of the position of valve 28, the communication of conduit 8 with conduit 5 by adjustment appropriate position of valve 7 and resumption of molasses supply from column 1.

On répète ensuite à intervalle de temps régulier les deuxième et troisième cycles.The second and third cycles are then repeated at regular time intervals.

On ajoutera, à titre indicatif, qu'au cours de l'opération d'adoucissement, le débit de mélasse clarifiée et diluée (10 à 70 % en poids de matière sèche) à travers chaque colonne 1,2 pourra être de l'ordre de 0,1 à 5 fois le volume du lit de résine/heure et qu'au cours de l'opération de régénération, le débit en liquide de régénération (raffinat concentré présent dans la cuve 25 et contenant 10 à 70 % en poids de matière sèche) à travers chaque colonne 1,2 pourra être de l'ordre de 0,1 à 5 fois le volume du lit de résine/heure.It will be added, as an indication, that during the softening operation, the flow of clarified and diluted molasses (10 to 70% by weight of dry matter) through each column 1,2 may be of the order 0.1 to 5 times the volume of the resin bed / hour and that during the regeneration operation, the flow rate of regeneration liquid (concentrated raffinate present in the tank 25 and containing 10 to 70% by weight of dry matter) through each column 1.2 may be of the order of 0.1 to 5 times the volume of the resin bed / hour.

En fait, ces débits seront choisis en fonction de la teneur en matière sèche du liquide mis en oeuvre. Ainsi, plus la teneur en matière sèche de la mélasse est élevée et plus le débit de mélasse à travers les colonnes 1,2 sera faible pour l'opération d'adoucissement. De même, plus la teneur en matière sèche du liquide de régénération (raffinat concentré) est élevée et plus le débit de ce liquide à travers les colonnes 1,2 sera faible.In fact, these flow rates will be chosen according to the dry matter content of the liquid used. Thus, the higher the dry matter content of the molasses, the lower the molasses flow rate through the columns 1,2 will be for the softening operation. Likewise, the higher the dry matter content of the regeneration liquid (concentrated raffinate), the lower the flow rate of this liquid through the columns 1,2.

D'autre part, on règlera la température du liquide de régénération pour disposer d'un liquide ayant une viscosité appropriée pour les opérations de régénération ; celle-ci pourra se situer dans la plage de 20 à 70° C en fonction de la teneur en matière sèche.On the other hand, the temperature of the regeneration liquid will be adjusted so as to have a liquid having a viscosity suitable for the regeneration operations; this may be in the range of 20 to 70 ° C depending on the dry matter content.

On précisera encore que, si on le souhaite, des ions Na⁺ et/ou K⁺ (sous la forme de NaCl et/ou KCl par exemple) pourront être ajoutés au raffinat concentré, par exemple au niveau de la cuve 25.It will also be specified that, if desired, Na⁺ and / or K⁺ ions (in the form of NaCl and / or KCl for example) can be added to the concentrated raffinate, for example at the level of tank 25.

On notera encore que tout ou partie de NaCl et/ou KCl ainsi ajouté pourra, si on le désire, être récupéré par cristallisation du raffinat concentré ayant servi à la régénération et issue du conduit 12a et/ou 13a.It will also be noted that all or part of the NaCl and / or KCl thus added can, if desired, be recovered by crystallization of the concentrated raffinate having served for regeneration and coming from the conduit 12a and / or 13a.

Exemple de mise en oeuvre de l'inventionExample of implementation of the invention

