EP0797686B1 - Procede et installation de fabrication d'une solution pure de sucres simples par hydrolyse d'au moins un sucre compose en presence d'un adsorbant selectif - Google Patents
Procede et installation de fabrication d'une solution pure de sucres simples par hydrolyse d'au moins un sucre compose en presence d'un adsorbant selectif Download PDFInfo
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- EP0797686B1 EP0797686B1 EP95941780A EP95941780A EP0797686B1 EP 0797686 B1 EP0797686 B1 EP 0797686B1 EP 95941780 A EP95941780 A EP 95941780A EP 95941780 A EP95941780 A EP 95941780A EP 0797686 B1 EP0797686 B1 EP 0797686B1
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- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K3/00—Invert sugar; Separation of glucose or fructose from invert sugar
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- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K1/00—Glucose; Glucose-containing syrups
- C13K1/06—Glucose; Glucose-containing syrups obtained by saccharification of starch or raw materials containing starch
Definitions
- the invention relates to a method and a installation for manufacturing a liquid solution of simple sugars (oses) from a liquid solution comprising at least one compound sugar (oside), and in particular a holoside (polysaccharide or oligosaccharide) such as sucrose, inulin, starch ...
- a holoside polysaccharide or oligosaccharide
- the compound sugars have, at these temperatures, high viscosity. It is not possible in convenient to use a starting solution strongly concentrated in compound sugar, and a concentration step should be scheduled after hydrolysis.
- FR-A-1526 029 describes a method of discoloration of juices, syrups, molasses and even sewers sweets allowing to transform in whole or in part sucrose including a bleaching step by ion exchange resins, with partial hydrolysis or total, a purification and discoloration step by ion exchange resins and a concentration step.
- the starting materials being very loaded with cations and anions, the resins are quickly saturated, so this process cannot find practical applications in industry.
- this process is in several steps, and requires a low input concentration (20 at 30 brix).
- the invention aims to overcome these disadvantages in proposing a method and an installation of manufacturing a solution of simple sugars in profitable conditions on an industrial scale.
- the subject of the invention is therefore a method and an installation which make it possible, by hydrolysis, simple sugars in solution with a yield, reaction rate and purity high enough to consider producing them industrial at a reasonable cost price and for limited industrial investments.
- the invention aims to propose a process which can be implemented works in installations of small size and capacity or medium.
- the invention further aims to provide such a process and such an installation compatible with ecological constraints of respect for the environment, especially without producing effluents.
- the invention thus aims to provide a sugar manufacturing process and installation simple in one step, continuous and solvent-free extraction by hydrolysis of a solution of sugar (s) compound (s).
- the invention also aims to provide a process and installation for manufacturing a solution pure, especially colorless, of simple sugars by hydrolysis.
- the invention aims to propose a method of manufacturing, in a single step and continuously of a aqueous solution of simple sugars of agri-food quality, especially colorless and more particularly comprising less than 1% of hydrolysis residues other than simple sugars.
- the invention also aims to provide a process for manufacturing a solution of simple sugars by hydrolysis of a solution of sugar (s) compound (s) having a conversion rate greater than 95% obtained with duration reaction time (or residence time) of less than 4 hours.
- the invention also aims to provide a process and installation for manufacturing a solution aqueous of simple sugars by hydrolysis at a temperature higher than 50 ° C - in particular of the order of 85 ° C - of a highly concentrated sugar solution (s) - especially whose weight proportion of dry matter is greater than 60% -.
- the invention relates more particularly to propose a manufacturing process and installation production of a pure and colorless solution of oses, in particular glucose and fructose- by hydrolysis of a polysaccharide (s) and / or oligosaccharide (s) solution - especially starch or sucrose.
- oses in particular glucose and fructose- by hydrolysis of a polysaccharide (s) and / or oligosaccharide (s) solution - especially starch or sucrose.
- the invention relates to a process for manufacturing a solution of simple sugars from a liquid solution comprising at least one sugar compound, by hydrolysis in the presence of a catalysis system heterogeneous (i.e. one or more catalysts solids), characterized in that the reaction medium is put hydrolysis on contact with at least one adsorbent compound microporous solid chosen to be compatible with hydrolysis and catalysis conditions and to adsorb selectively residues or by-products other than simple sugars under the reaction conditions of hydrolysis.
