FR2633940A1 - Glyoxal-treated scleroglucan and process for preparing it - Google Patents

Glyoxal-treated scleroglucan and process for preparing it Download PDF

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FR2633940A1
FR2633940A1 FR8809100A FR8809100A FR2633940A1 FR 2633940 A1 FR2633940 A1 FR 2633940A1 FR 8809100 A FR8809100 A FR 8809100A FR 8809100 A FR8809100 A FR 8809100A FR 2633940 A1 FR2633940 A1 FR 2633940A1
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scleroglucan
glyoxal
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solution
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FR2633940B3 (en
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Yves Huet
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Sanofi SA
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Sanofi SA
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0006Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
    • C08B37/0024Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/04Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds

Abstract

The subject of the present invention is the scleroglucan obtained by treating natural polysaccharide with 0.5 to 10 % by weight of glyoxal. Its subject is also three variants of the said treatment process.

Description

Scléroglucane traité au glyoxal et son procédé d'obtention.Scleroglucan treated with glyoxal and its process for obtaining.

La présente invention concerne le produit résultant du traitement du scléroglucane par le glyoxal et le procédé de traitement. The present invention relates to the product resulting from the treatment of scleroglucan with glyoxal and the method of treatment.

Le scléroglucane est un polysaccharide, constitoé de chaînes ramifiées d'unités D-Glucose, secrété notamment par des champignons du type Sclérotium, qui a été décrit pour la première fois dans le brevet US 3,301,848. Scleroglucan is a polysaccharide, constitated with branched chains of D-Glucose units, secreted in particular by fungi of the Sclerotium type, which has been described for the first time in US Pat. No. 3,301,848.

Ce composé peut être utilisé, pour ses propriétés gélifiantes et épaississantes en milieu aqueux, dans les industries cosmétique, alimentaire, pharmaceutique ou pétrolière. Dans toutes ces applications, il est très souhaitable que la poudre de polymère se mouille et se disperse facilement dans l'eau, sans qu'une agitation violente soit nécessaire et sans la formation de grumeaux, ce qui n'est pas le cas du polymère naturel isolé de façon classique par précipitation alcoolique du milieu de fermentation, et cela quelle que soit la granulométrie de la poudre. This compound can be used, for its gelling and thickening properties in an aqueous medium, in the cosmetics, food, pharmaceutical or petroleum industries. In all these applications, it is highly desirable that the polymer powder be wetted and dispersed easily in water, without the need for violent agitation and without the formation of lumps, which is not the case with the polymer. natural isolated in a conventional manner by alcoholic precipitation of the fermentation medium, and this whatever the particle size of the powder.

I1 est connu que le traitement par le glyoxal d'une macromolécule hydroxylée et notamment du xanthane, donne des produits à dispersibilité aqueuse améliorée, mais ceci n'avait jamais été décrit pour le scléroglucane. On a constaté que dans ce cas, la dispersibilité était suffisamment améliorée dans une large gamme de pH, de force ionique et de température pour qu'une agitation manuelle ou mécanique simple soit suffisante pour assurer la dissolution de la poudre sans formation de grumeaux.En outre, la solubilisation du polymère traité, et donc l'épaississement des solutions, s' effectue plus lentement, ce qui peut être avantageux dans la préparation de compositions nécessitant le mélange de plusieurs produits insolubles, ou dans les applications pétrolières lors du colmatage des voies d'eau ; enfin, si la viscosité des solutions de scléroglucane traité est plus faible au moment de la solubilisation, elle atteint en quelquesminutes la valeur des solutions du polysaccharide naturel.  It is known that treatment with glyoxal of a hydroxylated macromolecule and in particular xanthan gives products with improved aqueous dispersibility, but this has never been described for scleroglucan. It was found that in this case the dispersibility was sufficiently improved over a wide range of pH, ionic strength and temperature so that simple manual or mechanical agitation was sufficient to ensure the dissolution of the powder without lumping. in addition, the solubilization of the treated polymer, and therefore the thickening of the solutions, is carried out more slowly, which may be advantageous in the preparation of compositions requiring the mixing of several insoluble products, or in petroleum applications during clogging of the channels water; finally, if the viscosity of the treated scleroglucan solutions is lower at the time of solubilization, it reaches in a few minutes the value of the solutions of the natural polysaccharide.