  • 1/ Opération d'adoucissement
    • mélasse à adoucir : 15 % en poids de matière sèche ; dureté : 12000 ppm exprimés en ions Ca²⁺ par rapport à la matière sèche ;
    • résine d'adoucissement : résine IR®200 de Rohm et Haas (capacité d'échange de 1 équivalent/litre) ;
    • température : 40-80°C ;
    • débit de mélasse : 2 fois le volume du lit de résine d'adoucissement/heure ; il y a saturation de la résine après 2 heures 30 minutes de passage de mélasse ;
    • mélasse adoucie : présente une dureté moyenne de 2000 ppm exprimés en ions Ca²⁺ par rapport à la matière sèche.
    1 / Softening operation
    • molasses to be softened : 15% by weight of dry matter; hardness: 12,000 ppm expressed as Ca²⁺ ions relative to the dry matter;
    • softening resin: IR®200 resin from Rohm and Haas (exchange capacity of 1 equivalent / liter);
    • temperature : 40-80 ° C;
    • molasses flow rate : 2 times the volume of the softening resin bed / hour; there is saturation of the resin after 2 hours 30 minutes of molasses passage;
    • softened molasses : has an average hardness of 2000 ppm expressed as Ca²⁺ ions compared to the dry matter.
  • 2/ Opération de chromatographie
    • résine de chromatographie : Dowex ® C 356 de la société DOW
    • température : de l'ordre de 80° C
    • débit de mélasse adoucie : de l'ordre de 0,03 fois le volume du lit de résine de chromatographie/heure
    • débit d'eau d'élution : 16 fois le volume du lit de résine de chromatographie/heure
    • raffinat : teneur en matière sèche : ≃ 4 % en poids
    2 / Chromatography operation
    • chromatography resin : Dowex ® C 356 from DOW
    • temperature : around 80 ° C
    • softened molasses flow rate : about 0.03 times the volume of the chromatography resin bed / hour
    • elution water flow rate : 16 times the volume of the chromatography resin bed / hour
    • raffinate : dry matter content: ≃ 4% by weight
  • 3/ Opération de concentration du raffinat
    • unité de concentration : évaporateur à flot tombant (température d'évaporation ≃ 80°C)
    • teneur en matière sèche après concentration : 30 % en poids de matière sèche.
    3 / Operation of concentration of the raffinate
    • concentration unit : falling-stream evaporator (evaporation temperature ≃ 80 ° C)
    • dry matter content after concentration : 30% by weight of dry matter.
  • 4/ Régénération
    • température : 25°C
    • débit de raffinat concentré : 0,45 fois le volume de résine d'adoucissement/heure ; la régénération est terminée après passage d'un volume de raffinat concentré correspondant à 0,34 fois le volume du débit de résine.
    4 / Regeneration
    • temperature : 25 ° C
    • concentrated raffinate flow rate : 0.45 times the volume of softening resin / hour; regeneration is complete after passing a volume of concentrated raffinate corresponding to 0.34 times the volume of the resin flow rate.
  • 5/ Rinçage par l'eau de la résine d'adoucissement
    • débit d'eau : 2 fois le volume du lit de résine/heure ;
    • durée : 1 heure.
    5 / Rinsing the softening resin with water
    • water flow : 2 times the volume of the resin bed / hour;
    • duration : 1 hour.

Claims (13)