- the component (s) adsorbent (s) is (are) chosen (s) not to adsorb the (the) starting sugar (s).
- a microporous solid adsorbent compound which can be used in a process according to the invention is a mineral compound of natural or synthetic origin formed by three-dimensional sequences of tetrahedra T04 with T representing at least two different elements of the periodic classification such as Si, Al, B , Fe, Ga, Ge etc. In this sequence, the oxygen atoms of the T0 4 tetrahedra are in common with the neighboring tetrahedra.
- a solid microporous adsorbent compound is a solid having pores of dimensions generally less than about 10 -9 m.
- an absorbent microporous solid compound is distinguished from macroporous solids (whose pores have dimensions generally greater than 10 -8 m) such as resins, and mesoporous solids (whose pores have dimensions generally between 2.10 -9 m and 10 -8 m).
- the adsorbent compound (s) microporous solid (s) which captures (s) the by-products, it is possible to carry out the reaction at high temperature with a high conversion rate and a high initial sugar concentration, especially above 65 brix, for example of the order of 68 brix.
- the solution obtained is a syrup of great purity in simple sugars, and in particular is colorless.
- a tectosilicate or a clay is used under proton form as a heterogeneous acid catalyst of the hydrolysis reaction. Indeed, we see that such a catalyst provides conversion of the compound sugar greater than 99% in less than 2 h, with a optimal selectivity for simple sugars greater than 80%.
- zeolite aluminosilicate in protonic form, such as faujasite Y in H form of Si / Al ratio between 2 and 100, especially between 10 and 20, advantageously from around 15.
- the heterogeneous catalyst can itself have a role of selective adsorbent. However, we choose the catalyst so that it does not absorb sugars, and in particular, simple sugars.
- the invention relates in particular to a process for manufacturing a solution comprising at least a hexose from a solution comprising at least one holoside (such as sucrose) hydrolyzable to at least hexose (such as fructose and glucose).
- a solution comprising at least a hexose from a solution comprising at least one holoside (such as sucrose) hydrolyzable to at least hexose (such as fructose and glucose).
- holoside such as sucrose
- hexose such as fructose and glucose
- the invention is used as solid adsorbent compound microporous a molecular sieve whose porosity (pore and channel size) is defined for selectively adsorb by-products other than simple sugars and the starting sugar (s), and in particular to adsorb the molecules of by-products stained and / or HMF molecules.
- solid microporous adsorbent compound a tectosilicate or a clay, in particular an adsorbent zeolite, or alumina.
- a solid microporous adsorbent compound making simultaneously as a catalyst or catalyst support for hydrolysis.
- the reaction medium is brought into contact with a adsorbent zeolite, in particular in proton form, or in partially calcined ammonium form, which acts both heterogeneous acid catalyst and sieve molecular adsorbing unwanted products such as dyes and HMF.
- a adsorbent zeolite in particular in proton form, or in partially calcined ammonium form, which acts both heterogeneous acid catalyst and sieve molecular adsorbing unwanted products such as dyes and HMF.
- At least one compound is used solid microporous adsorbent separate from the catalyst heterogeneous.
- a zeolite in the form proton as a heterogeneous acid catalyst, and uses, as a microporous solid adsorbent compound, an adsorbent zeolite forming a molecular sieve of which the acidity is low but nevertheless compatible with the acid catalysis.
- This second variant offers the advantage of allow separate control of the catalysis of hydrolysis, and adsorption of dyes or HMF or other unwanted by-products.
- the hydrolysis reaction is carried out in a multicontact reactor -in particular a pulsed column of reaction / extraction- continuously.
- the minus a solid microporous adsorbent compound preferably preformed, in particular in extruded form, flowing against the current of the reaction medium.
- the solid microporous adsorbent compound can be regenerated into continuous especially by calcination after its passage in the reactor, then recycled to the reactor inlet.
- a heterogeneous catalyst in powder and we circulate this catalyst in cocurrent dispersion of the reaction medium in the reactor.
- the heterogeneous catalyst and the (the) microporous solid adsorbent compound (s) and circulates this mixture of solids against the current of the reaction medium.