On peut traiter le scléroglucane par une solution aqueuse de glyoxal soit lorsqu'il est encore en solution dans le milieu de fermentation avant sa précipitation par addition d'alcool, soit après mise en suspension dans un alcool ou même en humectant simplement la poudre de scléroglucane par une solution hydroalcoolique de glyoxal ; ainsi, selon l'invention, le scléroglucane est traité en solution, en suspension ou sensiblement à sec par 0,5 à 10 % en poids de glyoxal par rapport au poids du polysaccharide. The scleroglucan can be treated with an aqueous solution of glyoxal either when it is still in solution in the fermentation medium before its precipitation by the addition of alcohol, or after being suspended in an alcohol or even simply by moistening the scleroglucan powder. by a hydroalcoholic solution of glyoxal; thus, according to the invention, the scleroglucan is treated in solution, in suspension or substantially dry by 0.5 to 10% by weight of glyoxal relative to the weight of the polysaccharide.

Selon la première variante, on ajoute dans le moût en fin d'une fermentation classique, de 0,5 à 10 % en poids de glyoxal par rapport au poids du polysaccharide présent, et on le maintient à une température comprise entre 100C et 800C pendant 1 à 16 heures avant de traiter le milieu de façon classique, c'est-à-dire avant thermisation, précipitation par addition d'un alcool, comme l'éthanol ou l'isopropanol, isolement du précipité contenant le polysaccharide, séchage et broyage. On ajoute de préférence le glyoxal sous forme de solution aqueuse à 30 %. According to the first variant, 0.5 to 10% by weight of glyoxal relative to the weight of the polysaccharide present is added to the must at the end of a conventional fermentation, and is maintained at a temperature of between 100 ° C. and 800 ° C. 1 to 16 hours before treating the medium in a conventional manner, that is to say before thermization, precipitation by addition of an alcohol, such as ethanol or isopropanol, isolation of the precipitate containing the polysaccharide, drying and grinding . Glyoxal is preferably added as a 30% aqueous solution.

La durée du traitement est fonction de la concentration du milieu en glyoxal et de la température ; le pH peut être compris entre 2 et 7. The duration of the treatment depends on the concentration of the medium in glyoxal and the temperature; the pH can be between 2 and 7.

Dans la seconde variante, le scléroglucane, juste précipité du milieu de fermentation ou la poudre de scléroglucane obtenue dans une fabrication antérieure est mis en suspension dans un alcool, qui peut être un alcool jamais utilisé ou celui ayant servi à laver un précipité de scléroglucane précédemment isolé, en présence de 0,5 à 10 % en poids de glyoxal par rapport au poids de scléroglucane et le milieu est agité de 30 minutes à 8 heures avant filtration pour isoler le scléroglucane traité qui sera séché de façon classique vers 600C. Le glyoxal est de préférence introduit dans l'alcool, en solution aqueuse concentrée à 30 Gt environ. In the second variant, the scleroglucan just precipitated from the fermentation medium or the scleroglucan powder obtained in an earlier manufacture is suspended in an alcohol, which may be an alcohol that has never been used, or that used to wash a precipitate of scleroglucan previously isolated, in the presence of 0.5 to 10% by weight of glyoxal relative to the weight of scleroglucan and the medium is stirred for 30 minutes to 8 hours before filtration to isolate the treated scleroglucan which will be dried in a conventional manner to 600C. The glyoxal is preferably introduced into the alcohol in concentrated aqueous solution at about 30 Gt.

Dans la dernière variante, préférée, la poudre de scléroglucane est imprégnée avec une solution hydroalcoolique de glyoxal, le volume de la solution représentant avantageusement 5 % à 15 % en poids du poids du polysaccharide à traiter, à raison de 0,5 à 10 % en poids de glyoxal par rapport au poids du polysaccharide et les solvants sont éliminés après 10 minutes à une heure de contact, par chauffage en milieu ventilé, à une température comprise entre 500C et 700C. In the last, preferred variant, the scleroglucan powder is impregnated with a hydroalcoholic solution of glyoxal, the volume of the solution advantageously representing 5% to 15% by weight of the weight of the polysaccharide to be treated, in a proportion of 0.5 to 10% by weight of glyoxal relative to the weight of the polysaccharide and the solvents are removed after 10 minutes to one hour of contact, by heating in a ventilated medium, at a temperature between 500C and 700C.