Procédé d'adoucissement au moyen d'une résine échangeuse de cations, sous la forme Na⁺ et/ou K⁺, d'un jus sucré aqueux contenant des sucres et des ions Ca²⁺ et/ou Mg²⁺ tel qu'une mélasse de sucrerie, et de régénération de ladite résine, qui comprend : (a) une étape d'adoucissement consistant à amener ledit jus sucré en contact avec ladite résine échangeuse de cations, sous la forme Na⁺ et/ou K⁺, pour obtenir d'une part un jus sucré adouci appauvri en ions Ca²⁺ et/ou Mg²⁺ et chargé en ions Na⁺ et/ou K⁺ et d'autre part, une résine échangeuse de cations, chargée en ions Ca²⁺ et/ou Mg²⁺, et (b) une étape de régénération de cette dernière résine, caractérisé en ce que l'étape de régénération (b) consiste à amener ladite résine en contact avec un effluent liquide produit lors de la séparation par chromatographie des sucres d'un jus sucré aqueux adouci contenant des sucres et des ions Na⁺ et/ou K⁺, cet effluent liquide contenant la majeure partie des ions Na⁺ et/ou K⁺ initialement présents dans le jus sucré adouci.Method of softening by means of a cation exchange resin, in the Na⁺ and / or K⁺ form, of an aqueous sweet juice containing sugars and Ca²⁺ and / or Mg²⁺ ions such as a molasses of candy, and regeneration of said resin, which comprises: (a) a softening step consisting in bringing said sweet juice into contact with said cation exchange resin, in the Na⁺ and / or K⁺ form, to obtain on the one hand a sweetened sweet juice depleted in Ca²⁺ ions and / or Mg²⁺ and charged with Na⁺ and / or K⁺ ions and on the other hand, a cation exchange resin, charged with Ca²⁺ and / or Mg²⁺ ions, and (b) a step of regenerating this latter resin, characterized in that the regeneration step (b) consists in bringing said resin into contact with a liquid effluent produced during the separation by chromatography of the sugars of a sweetened aqueous sweet juice containing sugars and Na⁺ ions and / or K⁺, this liquid effluent containing the major part of the Na⁺ and / or K⁺ ions initially present in the sweetened sweet juice. Procédé selon la revendication 1, caractérisé en ce que l'effluent liquide mis en oeuvre à l'étape (b) est celui produit lors de la séparation par chromatographie des sucres du jus sucré adouci obtenu à l'étape (a).Method according to claim 1, characterized in that the liquid effluent used in step (b) is that produced during the separation by chromatography of the sugars from the sweetened sweet juice obtained in step (a). Procédé selon la revendication 1, caractérisé en ce que l'effluent liquide est concentré avant sa mise en oeuvre à l'étape (b).Method according to claim 1, characterized in that the liquid effluent is concentrated before its implementation in step (b). Procédé selon l'une des revendications 1 à 3, caractérisé en ce qu'avant d'amener ladite résine en contact avec ledit effluent liquide à l'étape (b), des ions Na⁺ et/ou K⁺ sont ajoutés audit effluent liquide.Method according to one of claims 1 to 3, characterized in that before bringing said resin into contact with said liquid effluent in step (b), Na⁺ and / or K⁺ ions are added to said liquid effluent . Procédé selon la revendication 1, 2, 3 ou 4, caractérisé en ce que la résine échangeuse de cations mise en oeuvre à l'étape (a) est une résine cationique forte sous la forme Na⁺ et/ou K⁺, et en ce que la chromatographie produisant l'effluent liquide mis en oeuvre à l'étape (b) est réalisée sur une résine cationique forte sous la forme Na⁺ et/ou K⁺ avec élution par l'eau.Process according to claim 1, 2, 3 or 4, characterized in that the cation exchange resin used in step (a) is a strong cationic resin in the form of Na⁺ and / or K⁺, and in that that the chromatography producing the liquid effluent used in step (b) is carried out on a strong cationic resin in the Na⁺ and / or K⁺ form with elution with water. Jus sucré adouci tel qu'obtenu par le procédé selon l'une des revendications 1 à 5.Sweetened sweet juice as obtained by the process according to one of claims 1 to 5. Procédé de récupération des sucres contenus dans un jus sucré aqueux contenant essentiellement des sucres, des ions Ca²⁺ et/ou Mg²⁺ et des colorants, tel qu'une mélasse de sucrerie, qui comprend : (i) une étape d'adoucissement consistant à amener ledit jus sucré aqueux en contact avec une résine échangeuse de cations, sous la forme Na⁺ et/ou K⁺, pour obtenir d'une part un jus sucré adouci appauvri en ions Ca²⁺ et/ou Mg²⁺ et chargé en ions Na⁺ et/ou K⁺ et d'autre part, une résine échangeuse de cations, chargée en ions Ca²⁺ et/ou Mg²⁺, et (ii) une étape de séparation des sucres consistant à soumettre le jus sucré adouci produit à l'étape (i) à une chromatographie pour obtenir un premier effluent liquide enrichi en ions Na⁺ et/ou K⁺ et appauvri en sucres, et un second effluent liquide enrichi en sucres et appauvri en ions Na⁺ et/ou K⁺, caractérisé en ce qu'il comprend en outre :