- the weight proportion of the material dry sugar (s) compound (s) can be greater than 60% (syrup of more than 60 brix) -in particular around 65% at 70% (syrup from 65 brix to 70 brix) -.
- the catalyst is used heterogeneous at a rate of 1% to 20% -in particular of the order of 7.5% - by weight of the dry matter of the solution departure.
- the adsorbent compound is used microporous solid at a rate of 2% to 40% -in particular of around 15% - by weight of the dry matter of the starting solution.
- a weight of adsorbent compound (when this adsorbent compound microporous solid is distinct from the heterogeneous catalyst) greater than the weight of the heterogeneous catalyst, in particular the order of twice the weight of the heterogeneous catalyst.
- microporous solid adsorbent compounds can be used simultaneously, each of them having properties selective adsorption defined to adsorb a by-product or a family of by-products.
- a solid microporous adsorbent compound able to adsorb HMF and another adsorbent compound microporous solid capable of adsorbing dyes and / or polymers.
- the ability of a molecular sieve to adsorb selectively this or that product depends on its structure in space, the size of pores, cages and channels that it contains and physico-chemical affinities.
- one or more can be used heterogeneous catalysts simultaneously producing effects separate.
- catalysts can be used which have distinct exhaustion rates, and / or catalysts promoting subsequent reactions of hydrolysis, for example isomerization of glucose to fructose...
- the reaction is carried out at a temperature between 60 ° C and 150 ° C -in particular of the order of 80 ° C to 85 ° C-, and we use solid catalyst (s) and adsorbent compound (s) microporous compatible with this temperature. He is at note in particular that the tectosilicates are resistant perfectly at this temperature range.
- the time of stay of the reaction medium in the reactor is lower at 2 o'clock and is in particular between 0.5 hour and 1 hour.
- the starting solution has at least one oside selected from the group consisting of inulin (polysaccharide), starch (polysaccharide), sucrose (oligosaccharide), maltose (oligosaccharide), cellobiose (oligosaccharide) or lactose (oligosaccharide).
- inulin polysaccharide
- starch polysaccharide
- sucrose oligosaccharide
- maltose oligosaccharide
- cellobiose oligosaccharide
- lactose oligosaccharide
- the invention relates in particular to a process for manufacturing a colorless solution of oses to from starch or sucrose in a liquid medium by hydrolysis in the presence of a heterogeneous acid catalyst.
- the starting solution (and therefore the reaction medium and the final solution) is an aqueous solution.
- the invention also relates to an installation for implementing a method according to the invention.
- a installation according to the invention is characterized in that that it includes at least one reactor and means for put a reaction medium for hydrolysis of a solution liquid comprising at least one compound sugar, on contact a heterogeneous hydrolysis catalysis system and at minus a solid microporous absorbent compound.
- the installation is characterized in that it comprises at least one column pulsed, and means for circulating simultaneously in continuous in the pulsed column the reaction medium hydrolysis liquid, the heterogeneous catalysis system hydrolysis and the solid absorbent compound (s) microporous.
- the installation is characterized in that it includes means for circulating the absorbent compound (s) microporous solid (s) against the current of the medium hydrolysis liquid reaction.
- the pulsed column makes not only as a separator, but also and especially a continuous multicontact reactor.
- the hydrolysis reaction and the selective extraction in continuous by-products and unwanted impurities (dyes, ).
- the starting sugar solution can be highly concentrated, the reaction time is reduced and the use of toxic or polluting solvents and effluent discharge pollutants.
- the invention also relates to a method and a sugar solution manufacturing facility simple comprising in combination all or part of the features mentioned above or below.
- the installation work of the manufacturing process according to the invention is essentially consists of a pulsed column 1 to the part lower 2 of which a solution is introduced concentrated sugar compound, especially starch or sucrose.
- a solution is introduced concentrated sugar compound, especially starch or sucrose.
- This heterogeneous catalyst is an acid catalyst, for example a zeolite Y (H) in powder form.
- This catalyst dispersed in the compound sugar solution which flows from bottom to top in column 1 is extracted with the liquid phase in which it is dispersed to the part upper 3.