Ce traitement peut être effectué en milieu neutre ou de préférence en milieu légèrement acide jusque vers pH 4, le glyoxal n'étant pas stable en milieu basique. This treatment may be carried out in a neutral medium or preferably in a slightly acidic medium up to pH 4, the glyoxal not being stable in basic medium.

On peut aussi traiter par le glyoxal, les mélanges de scléroglucane et d'au moins une autre gomme, tel que guar, caroube, alginate ou pectine ; les compositions alors obtenues, en appliquant les deux dernières variantes du procédé sont aussi un objet de l'invention. Glyoxal can also be used to treat mixtures of scleroglucan and at least one other gum, such as guar, carob, alginate or pectin; the compositions thus obtained, by applying the last two variants of the process are also an object of the invention.

Dans ce qui suit, on décrit des exemples de mise en oeuvre de l'invention et on compare les vitesses de mise en solution de différents échantillons ; celles-ci ont été estimées par la méthode dite du vortex. In what follows, examples of implementation of the invention are described and the dissolution rates of different samples are compared; these have been estimated by the so-called vortex method.

Pour cela, on introduit dans un bécher de 250 ml, de diamètre 70 mm équipé d'un agitateur magnétique avec un barreau de 40 mm, tournant à 600 tours par minute, 100 g d'eau à une température donnée. For this, is introduced into a 250 ml beaker, diameter 70 mm equipped with a magnetic stirrer with a 40 mm bar, rotating at 600 rpm, 100 g of water at a given temperature.

L'agitateur ne tournant pas, on disperse 1 g de la poudre à étudier sur la surface de l'eau et on déclenche l'agitation ; on mesure alors le temps mis jusqu'à disparition complète du vortex. With the stirrer not rotating, 1 g of the powder to be studied is dispersed on the surface of the water and stirring is initiated; the time taken until the complete disappearance of the vortex is measured.

Pour tous les essais réalisés avec les produits de l'invention, la dispersibilité était excellente, aucune formation de grumeaux n'a été constatée au cours de la dissolution.For all the tests carried out with the products of the invention, the dispersibility was excellent, no formation of lumps was observed during the dissolution.

Les viscosités des solutions ont été mesurées avec un viscosimètre Erookfield LVT équipé d'aiguilles nO 2 ou 3 tournant à 30 tours/minute. The viscosities of the solutions were measured with an Erookfield LVT viscometer equipped with nO 2 or 3 needles rotating at 30 rpm.

Dans ce qui suit, on décrit des exemples de l'invention. In what follows, examples of the invention are described.

EXEMPLE 1
On met en suspension 50 g du précipité, lavé à l'alcool, défibré et essoré à 45 % d'extrait sec résultant de l'introduction d'éthanol dans le milieu en fin de fermentation, dans 200 ml d'éthanol issus du lavage d'un lot de polysaccharide précédemment précipité et dont le pH est 7. On introduit ensuite et sous légère agitation 0,15 à 0,3 ml d'une solution aqueuse de glyoxal à 30 g/ 100 ml et maintient le mélange à température ambiante pendant deux heures.
EXAMPLE 1
50 g of the precipitate are suspended, washed with alcohol, defibrated and filtered with 45% of dry extract resulting from the introduction of ethanol into the medium at the end of fermentation, into 200 ml of ethanol obtained from the washing. of a batch of polysaccharide previously precipitated and whose pH is 7. 0.15 to 0.3 ml of a 30 g / 100 ml aqueous glyoxal solution are then introduced under slight stirring and the mixture is kept at ambient temperature. during two hours.

On isole alors le solide par filtration. Après lavage à l'isopropanol et séchage à 600C pendant 6 heures, on obtient 22 g de scléroglucane traité selon l'invention. The solid is then isolated by filtration. After washing with isopropanol and drying at 600C for 6 hours, 22 g of scleroglucan treated according to the invention are obtained.

On a mesuré à différents instants après l'addition du scléroglucane les viscosités des solutions aqueuses obtenues ; les grains de poudre faisaient 100 um environ ; le. scléroglucane a été introduit à raison de 5 g/l d'eau, à 200C, sous bonne agitation. The viscosities of the resulting aqueous solutions were measured at different times after the addition of scleroglucan; the grains of powder made about 100 μm; the. scleroglucan was introduced at a rate of 5 g / l of water, at 200C, with good stirring.

