FR2839073A1 - Production of an inulin solution comprises treating a chicory root extract with a coagulant and then a flocculant - Google Patents

Abstract

Production of an inulin solution comprises fragmenting chicory roots, extracting the fragments with water, liming the extract to adjust the pH to at least 9, adding a coagulant and then a flocculant, and decanting and filtering the mixture to obtain a solution with an inulin content of at least 85% (dry basis).

Description

HPV-16 containing antibodies according to claim 22.

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  PROCESS FOR INULIN EXTRACTION FROM CHICOREES

  The present invention relates to the manufacture of purified inulin powder from chicory roots (Cichorium intibus). Inulin, a fructose polymer of molecular weight, is the reserve polymer of the

  chicory; it constitutes all the sugars of chicoree.

  Current processes for making inulin based on inulin extraction from already known chicoree roots. In common, the roots of chicorees first wind epigees and levees. Wiles wind then cut into chips of 14-15 m / 100g thanks to a cutacines. These chips undergo countercurrent diffusion with hot water (extraction temperature: 65-70 ° C). The diffusion scattered juices are recovered and the chips are exhausted. Press juices are collected and collected with the diffusion juices. At this stage, the inulin juices contain a

  a high rate of impurities and therefore have to undergo treatment by calco-

  carbonic. In some processes, the blast and carbonates juice simultaneously, in other, they chaule directly at pH 13 then carbonates to pH 11. In a third case, they pre-chaulse at pH 11 then undergo a massive liming and a synchronous carbonation. In all

  the cases, they then wind decantes and filters.

  In the state of the art, large chunks are used with a reduced exchange surface. The diffusion of inulin therefore requires a relatively long contact time at high temperature in order to achieve a proper extraction. These working conditions lead to undesirable phenomena such as: - Oxidation of juices; Large diffusion of impurities (proteins, salts) together with inulin;

  - Bacterial development and generation of organic acids.

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  Regarding purification, the simultaneous "liming-carbonation"

  decantation juice difficult to filter, inducing loss of inulin.

  Massive liming, meanwhile, has a major drawback: a pH

  greater than 11 resulted in degradation of inulin to fructose and glucose.

  Finally, all the processes mentioned above imply an important use: lime, at the origin of high costs; - carbon dioxide, which causes CO2 emissions into the atmosphere,

  with a not insignificant impact on the environment.

  The object of the present invention is a process for obtaining a purified inulin juice requiring only a reduced amount of lime and no CO2, while reducing the loss of inulin and retaining its native structure, and this, mainly thanks to the implementation of agents of separation

  during the purification step.

  In this process, roots of chicorees wind fragmented. The fragments are brought into contact with water (possibly containing inulin), under conditions allowing the diffusion of most of the inulin into the liquid fraction. This liquid fraction is separated from the fragments in order to obtain a separate liquid fraction. The latter is then limed to a pH of at least 9. The impurities are then separated by the addition of caustic agents.

  separation, then decantation and finally, filtration of overflow juice obtained.

  This process is characterized by the fact that the separation is carried out by the first addition of a coagulation agent, after a coagulation period, of a flocculation agent. The respective amounts of the agents placed in the work wind such that the filter overflow juices have an inulin content, measured in the present patent by the analysis of sugars

  total of at least 85% on dry matter.

  For this, the contact chicoree with water is made on chicoree fragments having an exchange surface greater than that of the chips. In addition, the extraction is carried out by pressing and not by simple diffusion, which allows to reduce the extraction temperature and the contact time, while maintaining an interesting extraction yield of quinine. The extraction juice obtained is of better quality. Finally, to the extent that the treatment consists of carrying out a moderate pH liming followed

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  of a separation of the impurities with the aid of agents coagulants and flocculants instead of the stage of classic calc-carbonation, the quantities of lime wind

  reduced and we do not use carbon dioxide.

  More specifically, the process consists of: a) spraying and washing fresh chicory roots (Cichorium intibus); b) To break them into small fragments: - Either by means of a rape, which may be for example Bucher brand, type C6, operating with a rotor with 3 hammers rotating at 730trs / min, and having 26 rows of knives on the edge of the rapier chamber; - Either by means of a root cutter followed by a grass grinder, the root cutter may be, for example, PUTSH brand, grass grinder may be, for example, the brand

  Maguin, type SB 120A RG, rotating at 1000 rpm.