- a filter 5 makes it possible to separate the catalyst of the aqueous solution of simple sugars at the outlet of the column 1.
- the catalyst recovered on filter 5 is recycled in mixer 4 either directly if it is still active, either after a regeneration step by example by passing through a calcination oven 6 or all other regeneration device appropriate according to the nature of the catalyst.
- microporous solid adsorbent compound which flows (s) by gravity from top to bottom in column 1 and which we recover at the lower part 2.
- the compound adsorbent is for example an extruded Y (H) zeolite shaped (granules, sticks, cylinders, balls, ...) forming adsorbent molecular sieve.
- the adsorbent compound microporous solid must be compatible with the catalyst acid used for hydrolysis. In particular, it should not not neutralize the acidity of the catalyst.
- the pieces of solid microporous adsorbent compound partially recovered lower 2 are transported by a device forming hydraulic lift to a sieve 7 allowing to isolate the granules and / or cylinders which are then introduced into a calcination oven 8 in which the solid microporous adsorbent compound is regenerated, products trapped in the pores of this compound being burned.
- the solid adsorbent compound microporous can be recycled and reintroduced to the part upper 2 of column 1 continuously.
- Pulsed columns are devices known vertical multicontacts in which we can maintain pulsations (see for example the document "Pulsed Perforated-Plate Columns", D.H. Logsdail, M.J. Slaten, Handbook of Solvent Extraction, Teh C. Lo Malcolm H.I. Baird, Carl Hanson, Krieger Publishing Company, Malabar, Florida, 1991, 11-2, p 335-372, incorporated by reference to this description).
- the packing (baskets and crowns, or discs and crowns) as well as the amplitude and frequency pulses are determined to get circulation continues from bottom to top of the reaction medium and the continuous circulation of solid catalyst (s) and microporous solid absorbent compound (s).
- the temperature inside the pulsed column can be maintained at the reaction temperature, in particular between 80 ° and 85 ° C.
- the weight proportions of the starting solution of compound sugar (s), of catalyst acid and microporous solid adsorbent compound (s) as indicated above by adjusting the flow rates of different components and the speed of circulation in the column 1 pulsed so that the desired conversion of the sugar (s) compound (s) is obtained at exit 3 upper part of the pulsed column 1. Thanks to the invention, a total conversion of compound sugar can be achieved despite a residence time of the reaction medium in the column pulsed 1 which is weak, in particular less than two hours.
- the variant in Figure 2 differs from that of Figure 1 only in the fact that the catalyst heterogeneous acid is no longer introduced co-current with the starting solution of sugar (s) compound (s), but circulates counter-current with the adsorbent compound (s) microporous solid (s).
- the acid catalyst is present so not in powder form, but in the form of granules and / or balls and / or cylinders to be able to flow by gravity through the pulsed column 1 of the upper part 3 to lower part 2.
- the catalyst heterogeneous acid is recovered with the adsorbent compound microporous solid at the bottom 2 of column 1 and transported by hydraulic lift to the sieve 7 which is in this case a double sieve allowing to separate the beads and / or granules and / or cylinders of acid catalyst granules and / or cylinders of solid adsorbent compound microporous.
- the particle size of the catalyst acid will be different from that of the solid adsorbent compound microporous.
- the acid catalyst is either directly reintroduced at the top 3 of column 1 if it is still active, or regenerated, by example through a calcination furnace 6 or other regeneration device, before recycling to the part superior 3.
- the solid microporous adsorbent compound follows the same circuit as that described with reference to the figure 1. It should be noted that the heterogeneous acid catalyst can also act as a selective adsorbent of one or more reaction residue (s) or by-product (s).
- the solution concentrated sugar (s) compound (s) is directly introduced at the bottom 2 and flows from bottom to high in the pulsed column 1. At the top 3, we collects the simple sugar solution directly.
- the operations of the Figure 1 of mixing in mixer 4 and filtration in filter 5 are deleted.
- Figure 3 illustrates a similar variant in Figure 1 in which the solid adsorbent compound microporous and the acid catalyst are formed of a single and same microporous solid adsorbing in protonic form.