Les résultats figurent dans le tableau I. The results are shown in Table I.

TABLEAU I

Figure img00050001
TABLE I
Figure img00050001

Concentration
<tb> en <SEP> glyoxal <SEP> 1 <SEP> min <SEP> 2 <SEP> min <SEP> 3 <SEP> min <SEP> 5 <SEP> min <SEP> 10 <SEP> min <SEP> 20 <SEP> min <SEP> Remarques
<tb> (g/100 <SEP> ml)
<tb> 0,6 <SEP> 0 <SEP> 10 <SEP> 30 <SEP> 60 <SEP> 240 <SEP> 460 <SEP> 680 <SEP> dispersion <SEP> excellente
<tb> 0,5 <SEP> 0 <SEP> 20 <SEP> 60 <SEP> 80 <SEP> 300 <SEP> 520 <SEP> 700 <SEP> dispersion <SEP> excellente
<tb> 0,4 <SEP> 5 <SEP> 30 <SEP> 80 <SEP> 120 <SEP> 320 <SEP> 580 <SEP> 710 <SEP> dispersion <SEP> excellente
<tb> 0,3 <SEP> 10 <SEP> 40 <SEP> 100 <SEP> 140 <SEP> 360 <SEP> 600 <SEP> 700
<tb> 0 <SEP> 5 <SEP> 20 <SEP> 80 <SEP> 100 <SEP> 250 <SEP> 480 <SEP> 600 <SEP> nombreux <SEP> grumeaux
<tb>
EXEMPLE 2
On introduit 5 kg de poudre d'un scléroglucane commercial, par exemple celui commercialisé par MERO ROUSSELOT
SATIA (France) sous la référence Actigum CS 6, dans un mélangeur à palettes, type Lodigue et on verse rapidement sur la poudre agitée une solution de glyoxal préparée avec 16 ml de solution aqueuse de glyoxal à 30 g/100 ml, 8 g de citrate de monosodique pour obtenir un pH proche dé la neutralité, 100 ml d'eau et 300 ml d'alcool isopropylique. Après 20 minutes de brassage, les solvants sont éliminés, par exemple, en maintenant le mélange en étuve ventilée à 600C, pendant 2 heures.
Concentration
<tb> in <SEP> glyoxal <SEP> 1 <SEP> min <SEP> 2 <SEP> min <SEP> 3 <SEP> min <SEP> 5 <SEP> min <SEP> 10 <SEP> min <SEP > 20 <SEP> min <SEP> Notes
<tb> (g / 100 <SEP> ml)
<tb> 0.6 <SEP> 0 <SEP> 10 <SEP> 30 <SEP> 60 <SEP> 240 <SEP> 460 <SEP> 680 <SEP> dispersion <SEP> excellent
<tb> 0.5 <SEP> 0 <SEP> 20 <SEP> 60 <SEP> 80 <SEP> 300 <SEP> 520 <SEP> 700 <SEP> dispersion <SEP> excellent
<tb> 0.4 <SEP> 5 <SEP> 30 <SEP> 80 <SEP> 120 <SEP> 320 <SEP> 580 <SE> 710 <SEP> dispersion <SEP> excellent
<tb> 0.3 <SEP> 10 <SEP> 40 <SEP> 100 <SEP> 140 <SEP> 360 <SEP> 600 <SEP> 700
<tb> 0 <SEP> 5 <SEP> 20 <SEP> 80 <SEP> 100 <SEP> 250 <SEP> 480 <SEP> 600 <SEP> many <SEP> lumps
<Tb>
EXAMPLE 2
5 kg of powder of a commercial scleroglucane, for example that marketed by MERO ROUSSELOT, are introduced.
SATIA (France) under the reference Actigum CS 6, in a Lodigue-type vane mixer, and a solution of glyoxal prepared with 16 ml of aqueous 30 g / 100 ml glyoxal solution, 8 g of glyoxal, is rapidly poured into the stirred powder. monosodium citrate to obtain a near neutral pH, 100 ml of water and 300 ml of isopropyl alcohol. After stirring for 20 minutes, the solvents are removed, for example, keeping the mixture in a ventilated oven at 600 ° C. for 2 hours.