  The aim is to obtain fragments of which at least 50% have a particle size less than 1.6 mm, and advantageously whose particle size is as follows: Granulometry%

> 3.15 10-20%

> 2.24 9-12%

> 1.6 10-16%

> 1.25 6-10%

> 0.8 7-10%

> 0.5 5-7%

  Background 31-38% The particle size is determined by passing the wet mill material through sieves having different mesh sizes, with watering. The method is as follows: - Each sieve is weighed dry (M1) and then placed on the sifter; - 1Og of grind deposited on the first sieve (M2);

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  - The sieve is started; - 51 of water poured on the first sieve; - The sieving is conducted for 10 minutes; - The excess water is blimine and each sieve is weighed tM3); The proportion of each granulometric fraction is calculated as follows: 1% of wet product on the sieve = (M3-M1) / M2x1 ool and whose composition is as follows: Composg% on MS Dry matter 23 - 25% Insoluble dry matter 16 - 18% Total nitrogen 0, 7 - 0,9% Ash 4,4 - 5,5% Free sugar 4 - 8% Total sugar 68 - 73% - The sugar content (glucose, fructose) is determined by HPLC a C ion-exchange column in calcium form (Biorad brand, Aminex HPX 87C ref., size 300 x 7.8 mm) equipped with a pre-column (Biorad brand, aminex HPX 87C reference, size 30 x 4.6 mm); a flow rate of 0.6 ml / minute detection by refractometry - the free sugars are dosed after diffusion, the total sugars after

enzymatic hydrolysis.

  - Protocol for the preparation of the sample for the determination: * Free sugars: - Dissolve, for 30 minutes at 80 ° C., 1 g of chicorde dry matter in 150 g of water, - Dilute for analysis to reduce to 1 g of MS / liter

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  Filter on C18 and 0.22 m before HPLC analysis.

  * Total sugars - Spread 30 minutes at 80 ° C, 1 g of chicoree dry matter in 150 g of water, - Adjust the pH to 4.5 - Add 1 ml of N230 NOVO NORDISK enzyme - Stir in 60 C waterbath 30 minutes - Cool - Dilute for analysis to reduce to 1 g MS / liter

  - Filter on C18 and 0.22 m before HPLC analysis.

  During the enzymatic hydrolysis of inulin, the breakdown of the osidic bond causes an increase in the dry matter. The total sugar content is thus calculated according to a formula taking into account this variation of the dry matter: Total sugar = total sugars measured by HPLC x 0.951 The determination of the total nitrogen content is carried out according to the Kjeldahl method. The principle of this method consists of transforming organic nitrogen into ammonium sulphate by the action of concentrated, hot sulfuric acid in

presence of a catalyst.

  The ammonia is then liberated from its salt with sodium hydroxide and is then distilled off, and finally collected in a solution of boric acid at pH 4.65. The titration is carried out with dilute sulfuric acid until it returns to

initial pH.

  1) Weigh approximately exactly mg of product to be analyzed (eg m = 2 g dry material of the analyte) 2) Stir the sample into a 250 ml flask 3) Introduce two pellets of Kjeltabs W mineralization catalyst 4) Add 25 mL of sulfuric acid concentrated in a hood 5) Gradual mineralization at medium thermostat until white smoke appears (Gerhardt miner, Kjeldatherm)

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  6) Then rise to a temperature of 400 C, stay 2 hours (disappearing greenish color) 7) Check serie must include: - 1 NH4CI standard dry 1 h30 to 1 1 0 C (100 mg) s (theoretical value in nitrogen : 26.17%) -1 white, NT, reagents and material 8) Introduce sodium hydroxide solution into the mineralization tube until a black or blue coloration is obtained. 9) Distill for 5 minutes (Distillator - Titrator Gerhardt, Vapodest 6) and collect the distillate in 50 mL of boric acid at 20 g / L) Titration of the distillate by pH-metry with 0.1N sulfuric acid solution 11) Final pH of 4.65 titration (corresponds to the return at the initial pH of boric acid) The total nitrogen content of the product is obtained using the following formula: | ((V1 -V2) x14x0.1 x100) / m With: V1 Volume H2SO4 titrant of the sample V2 Volume H2SO4 titrant of white m Mass in mg of the test sample The determination of the ash content is carried out by incineration of the

  product to be analyzed in oxidizing atmosphere at 550 C.