- the variant of Figure 3 is distinguished from that of FIG. 1 only by the fact that the mixer 4, the filter 5 and the regeneration step 6 are deleted. In this variant, only one compound solid circulates in the pulsed column 1.
- sucrose syrup comprising 300 g of sucrose, 167.5 g of water and 22.5 g of zeolite Y in protonic form whose Si / Al ratio is of 15, in powder form.
- zeolite Y in protonic form whose Si / Al ratio is of 15, in powder form.
- the solution obtained is a glucose and fructose syrup with a conversion rate 95% sucrose.
- the solution is clear, transparent, but colored yellow.
- Liquid chromatographic analysis under pressure of HPLC type makes it possible to note the presence 600 ppm HMF. This presence is explained by the use too small a quantity of zeolite whose power adsorption is too low.
- the syrup is prepared in the same way as Example 1 and this syrup is kept in the mixer at 82 ° C for a period of 40 minutes.
- the final solution is a glucose and fructose solution, the conversion rate sucrose being 100%.
- Chromatographic analysis HPLC reveals the presence of 1200 ppm of HMF in the solution.
- the glucose and fructose solution is limpid, transparent, but colored yellow.
- a sucrose syrup is prepared in an identical manner to examples 1 and 2 with the 22.5 g of zeolite Y in the protonic powder form of example 1. Then 45 g of adsorbent zeolite Y in ammonium (NH 4 ) form partially calcined, extruded, shaped into cylinders and whose Si / Al ratio is 15. This zeolite has a binder and is therefore less acidic and less active than the previous one.
- the final solution is a glucose syrup and perfectly clear, transparent, colorless fructose and which remains stable for several months. Chromatography HPLC liquid reveals the presence of 60 ppm of HMF, corresponding to food purity. We note by against that the extruded adsorbent zeolite is colored beige-brown.
- Example 3 We prepare the same sucrose syrup as in Example 3 with 22.5 g of powdery zeolite and 45 g of adsorbent zeolite. We wait 40 minutes instead 25 minutes of Example 3, then cool suddenly at 25 ° C. It is found that the syrup obtained from fructose and glucose is perfectly clear, transparent, colorless, stable over several months. The conversion rate sucrose is 100%. HPLC chromatography reveals the presence of 100 to 120 ppm of HMF. The adsorbent zeolite is colored beige-brown.
- Examples 3 and 4 demonstrate that with a residence time between 25 minutes and 40 minutes, we obtains, in a batch reactor, a conversion of sucrose 95 to 100% glucose and fructose with a food purity.
- the reactions of the above examples can be performed continuously in facilities represented in the figures with still residence times weaker.
- aqueous starch syrup comprising 500 g / l of starch, and more than 20 g / l of zeolite Y in protonic form with an Si / Al ratio of 15 (Faujasite) as shown in Example 1.
- the reaction temperature is 150 ° C. and the reaction time is 60 minutes.
- the final solution is a solution of simple sugars, (the conversion rate into simple sugars is 100%) of which more than 85% glucose and less than 15% maltose.
- Maltose is a diholoside composed of two units of D glucose. So it's a glucose precursor which can be recycled into the hydrolysis starting solution.
- the invention is also applicable to hydrolysis of other sugars composed into simple sugars.
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Description
- la réaction d'hydrolyse s'effectue avec une conversion supérieure à 99 % du(des) sucre(s) composé(s) et avec une sélectivité en sucres simples supérieure à 80 %,
- le(les) composé(s) adsorbant(s) solide(s) microporeux est(sont) apte(s) à adsorber toute la quantité de résidus ou sous-produits pendant la durée de la réaction.
- une charpente tridimensionnelle formée par l'enchaínement de tétraèdres TO4, SiO4, T représentant un élément de classification tel que Al, B, Ga, Ge, ... et,
- un réseau monodimensionnel, bidimensionnel, ou tridimensionnel de canaux et cavités de dimensions moléculaires contenant des cations de compensation éventuels, de l'eau ou d'autres molécules ou sels.
- la figure 1 est un schéma illustrant une installation de mise en oeuvre d'un procédé selon une première variante de l'invention,
- la figure 2 est un schéma illustrant une installation de mise en oeuvre d'un procédé selon une deuxième variante de l'invention,
- la figure 3 est un schéma illustrant une installation de mise en oeuvre d'un procédé selon une troisième variante de l'invention.