On obtient ainsi 5 kg de scléroglucane dont les vitesses de dissolution, à différentes températures, dans l'eau distillée, à pH 6,8 et dans l'eau de ville, à pH 8 ont été mesurées et comparées à celle du produit de départ, pour lequel on a relevé la formation de nombreux grumeaux pendant la dissolution. This gives 5 kg of scleroglucan whose dissolution rates, at different temperatures, in distilled water, at pH 6.8 and in tap water, at pH 8 were measured and compared with that of the starting material. , for which the formation of numerous lumps during the dissolution has been noted.

Dans le tableau II, figurent les temps au bout desquels le vortex a disparu dans les essais de dissolution. In Table II are the times at which the vortex disappeared in the dissolution tests.

TABLEAU II

Figure img00060001
TABLE II
Figure img00060001

<tb> <SEP> TEMPERATURE <SEP> ! <SEP> Eau <SEP> distillée <SEP> ! <SEP> Eau <SEP> ville <SEP> !
<tb> Départ <SEP> Traité <SEP> Départ <SEP> Traité
<tb> 20 C <SEP> 5 <SEP> min <SEP> 20 <SEP> s <SEP> 12 <SEP> min <SEP> 30 <SEP> s <SEP> 4 <SEP> min <SEP> 15 <SEP> s <SEP> 8 <SEP> min <SEP> 30 <SEP> s
<tb> ! <SEP> 450C <SEP> !3 <SEP> min <SEP> 40 <SEP> s <SEP> ! <SEP> 8 <SEP> min <SEP> 20 <SEP> s <SEP> ! <SEP> 3 <SEP> min <SEP> 10 <SEP> s <SEP> ! <SEP> 5 <SEP> min <SEP> 30 <SEP> s!
<tb> ! <SEP> 70 C <SEP> !2 <SEP> min <SEP> 25 <SEP> s <SEP> ! <SEP> 5 <SEP> min <SEP> 10 <SEP> s <SEP> ! <SEP> 2 <SEP> min <SEP> 15 <SEP> s <SEP> ! <SEP> 3 <SEP> min <SEP> 45 <SEP> s!
<tb>
Dans le tableau III sont indiquées les viscosités mesurées à différents temps dans les conditions de l'exemple 1.
<tb><SEP> TEMPERATURE <SEP>! <SEP> Water <SEP> distilled <SEP>! <SEP> Water <SEP> city <SEP>!
<tb> Departure <SEP> Treaty <SEP> Departure <SEP> Treaty
<tb> 20 C <SEP> 5 <SEP> min <SEP> 20 <SEP> s <SEP> 12 <SEP> min <SEP> 30 <SEP> s <SEP> 4 <SEP> min <SEP> 15 <SEP> s <SEP> 8 <SEP> min <SEP> 30 <SEP> s
<tb>! <SEP> 450C <SEP>! 3 <SEP> min <SEP> 40 <SEP> s <SEP>! <SEP> 8 <SEP> min <SEP> 20 <SEP> s <SEP>! <SEP> 3 <SEP> min <SEP> 10 <SEP> s <SEP>! <SEP> 5 <SEP> min <SEP> 30 <SEP> s!
<tb>! <SEP> 70 C <SEP>! 2 <SEP> min <SEP> 25 <SEP> s <SEP>! <SEP> 5 <SEP> min <SEP> 10 <SEP> s <SEP>! <SEP> 2 <SEP> min <SEP> 15 <SEP> s <SEP>! <SEP> 3 <SEP> min <SEP> 45 <SEP> s!
<Tb>
In Table III are indicated the viscosities measured at different times under the conditions of Example 1.