  1) Place porcelain crucibles for one hour in an oven

  (for example Carbolite CSF 1200) preheated to 700 C.

  2) Weigh (PO) the crucibles after cooling in the desiccator.

  3) Cool the oven at room temperature.

  4) Introduce exactly 3 to 4 g of product (P1) into the crucibles. ) Preheat the crucibles with a hotplate until the test portions are completely charred.

  6) Place the crucibles in the oven.

  7) Rise in temperature very gradually until reaching

550 C.

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  8) Leave at 550 ° C for 12 hours or until you get ashes

homogenous (white).

  9) Weigh (P2) the crucibles after cooling in the desiccator.

  The ash percentage of the product is obtained by the formula: I ((P2 PO) / P1) x 100 | And whose polymerization degree inulin (DP) has the following distribution:

  DP DP2 DP3 DP4 DP5 DP6 DP7 DP8 DP9 DP10 DP11 DP12 DP13 DP14 DP15 DP16 DP17

  % 17 20.5 9.5 7.5 7.5 7.5 7 6 4.5 4 3.5 3 3.5 2 2 1

  The degree of polymerization expresses the number of osidic residues (fructose and glucose in the case of inulin) which is

constitutes a polymer.

  The determination of the degree of polymerization of the inulin is carried out by HPLC according to the protocol described in the

  reference: << Journal of Chromatography >>, 1984, 303, 417-421.

  Column: Nucleosil grafted silica NH2, Supplier: Macherey-Nagel, Size 250 x 4.6 mm Column Temperature: 35 C Eluent: Acetonitrile / Water / Polyethylene Glycol 10000 / 1,4 Diaminobutane:

/50/0.2/0.02

  Flow rate: 1 ml / min (maximum pressure <200 bar) Detector: Refractometry Calibration: Injection of DP1 to DP7 in glucose Assay: Prepare solutions at 25 g / l in water c) Put these fragments in contact with water water, possibly containing inulin,

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  - In a tank of 1 m3 stirred at about X rpm; At a temperature of between 55 ° C. and 70 ° C. and preferably between 60 ° C. and 65 ° C .; - In the presence of an antioxidant, such as sodium bisulfite, 0.2 to 0.6% of sodium bisulfite on dry matter, and preferably 0.3% of sodium bisulfite on the material dried; - For a period of between 15 to 30 minutes and preferably between 20 and 25 minutes - such that the water represents between 80 and 90%, and preferably 85% by weight of the diluted ground material; in order to obtain a liquid fraction containing inulin and

some impurities.

  The advantage of working at this temperature is to limit the phenomena of oxidation and the solution of impurities; that of working quickly is to limit the bacterial and

The appearance of organic acids.

  d) To separate the solid fraction from the liquid fraction in order to recover this back and to purify it. The separation can be carried out by different technologies: - By pressing on a press-filter of the brand Choquenet, equipped with trays of 800x800 mm, and having a filtering surface of 1m2 per tray; the pressing can be carried out in one stage or, preferably in two stages with a recycling of the filter-press sludge; - And, preferably, by pressing on a twin-screw type P35 brand Stord, equipped with screws Babbini brand, and whose grid has the following porosite characteristics: Length of the pore size of the gate grate Up to 46 cm 2 mm De46a62cm 1,5mm From 62 to 157 cm 1 mm

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  The pressing can take place in a floor; we then obtain a

  solid fraction 1 and a liquid fraction 1.

  Advantageously, a second pressing stage is carried out: for this, the solid fraction 1 (from the first stage) is brought into contact with water, so that the water represents, by mass, 90% of the solid waterfraction mixture, for 15 to 30 minutes and preferably between 20 and 25 minutes. The mixture is then pressed; the liquid fraction 2 obtained is then used for contacting the initial fragments, in total substitution of the water, so that the water represents by weight in the ground matter

  diluted between 80 and 90%, and preferably 85%.