Claims (28)
- Procédé de fabrication d'une solution de sucres simples à partir d'une solution liquide comprenant au moins un sucre composé, par hydrolyse en présence d'un système de catalyse hétérogène, caractérisé en ce qu'on met le milieu réactionnel d'hydrolyse au contact d'au moins un composé adsorbant solide microporeux choisi pour être compatible avec les conditions d'hydrolyse et de catalyse et pour adsorber sélectivement les résidus ou sous-produits autres que les sucres simples dans les conditions réactionnelles de l'hydrolyse.
- Procédé selon la revendication 1 de fabrication d'une solution comprenant au moins un hexose à partir d'une solution comprenant au moins un holoside hydrolysable en au moins un hexose, caractérisé en ce qu'on utilise, à titre de composé adsorbant solide microporeux, un tamis moléculaire apte à adsorber les molécules d'hydroxyméthylfurfural et/ou de sous-produits colorés.
- Procédé selon l'une des revendications 1 et 2, caractérisé en ce qu'on choisit le système de catalyse et le(s) composé(s) adsorbant(s) solide(s) microporeux (s) de telle sorte que :la réaction d'hydrolyse s'effectue avec une conversion supérieure à 99 % du(des) sucre(s) composé(s) et avec une sélectivité en sucres simples supérieure à 80 %,le(s) composé(s) adsorbant(s) solide(s) microporeux est(sont) apte(s) à adsorber toute la quantité de résidus ou sous-produits pendant la durée de la réaction.
- Procédé selon l'une des revendications 1 à 3, caractérisé en ce qu'on utilise un tectosilicate ou une argile à titre composé adsorbant solide microporeux.
- Procédé selon la revendication 4, caractérisé en ce qu'on utilise une zéolithe adsorbante à titre de composé adsorbant solide microporeux.
- Procédé selon la revendication 5, caractérisé en ce que la zéolithe adsorbante est sous forme ammonium.
- Procédé selon l'une des revendications 1 à 6, caractérisé en ce qu'on utilise un catalyseur faisant aussi office de composé adsorbant solide microporeux.
- Procédé selon l'une des revendications 1 à 6, caractérisé en ce qu'on utilise un composé adsorbant solide microporeux distinct du catalyseur hétérogène.
- Procédé selon la revendication 8, caractérisé en ce qu'on utilise un poids àe composé adsorbant solide microporeux supérieur au poids de catalyseur hétérogène, -notamment àe l'ordre du double àu poids au catalyseur hétérogène-.
- Procédé selon l'une des revendications 1 à 9, caractérisé en ce qu'on choisit le catalyseur hétérogène et les conditions opératoires de façon à minimiser la formation de l'hydroxyméthylfurfural et/ou de sous-produits colorants.
- Procédé selon l'une des revendications 1 à 10, caractérisé en ce qu'on utilise un tectosilicate ou une argile sous forme protonique à titre de catalyseur hétérogène.
- Procédé selon la revendication 11, caractérisé en ce qu'on utilise, à titre de catalyseur hétérogène, une zéolithe sous forme protonique de rapport Si/Al compris entre 2 et 100.
- Procédé selon la revendication 11, caractérisé en ce qu'on utilise une faujasite Y sous forme H.
- Procédé selon l'une des revendications 12 et 13, caractérisé en ce qu'on utilise une zéolithe sous forme protonique de rapport Si/Al compris entre 10 et 20, notamment de l'ordre de 15.
- Procédé selon l'une des revendications 1 à 14, caractérisé en ce qu'on réalise l'hydrolyse dans un réacteur multicontact -notamment une colonne pulsée (1) de réaction/extraction- en continu, et en ce qu'on fait circuler le (les) composé(s) adsorbant(s) solide(s) microporeux à contre-courant du milieu réactionnel.
- Procédé selon la revendication 15, caractérisé en ce qu'on utilise un composé solide préformé notamment sous forme extrudée, circulant à contre-courant, à titre de composé adsorbant solide microporeux.