TABLEAU III
Viscosité en mPa.s

Figure img00070001
TABLE III
Viscosity in mPa.s
Figure img00070001

<tb> Instant <SEP> de <SEP> la <SEP> mesure <SEP> Témoin <SEP> Traité <SEP> au <SEP> gly@@al
<tb> ! <SEP> 1 <SEP> min <SEP> ! <SEP> 50 <SEP> ! <SEP> 10
<tb> ! <SEP> 2 <SEP> min <SEP> ! <SEP> 660 <SEP> ! <SEP> 50
<tb> ! <SEP> 3 <SEP> min <SEP> ! <SEP> 1 <SEP> 240 <SEP> @ <SEP> 480
<tb> ! <SEP> 5 <SEP> min <SEP> ! <SEP> 1 <SEP> 400 <SEP> ! <SEP> 1 <SEP> 220
<tb> ! <SEP> 10 <SEP> min <SEP> ! <SEP> 1 <SEP> 560 <SEP> ! <SEP> 1 <SEP> 520
<tb> ! <SEP> 15 <SEP> min <SEP> ! <SEP> 1 <SEP> 680 <SEP> ! <SEP> 1 <SEP> 600
<tb> ! <SEP> 20 <SEP> min <SEP> ! <SEP> 1 <SEP> <SEP> 800 <SEP> ! <SEP> 1 <SEP> 760
<tb>
EXEMPLE 3
On introduit dans un mélangeur 2 kg de scléroplucane
Actigum CS 11 commercialisé par MERO ROUSSELOT SATIA (Franc , et verse sur la poudre sous agitation, une solution préparée ave- 16 g de citrate monosodique, 80 ml d'eau, 8 ml de solution aqueuse de glyoxal à 30 S et 160 ml d'alcool isopropylique.
<tb> Instant <SEP> of <SEP> the <SEP> metric <SEP><SEP> Treated <SEP><gly @@ al
<tb>! <SEP> 1 <SEP> min <SEP>! <SEP> 50 <SEP>! <SEP> 10
<tb>! <SEP> 2 <SEP> min <SEP>! <SEP> 660 <SEP>! <SEP> 50
<tb>! <SEP> 3 <SEP> min <SEP>! <SEP> 1 <SEP> 240 <SEP> @ <SEP> 480
<tb>! <SEP> 5 <SEP> min <SEP>! <SEP> 1 <SEP> 400 <SEP>! <SEP> 1 <SEP> 220
<tb>! <SEP> 10 <SEP> min <SEP>! <SEP> 1 <SEP> 560 <SEP>! <SEP> 1 <SEP> 520
<tb>! <SEP> 15 <SEP> min <SEP>! <SEP> 1 <SEP> 680 <SEP>! <SEP> 1 <SEP> 600
<tb>! <SEP> 20 <SEP> min <SEP>! <SEP> 1 <SEP><SEP> 800 <SEP>! <SEP> 1 <SEP> 760
<Tb>
EXAMPLE 3
2 kg of scleroplucan are introduced into a mixer
Actigum CS 11 sold by MERO ROUSSELOT SATIA (Frank), and poured onto the powder with stirring, a solution prepared with monosodium citrate, 80 ml of water, 8 ml of 30 S aqueous glyoxal solution and 160 ml of water. 'Isopropylic alcohol.

Après 10 minutes d'agitation, on sèche le mélange à 600C pendant 2 heures. After stirring for 10 minutes, the mixture is dried at 600 ° C. for 2 hours.

Une solution aqueuse de ce produit à 5 g/l, a un -H de 7,8 alors que le pH du scléroglucane de départ, dans les mêmes conditions est 8,6. An aqueous solution of this product at 5 g / l has a -H of 7.8 whereas the pH of the starting scleroglucan under the same conditions is 8.6.

On a mesuré les viscosités des solutions aqueuses du scléroglucane traité et du produit de départ dans les mêmes conditions que précédemment ; les résultats figurent des le tableau IV.  The viscosities of the aqueous solutions of the treated scleroglucan and of the starting material were measured under the same conditions as above; the results are shown in Table IV.