  The separated liquid fraction 1 thus obtained has the following characteristics: A q Dry matter 11-14% Total nitrogen 0.5-1% Total sugar 8184% e) To be subjected to this liquid fraction 1 separated from the liming: Either a massive liming by adding at once a quantity of lime (at 180 g / l of CaO) to reach a pH of at least 9, preferably 9, which generally represents a quantity of CaO less than 2 g / l of CaO / liter separated liquid fraction; - Or, and preferentially, a progressive liming, by adding to it a first amount of lime (at 180g / l of CaO) to reach a pH of between 7 and 8, preferably 7.5, then a second quantity of fact of lime to reach a pH of between 8 and 9, preferably 8.5 and finally, by adding a final amount of lime to reach a pH of at least 9, preferably 9, which generally represents a amount of CaO less than 2 g / l of CaO per liter of separated liquid fraction;

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  Stir this solution for a period of 10 to 20 minutes. preferably 15 min at a temperature between 75 and 85

 C preferably 80 C.

  A chalyzed liquid fraction with the following characteristics is then obtained: Dry matter 12-14% Total sugar (% on MS) 85-89% haze 30-40 The haze is detected at 420 nm on an unfiltered solution. The method is as follows: a. The solution to be analyzed is diluted with distilled water so as to obtain an optical density of between 0.2 and 0.8; b. The absorbance is then read at 420 nm on the filtered solution and

unfiltered.

  The absorbance is calculated as follows: bs = DO non-filter DO filter | The disorder is calculated as well, taking into account the conversion tables: - Inulin conversion: brix corrects = (1,2xBrix read - 0,8) - Fructose conversion: brix corrects = (1,017xBrix read-0,0719) ruble (Ul ) = (100 000xabs) i (length of the tank x brig | corrigej | f) To separate the impurities from the liquid fraction chaulee gr3ce

  the use of separating agents facilitating decantation and filtration.

  This method avoids the use of carbon dioxide.

  (g) For this purpose, a polyamine-type organic coagulation agent having a molecular weight (5.104 Daltons) and a mean viscosity (200-450 cps at C) is added to this lime liquid fraction, for example Agent Sucazur 4583, from the company Degremont Erpac, in the following manner: - The coagulation agent is first diluted in water so that the agent represents 1% of the volume of the solution of coagulating agent; The coagulating agent solution is added to the lime liquid fraction, so that the clotting agent is between 1 and 20 ppm, and preferably 5 ppm on the lime liquid fraction; The lime liquid fraction thus coagulated is mixed for at least 5 minutes; h) To this coagulated liquid fraction is added a high molecular weight (107 Daltons) acrylamide copolymer flocculating agent having a high viscosity in solution at 5g / cm (800cps), preferably The flocculating agent Prosedim AS 23 Suc of the Degremont Erpac brand, in the following manner: The flocculation agent is first diluted in water so that the flocculation agent represents % of the volume of the flocculating agent solution; The flocculating agent solution is added to the coagulated liquid fraction, so that the flocculating agent is between 1 and 20 ppm, and preferably 5 ppm on the coagulated liquid fraction; the coagulated-flocculated liquid fraction thus obtained is then stirred for at least 5 minutes; i) To decant this coagulated-flocculated liquid fraction for at least 1 hour, at a temperature of between 75 and 85 [deg.] C. and preferably 80 [deg.] C., so as to obtain sludge and overflow juice having the following characteristics: dry 11-13% Total sugars (% on MS) 84-86% Trouble 30-36 k) To recover the sugar juice;

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  I) To pass the settling sludge on thickening filter so as to recover the juices; m) To mix the overflow juice and juice sludge, then to make them undergo a filtration on a 10 m porosite cellulosic plate filter, for example plates of the mark Seitz, type T1000, possibly and advantageously followed by a second filtration on 0.22 μm porosite plates to ensure sterility; in order to obtain a filter overflow juice having the following characteristics: Dry matter 1 1-13% Total sugars (% on MS) 84-87% Trouble 0-6 n) To acidify this overflow juice filter: - Either by electrodialysis; Or, preferably, on a strongly acidic cation exchange resin of polystyrene type, and preferably Amberlite 200C Na; And, to obtain the powdered inulin: o) To concentrate this acidified overflow juice to 25-35% of dry matter and preferably 30%, on a falling flake evaporator; p) To atomize this acidified juice to obtain an inulin powder having the following characteristics: Dry matter 95-99% Total nitrogen (% on MS) 25% Ash (% on MS) 1-4% Free fructose / sugar total 8-9% Total sugars (% on MS) 89-91% Calcium (% on MS) 0-0.05% Organic acids (% on MS) 1-3% And whose degree of polymerization inulin present the following distribution:

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  % of each oligomer DP2 DP3 DP4 DP5 DP6 DP7 DP8 DP9 in the fragments

17 2O, 5 9.5 7.5 7.5 7.5 7 6

I)

  DP10 DP11 DP12 DP13 DP14 DP15 DP16 DP17

4.5 4 3.5 3 3.5 2 2 1

4 3 3 2 2 2 1 0

  Non-degraded inulin is thus obtained, since the distribution of the degree of polymerization of its oligomers is very close to that of the oligomers of inulin found in the crushed fragments.