- Procédé selon l'une des revendications 15 et 16, caractérisé en ce qu'on régénère le composé adsorbant solide microporeux après son passage dans le réacteur (1) et en ce qu'on le recycle à l'entrée du réacteur.
- Procédé selon l'une des revendications 15 à 17, caractérisé en ce qu'on utilise un catalyseur hétérogène en poudre et en ce qu'on fait circuler ce catalyseur en dispersion à co-courant du milieu réactionnel.
- Procédé selon la revendication 8 et l'une des revendications 15 à 18, caractérisé en ce qu'on mélange un catalyseur hétérogène et le (les) composé(s) adsorbant(s) solide(s) microporeux, et en ce qu'on fait circuler le mélange à contre-courant du milieu réactionnel.
- Procédé selon l'une des revendications 1 à 19, caractérisé en ce qu'on utilise une solution de départ dont la proportion pondérale de la matière sèche en sucre(s) composé(s) est supérieure à 60 % -notamment de l'ordre de 65 % à 70 %-.
- Procédé selon l'une des revendications 1 à 20, caractérisé en ce qu'on utilise le catalyseur hétérogène à raison de 1 % à 20 % -notamment de l'ordre de 7,5 %- en poids de la matière sèche de la solution de départ.
- Procédé selon l'une des revendications 1 à 21, caractérisé en ce qu'on utilise le composé adsorbant solide microporeux à raison de 2 % à 40 % -notamment de l'ordre de 15 %- en poids de la matière sèche de la solution de départ.
- Procédé selon l'une des revendications 1 à 22, caractérisé en ce qu'on effectue la réaction à une température comprise entre 60° C et 150° C - notamment de l'ordre de 80° C à 85° C- et en ce qu'on utilise des catalyseur(s) et composé(s) adsorbant(s) solide(s) microporeux compatible(s) avec cette température.
- Procédé selon la revendication 14 et l'une des revendications 1 à 23, caractérisé en ce que le temps de séjour du milieu réactionnel dans le réacteur (1) est inférieur à 2 heures -notamment est compris entre 0,5 heure et 1 heure-.
- Procédé selon l'une des revendications 1 à 24 caractérisé en ce que la solution de départ comporte au moins un oside choisi dans le groupe formé de l'inuline, l'amidon, le saccharose, le maltose, le cellobiose ou le lactose.
- Installation pour la mise en oeuvre d'un procédé selon l'une des revendications 1 à 25, caractérisée en ce qu'elle comporte au moins un réacteur (1), et des moyens pour mettre un milieu réactionnel d'hydrolyse d'une solution liquide comprenant au moins un sucre composé au contact d'un système de catalyse hétérogène d'hydrolyse et d'au moins un composé absorbant solide microporeux.
- Installation selon la revendication 26, caractérisée en ce qu'elle comporte au moins une colonne pulsée (1) et des moyens pour faire circuler simultanément en continu dans la colonne pulsée (1) le milieu réactionnel liquide d'hydrolyse, le système de catalyse hétérogène d'hydrolyse et le (les) composés absorbant(s) solide(s) microporeux.