TABLEAU IV

Figure img00080001
TABLE IV
Figure img00080001

<tb> ! <SEP> Instant <SEP> de <SEP> la <SEP> mesure <SEP> ! <SEP> Témoin <SEP> ! <SEP> Traité
<tb> ! <SEP> 1 <SEP> min <SEP> ! <SEP> 7 <SEP> ! <SEP> 15
<tb> ! <SEP> 2 <SEP> min <SEP> ! <SEP> 20 <SEP> ! <SEP> 15
<tb> ! <SEP> 3 <SEP> min <SEP> ! <SEP> 53 <SEP> ! <SEP> 18
<tb> ! <SEP> 5 <SEP> min <SEP> ! <SEP> 125 <SEP> ! <SEP> 44
<tb> ! <SEP> 10 <SEP> min <SEP> 260 <SEP> ! <SEP> 320
<tb> ! <SEP> 15 <SEP> min <SEP> ! <SEP> 386 <SEP> ! <SEP> 520
<tb> ! <SEP> 20 <SEP> min <SEP> ! <SEP> 685 <SEP> !
<tb>
EXEMPLE 4
On introduit dans un mélangeur 2,5 kg d'Actigum CS 6 et 2,5 kg de farine de guar HV 3000T commercialisée par MERO
ROUSSELOT SATIA (France). On ajoute sur la poudre. une solution de glyoxal préparée avec 30 ml de solution aqueuse de glyoxal à 30 g dans 100 ml, 6 g d'acide citrique, 100 ml d'H20 et 300 ml d'alcool isopropylique.
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<tb>! <SEP> 10 <SEP> min <SEP> 260 <SEP>! <SEP> 320
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<tb>! <SEP> 20 <SEP> min <SEP>! <SEP> 685 <SEP>!
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EXAMPLE 4
2.5 kg of Actigum CS 6 and 2.5 kg of HV 3000T guar meal marketed by MERO are introduced into a mixer.
ROUSSELOT SATIA (France). We add on the powder. a solution of glyoxal prepared with 30 ml of aqueous glyoxal solution at 30 g in 100 ml, 6 g of citric acid, 100 ml of H 2 O and 300 ml of isopropyl alcohol.

Après 30 minutes d'agitation, le mélange de polysaccharide est séché à 700C pendant 2 heures. After stirring for 30 minutes, the polysaccharide mixture is dried at 700 ° C. for 2 hours.

Le mélange de polysaccharide ainsi traité donne une poudre ayant une excellente dispersibilité dans l'eau et ne formant pas de grumeaux.  The polysaccharide mixture thus treated gives a powder having excellent dispersibility in water and does not form lumps.

Claims (7)

REVENDICATIONS 1. Scléroglucane caractérisé en ce que le polysaccharide naturel est traité par 0,5 à 10 % en poids de glyoxal.1. Scleroglucan characterized in that the natural polysaccharide is treated with 0.5 to 10% by weight of glyoxal. 2. Scléroglucane selon la revendication 1, caractérisé en ce que le scléroglucane est traité en solution, en suspension, ou sensiblement à sec.2. Scleroglucan according to claim 1, characterized in that the scleroglucan is treated in solution, in suspension, or substantially dry. 3. Sciéroglucane selon l'une des revendications 1 ou 2, caractérisé en ce qu'il est traité en mélange. avec au moins une autre gomme.3. Scieroglucan according to one of claims 1 or 2, characterized in that it is treated in mixture. with at least one other eraser. 4. Procédé d'obtention du scléroglucane selon l'une des revendications 1 ou 2, caractérisé en ce que l'on introduit le glyoxal dans le moût en fin de fermentation à une température comprise entre 100C et 800C et que l'on précipite le polysaccharide après 1 à 16 heures.4. Process for obtaining scleroglucan according to one of claims 1 or 2, characterized in that the glyoxal is introduced into the must at the end of fermentation at a temperature between 100C and 800C and that is precipitated. polysaccharide after 1 to 16 hours. 5. Procédé d'obtention du scléroglucane selon l'une des revendications 1 ou 2, caractérisé en ce que le scléroglucane en suspension dans un alcool est traité par le glyoxal pendant 30 minutes à 8 heures.5. Process for obtaining scleroglucan according to one of claims 1 or 2, characterized in that the scleroglucan suspended in an alcohol is treated with glyoxal for 30 minutes to 8 hours. 6. Procédé d'obtention du scléroglucane selon l'une des revendications 1 ou 2, caractérisé en ce que la poudre de scléroglucane est imprégnée d'une solution hydroalcoolique de glyoxal et que les solvants sont éliminés par chauffage après 10 minutes à 1 heure de contact.6. Process for obtaining scleroglucan according to one of claims 1 or 2, characterized in that the scleroglucan powder is impregnated with a hydroalcoholic solution of glyoxal and that the solvents are removed by heating after 10 minutes to 1 hour of contact. 7. Procédé d'obtention du scléroglucane selon la revendication 3, caractérisé en ce qu'il est traité en mélange avec au moins une autre gomme selon un procédé tel que défini à la revendication 5 ou 6. 7. Process for obtaining scleroglucan according to claim 3, characterized in that it is treated in admixture with at least one other gum according to a process as defined in claim 5 or 6.
FR8809100A 1988-07-05 1988-07-05 GLYOXAL TREATED SCLEROGLUCANE AND PROCESS FOR OBTAINING SAME Expired - Lifetime FR2633940B3 (en)

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