Example 1

  The following example illustrates the process of extracting inulin using root-cutting / grass-cutting and press-pressing. 1219 kg of fresh chicoree raised so as to obtain 1000 kg of epigeous chicory at 24% of dry matter and 69.8% of total sugars. Wiles wind then fragmented by passing through a root cutter PUTSH followed by a grass grinder MAGUIN equipped with a grid having orifices of x25 mm. The grinding material obLenu has the following characteristics: Granulometry%

> 3.15 18.3

> 2.24 10.3

> 1.6 10.0

> 1.25 8.5

> 0.8 8.2

> 0.5 6.7

Background 38.0

  The ground material is then diluted with the liquid fraction 2 resulting from the downstream of the process.

  5 kg of a solution of 15% sodium bisulfite and 655 kg of

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  liquid fraction 2 from the downstream of the process. The mixture is heated to 60 C by direct steam injection which represents a water intake of 120 kg. 1780 Kg of diluted material is then heated to 15% of dry matter. It is then press on a twin-screw press of the brand STORD equipped with two screws of the brand BABBINI. 249 kg of a solid fraction 1 a, 1% of dry matter and 1531 kg of a liquid fraction 1 are obtained at 12.6% of

  dry matter. The solid fraction 1 is diluted again with 570 kg of water.

  This mixture is again press in the same way as before.

  163.4 kg of a solid fraction 2 and 655 kg of a liquid fraction 2 were obtained at 4.1% of dry matter. This back is retrieved and used in

  upstream of the process for diluting the initial ground material.

  The liquid fraction 1 has the following characteristics: Dry matter 12.6% Total nitrogen (% on MS) 0.7% Total sugars (% on MS) 83.5% Disturbance 60 The liquid fraction 1 is then limed with fa For this purpose, 8 kg of lime with 18% of dry matter added to it in this foamed liquid fraction then added 0.77 kg of a solution of SUCAZUR 4583 coagulant at 1% dry matter. The coagulated solution is then stirred at X rpm for 5 minutes. To this coagulated liquid fraction is then added 7.7 kg of flocculant solution AS 23 at 0.1% dry matter. The coagulated liquid fraction is then stirred at X rpm for 5 minutes. The coagulated-flocculated liquid fraction is then sent to a static decant of residence time 1 h. After this time, 1377 kg of overflow juice is recovered at 12.2% dry matter and 170 kg of sludge at 16% dry matter. This thick sludge thickened on thickening filter in order to recover just 34 kg thick sludge and 136 kg of juice to 12.2% dry matter. This juice is added to the overflow juice: the mixture is then filtered on cellulosic plates of 10pm of the brand SEITZ. 1506 kg of filter overflow juice with 12.1% of dry matter are then obtained. It has the following characteristics: Dry matter 12.1%

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  Total sugars (% on MS) 86.5% Disorder 2 This is then acidified by passing on a strong cationic resin Amberlite 200C Na, at 8BV / h. The juice is then pre-concentrated until

  a dry matter of 30% then atomizes.

  In this case 176 kg of inulin powder is obtained, having the following composition: Compose% on MS. Dry matter 97% Total nitrogen 0.6% Ashes 2.5% Fructose free / Total sugars 8.1% Total sugars 90.6% Calcium 0.03% Organic acids 2.1% And whose degree of polymerization Inulin show the following distribution

  DP DP2 DP3 DP4 DP5 DP6 DP7 DP8 DP9 DP10

% 20 10 7 7 7 6 6 5 4

DP11 DP12 DP13 DP14 DP15 DP16 DP17

3 3 2 2 2 1 0

  The graph below shows that the inulin has kept its native structure since the degree of polymerization follow the same distribution in the

  final powder only in the initial grindstone.