- Installation selon la revendication 27, caractérisée en ce qu'elle comporte des moyens pour faire circuler le (les) composés absorbant(s) solide(s) microporeux à contre-courant du milieu réactionnel liquide d'hydrolyse.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR9414961A FR2727980A1 (fr) | 1994-12-07 | 1994-12-07 | Procede de fabrication d'une solution pure de sucres simples par hydrolyse d'au moins un sucre compose en presence d'un adsorbant selectif |
FR9414961 | 1994-12-07 | ||
PCT/FR1995/001615 WO1996017962A1 (fr) | 1994-12-07 | 1995-12-06 | Procede et installation de fabrication d'une solution pure de sucres simples par hydrolyse d'au moins un sucre compose en presence d'un adsorbant selectif |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0797686A1 EP0797686A1 (fr) | 1997-10-01 |
EP0797686B1 true EP0797686B1 (fr) | 1999-04-14 |
Family
ID=9469738
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP95941780A Expired - Lifetime EP0797686B1 (fr) | 1994-12-07 | 1995-12-06 | Procede et installation de fabrication d'une solution pure de sucres simples par hydrolyse d'au moins un sucre compose en presence d'un adsorbant selectif |
Country Status (8)
Country | Link |
---|---|
US (1) | US5888306A (fr) |
EP (1) | EP0797686B1 (fr) |
AT (1) | ATE178947T1 (fr) |
AU (1) | AU4308796A (fr) |
CA (1) | CA2207061A1 (fr) |
DE (1) | DE69509121D1 (fr) |
FR (1) | FR2727980A1 (fr) |
WO (1) | WO1996017962A1 (fr) |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
NL1001956C2 (nl) * | 1995-12-21 | 1997-06-24 | Suiker Unie | Werkwijze voor het bereiden van gezuiverd inuline. |
ITMI20031679A1 (it) * | 2003-08-29 | 2005-02-28 | Opocrin Spa | Processo per la produzione di eparine a basso peso |
US8092609B2 (en) | 2007-02-05 | 2012-01-10 | European Sugar Holdings S.A.R.L. | Sucrose inversion process |
BR112020010409B1 (pt) | 2017-11-28 | 2023-03-21 | Blue Tree Technologies Ltd | Métodos e sistemas para produzir bebidas com baixo teor de açúcar |
Family Cites Families (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US118523A (en) * | 1871-08-29 | Improvement in the preparation of fermentable saccharine matters | ||
GB240253A (en) * | 1924-07-09 | 1925-10-01 | Karel Urban | Improvements in the purification of sugar solutions |
US2332758A (en) * | 1941-05-28 | 1943-10-26 | American Maize Prod Co | Method of making starch conversion products |
DE1136676B (de) * | 1957-03-21 | 1962-09-20 | Usines De Melle S A | Verfahren zur kontinuierlichen Durchfuehrung katalytischer Reaktionen in fluessiger Phase |
FR1526029A (fr) * | 1967-03-09 | 1968-05-24 | Procédé pour l'obtention d'un sirop concentré, pour et incolore de saccharose et de suere interverti, plus particulièrement à partir de bas produits de sucrerie | |
US3963788A (en) * | 1974-08-20 | 1976-06-15 | Kruse Walter M | Polyhydric alcohol production using ruthenium zeolite catalyst |
GB1516435A (en) * | 1976-06-08 | 1978-07-05 | Toray Industries | Separating fructose from a mixture of sugars |
US4746368A (en) * | 1986-02-28 | 1988-05-24 | Akzo America Inc. | Decolorization of aqueous saccharide solutions and sorbents therefor |
FI88933C (fi) * | 1990-10-15 | 1993-07-26 | Xyrofin Oy | Foerfarande foer produktion av glukos och fruktos av sackaros |
FR2697023B1 (fr) * | 1992-10-16 | 1994-12-30 | Roquette Freres | Polymère soluble hypocalorique du glucose et procédé de préparation de ce polymère . |
-
1994
- 1994-12-07 FR FR9414961A patent/FR2727980A1/fr active Pending
-
1995
- 1995-12-06 DE DE69509121T patent/DE69509121D1/de not_active Expired - Lifetime
- 1995-12-06 AT AT95941780T patent/ATE178947T1/de not_active IP Right Cessation
- 1995-12-06 AU AU43087/96A patent/AU4308796A/en not_active Abandoned
- 1995-12-06 EP EP95941780A patent/EP0797686B1/fr not_active Expired - Lifetime
- 1995-12-06 CA CA002207061A patent/CA2207061A1/fr not_active Abandoned
- 1995-12-06 US US08/849,396 patent/US5888306A/en not_active Expired - Fee Related
- 1995-12-06 WO PCT/FR1995/001615 patent/WO1996017962A1/fr active IP Right Grant
Also Published As
Publication number | Publication date |
---|---|
AU4308796A (en) | 1996-06-26 |
CA2207061A1 (fr) | 1996-06-13 |
WO1996017962A1 (fr) | 1996-06-13 |
US5888306A (en) | 1999-03-30 |
ATE178947T1 (de) | 1999-04-15 |
DE69509121D1 (de) | 1999-05-20 |
MX9704209A (es) | 1997-09-30 |
FR2727980A1 (fr) | 1996-06-14 |
EP0797686A1 (fr) | 1997-10-01 |
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