   (iii) une étape de régénération consistant à amener la résine échangeuse de cations chargée en ions Ca²⁺ et/ou Mg²⁺ obtenue à l'étape (i) en contact avec ledit premier effluent liquide produit à l'étape (ii) pour obtenir d'une part, un effluent liquide enrichi en ions Ca²⁺ et/ou Mg²⁺ et d'autre part, une résine échangeuse de cations régénérée, sous la forme Na⁺ et/ou K⁺.Process for recovering the sugars contained in an aqueous sweet juice essentially containing sugars, Ca²⁺ and / or Mg²⁺ ions and colorings, such as a sugar molasses, which comprises: (i) a softening step consisting in bringing said aqueous sweet juice into contact with a cation exchange resin, in the Na⁺ and / or K⁺ form, to obtain on the one hand a sweetened sweet juice depleted in Ca²⁺ ions and / or Mg²⁺ and charged with Na⁺ and / or K⁺ ions and on the other hand, a cation exchange resin, charged with Ca²⁺ and / or Mg²⁺ ions, and (ii) a sugar separation step consisting in subjecting the sweetened sweet juice produced in step (i) to chromatography to obtain a first liquid effluent enriched in Na⁺ and / or K⁺ ions and depleted in sugars, and a second liquid effluent enriched in sugars and depleted in Na⁺ and / or K⁺ ions, characterized in that it further comprises:
(iii) a regeneration step consisting in bringing the cation exchange resin loaded with Ca²⁺ and / or Mg²⁺ ions obtained in step (i) in contact with said first liquid effluent produced in step (ii) to obtain on the one hand, a liquid effluent enriched in Ca²⁺ and / or Mg²⁺ ions and on the other hand, a regenerated cation exchange resin, in the form Na⁺ and / or K⁺. Procédé selon la revendication 7, caractérisé en ce que ledit premier effluent liquide est concentré avant sa mise en oeuvre à l'étape (iii).A method according to claim 7, characterized in that said first liquid effluent is concentrated before its implementation in step (iii). Procédé selon la revendication 7 ou 8, caractérisé en ce que des ions Na⁺ et/ou K⁺ sont ajoutés audit premier effluent avant la mise en oeuvre de ce dernier à l'étape (iii).Method according to claim 7 or 8, characterized in that Na⁺ and / or K⁺ ions are added to said first effluent before the implementation of the latter in step (iii). Procédé selon la revendication 7, 8 ou 9, caractérisé en ce que la résine échangeuse de cations mise en oeuvre à l'étape (i) est une résine cationique forte sous la forme Na⁺ et/ou K⁺ et en ce que la chromatographie mise en oeuvre à l'étape (ii) est réalisée sur une résine cationique forte sous la forme Na⁺ et/ou K⁺ avec élution par l'eau.Process according to claim 7, 8 or 9, characterized in that the cation exchange resin used in step (i) is a strong cationic resin under the Na⁺ and / or K⁺ form and in that the chromatography used in step (ii) is carried out on a strong cationic resin in the Na⁺ and / or K⁺ form with elution by water. Effluent liquide enrichi en sucres tel qu'obtenu par le procédé selon l'une quelconque des revendications 7 à 10.Liquid effluent enriched in sugars as obtained by the process according to any one of Claims 7 to 10. Installation pour la mise en oeuvre du procédé selon l'une des revendications 7 à 10 qui comprend : - au moins une unité d'adoucissement (1, 2) contenant une résine échangeuse de cations, sous la forme Na⁺ et/ou K⁺, et comportant des moyens (3, 4) d'amenée de jus sucré aqueux à adoucir, des moyens (12, 13) d'amenée de liquide de régénération, des moyens (5, 6) d'extraction de jus sucré aqueux adouci et des moyens (12a, 12b) d'extraction de liquide de régénération usé, et - au moins une unité de chromatographie (9) comportant des moyens (14) d'amenée d'éluant, des moyens (8) d'amenée de jus sucré aqueux adouci produit dans l'unité d'adoucissement (1, 2) et des moyens (16) d'extraction d'un effluent liquide enrichi en ions Na⁺ et/ou K⁺ et appauvri en sucres, caractérisée en ce qu'elle comprend en outre des moyens de liaison (17-30) pour relier lesdits moyens d'amenée de liquide de régénération aux moyens d'extraction de l'unité de chromatographie.Installation for implementing the method according to one of claims 7 to 10 which comprises: - at least one softening unit (1, 2) containing a cation exchange resin, in the Na⁺ and / or K⁺ form, and comprising means (3, 4) for supplying aqueous sweet juice to be softened, means (12, 13) for supplying regeneration liquid, means (5, 6) for extracting sweetened aqueous sweet juice and means (12 a , 12 b ) for extracting spent regeneration liquid, and at least one chromatography unit (9) comprising means (14) for supplying eluent, means (8) for supplying sweetened aqueous sweet juice produced in the softening unit (1, 2) and means (16) for extracting a liquid effluent enriched in Na⁺ and / or K⁺ ions and depleted in sugars, characterized in that it further comprises connecting means (17-30) for connecting said means for supplying regeneration liquid to the means for extracting the chromatography unit. Installation selon la revendication 12, caractérisée en ce que lesdits moyens de liaison comprennent une unité de concentration (21).Installation according to claim 12, characterized in that said connecting means comprise a concentration unit (21).
EP94401313A 1993-06-11 1994-06-10 Process for softening a sugar containing juice such as molasses and the application thereof to a process for the recovery of the sugars contained in this juice Expired - Lifetime EP0629707B1 (en)