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2s, 0% lli -

  2.7 o, o% in Broyat o, oYO i: i 2 in: e

OO. = ;! -

  o o% i s 1 <<3 Q << <t gN <<> Q Q Og <> Q <t <;, Q <O Q Q O O Deores of polymerization of inulin in ground matter and in atomized powder

Example 2

  This example follows the same method as that previously presented, except that the fragmentation of the roots of chicoree is carried out by means of a brand Bucher brand scrap, type C6, operating with a rotor with 3 hammers rotating at 730 trs / min, and presenting 26 rows of knives on the edge of the rapier chamber. Thus, the fragments obtained have the following granulometric profile: Granulometry%

> 3.15 14.1

> 2.24 10.4

> 1.6 15.6

> 1.25 9.3

> 0.8 8.1

> 0.5 5.4

Bottom 37

  The mash then follows the same steps as in Example 1.

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Example 3

  The following example is the same method as that presented in Example 1, except that separation of the liquid and solid fractions takes place by means of a filter press. Thus, 500 Kg of fresh chicorees has 24% dry matter ground using a root cutter and a grass grinder. The fragments obtained were brought into contact with 210 kg of water and 55 kg of liquid fraction from downstream of the process plus 3 kg of a solution of 15% sodium bisulfite. The mixture is heated to 60 C with direct steam corresponding to 70 kg of water. The

  837Kg of ground material diluted to 14.6% dry matter then presses on filter-

CHOQUENET brand press.

  For this, the ground material undergoes a first phase of filtration: it is sent under pressure against the filter cloth. He then undergoes a compaction step

  or air is injected between the trays. After this filtration step-

  compaction, 782Kg of separated liquid fraction at 12.4% of

dry matter.

  The ground material undergoes a third step of rinse, cage: 75 kg of water wind sent under pressure through the cakes. At this stage, 75.7 kg of solid fraction and 55 kg of separated liquid fraction are recovered. This liquid fraction is

  recovered and used for the initial dilution of the crushed material.

  The separated liquid fraction 1 has the following characteristics: Dry matter 12.0% Total nitrogen (% on MS) 0.7% Total sugar 82%

  The separated liquid fraction is then limed and then separated according to Example 1.

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Claims (9)

  A process for preparing an inulin solution from chicory, wherein the chicory roots are comminuted into fragments, the fragments are contacted with water possibly containing inulin, under conditions in which the most of the inulin contained in the fragments passes into the liquid fraction, the liquid fraction is separated from the fragments to obtain a separate liquid fraction, the separated liquid fraction is limed until a lime liquid fraction of one is obtained. Final pH at least equal to 9, the impurities are separated from the liquid fraction by addition of separating agents and by decantation and filtration, to obtain as filter overflow juice, the inulin solution, and characterized in that it performs separating the impurities from the liquid fraction by adding, firstly a clotting agent, after a coagulation time, a flocculating agent, the quantities of the two agents being such that the filter overflow juice has an inulin content, measured in the present patent by the analysis of total sugars, of at least 85% on dry matter.   2. Process according to claim 1, characterized in that the coagulation agent is a cationic polyamine of molecular weight, added at a dose of between 1 and 20 ppm in the juice and preferably of 5 ppm.   3. Method according to any one of the claims   preceded by the fact that the flocculation agent is a high molecular weight acrylamide copolymer, added at a dose of between 1 and   ppm (in ppm on the volume of limed solution).   4. Method according to any one of the claims   precedents, characterized in that the chaulee liquid fraction is agitated   for at least 5 minutes after addition of coagulant.   5. Method according to any one of the claims   precedents, characterized in that the coagulated liquid fraction is agitated   for at least 5 minutes after addition of flocculating agent.   6. Method according to any one of the claims   precedents, characterized in that the filter overflow juice has a purity in sugar of at least 85% (expressed as sugar on dry matter).   7. Method according to any one of the claims   precedents, characterized in that the final pH of the chaulee liquid fraction   is at least 9, and preferably 9.   8. Process according to any one of the claims   precedents, characterized in that at least 50% of the fragments present   a particle size less than 1.6 mm.   9. Method according to any one of the claims   preceded by the fact that the filter overflow juice is acidified by passing it over an ion exchange resin, then concentrated to 30 Bx and finally atomized in a obtain an inulin powder containing at least 89% of inulin expressed as total sugars on