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EP0655507A3 (en) * 1993-11-12 1996-03-20 Applexion Process for preparing crystallized sugar from aqueous sugar juice, e.g. sugar cane juice a sugar beet juice.
FR2732358A1 (en) * 1995-03-27 1996-10-04 Resindion Srl Regeneration of cationic ion-exchange resin used to treat sugar soln. from sugar beet,
FR2753456A1 (en) * 1996-09-18 1998-03-20 Generale Sucriere Sa PROCESS FOR REGENERATION OF ION EXCHANGE RESINS IN THE DECALCIFICATION PROCESS OF SWEET JUICES

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IL147529A0 (en) * 2002-01-09 2002-08-14 Oladur Ltd A method for the production of soybean sugars and the product produced thereof
FR2844151B1 (en) * 2002-09-06 2006-05-26 Applexion Ste Nouvelle De Rech METHOD FOR DECALCIFYING AQUEOUS SOLUTION AND USE THEREOF FOR LACTOSERUM DECALCIFICATION OR LACTOSERUM ULTRAFILTRATION PERMEAT
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BRPI0816467A2 (en) * 2007-08-30 2015-03-24 Iogen Energy Corp Calcium removal process and sulfate salts obtained from an aqueous sugar solution
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WO2012106761A1 (en) 2011-02-08 2012-08-16 Horizon Science Pty Ltd Sugar extracts
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CN112795710A (en) * 2020-12-08 2021-05-14 武汉美味源生物工程有限公司 Regeneration method of ion exchange resin in sugar production process
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FR2753456A1 (en) * 1996-09-18 1998-03-20 Generale Sucriere Sa PROCESS FOR REGENERATION OF ION EXCHANGE RESINS IN THE DECALCIFICATION PROCESS OF SWEET JUICES
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SK280574B6 (en) 2000-04-10
UA27814C2 (en) 2000-10-16
CN1043903C (en) 1999-06-30
MA23222A1 (en) 1994-12-31
US5443650B1 (en) 1998-05-26
AU668305B2 (en) 1996-04-26
CZ289046B6 (en) 2001-10-17
CN1111678A (en) 1995-11-15
CZ139394A3 (en) 1995-02-15
EP0629707A3 (en) 1995-02-15
PL303771A1 (en) 1995-01-09
US5443650B2 (en) 2000-05-30
PH31548A (en) 1998-11-03
SK70594A3 (en) 1995-03-08
AU6467694A (en) 1994-12-15
DE69417292D1 (en) 1999-04-29
DK0629707T3 (en) 1999-10-11
CA2125749A1 (en) 1994-12-12
DE69417292T2 (en) 1999-09-02
RU2122031C1 (en) 1998-11-20
ATE178099T1 (en) 1999-04-15
GR3030118T3 (en) 1999-07-30
ES2130375T3 (en) 1999-07-01
ZA944017B (en) 1995-02-09
US5443650A (en) 1995-08-22

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