WO2016166264A1 - Method for producing an additive for animal feed and corresponding additive - Google Patents

Method for producing an additive for animal feed and corresponding additive Download PDF

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Publication number
WO2016166264A1
WO2016166264A1 PCT/EP2016/058307 EP2016058307W WO2016166264A1 WO 2016166264 A1 WO2016166264 A1 WO 2016166264A1 EP 2016058307 W EP2016058307 W EP 2016058307W WO 2016166264 A1 WO2016166264 A1 WO 2016166264A1
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WIPO (PCT)
Prior art keywords
particles
substance
powder
additive
liquid
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PCT/EP2016/058307
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French (fr)
Inventor
Bastien VIEL
Catherine IONESCU
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Pancosma Sa
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Publication of WO2016166264A1 publication Critical patent/WO2016166264A1/en

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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K40/00—Shaping or working-up of animal feeding-stuffs
    • A23K40/10—Shaping or working-up of animal feeding-stuffs by agglomeration; by granulation, e.g. making powders
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K20/00—Accessory food factors for animal feeding-stuffs
    • A23K20/10—Organic substances
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K20/00—Accessory food factors for animal feeding-stuffs
    • A23K20/10—Organic substances
    • A23K20/111—Aromatic compounds

Definitions

  • the present invention relates to a method of manufacturing an additive for animal feed and a corresponding additive.
  • Plant extracts can be an alternative to some antibiotics that are commonly used as a preventative in animal nutrition but could potentially have undesirable side effects on consumer health such as developing bacterial resistance in humans.
  • oleoresin of capsicum contains in particular two active substances: capsaicin and dihydrocapsaicin. It is generally in the form of a viscous liquid.
  • the use of oleoresin capsicum is known to modify dietary behavior, including food intake, to improve the digestibility of certain nutrients such as carbohydrates and fats and to modulate the immune response in animals. ruminants and / or monogastrics.
  • capsaicin and dihydrocapsaicin are extremely irritating substances when they come into contact with the nasal mucosa. They are not volatile, however. Therefore, used in liquid form, they do not present a risk of irritation of the nasal mucosa, even at a small distance, insofar as it avoids any direct contact with the mucosa. In order to limit the risk of irritation, especially for users who must handle these substances in order to incorporate them into the animal feed, capsaicin and dihydrocapsaicin are therefore usually used in liquid form.
  • the use of a food additive in liquid form is restrictive and poorly adapted. In the case where the additive must be mixed with a powder before being supplied to the animal, the final mixture obtained may have certain disadvantages: non-homogeneous distribution of the active substances, formation of aggregates, irritancy.
  • a known solution is to mix the oleoresin capsicum with fat, for example a vegetable oil, and form particles in the form of beads.
  • fat for example a vegetable oil
  • FR 2,908,600 discloses a method of manufacturing a powdered animal feed additive by cold atomization of a liquid mixture containing an encapsulating fat and an active agent such as capsaicinoids.
  • an active agent such as capsaicinoids.
  • the use of a fatty support for encapsulation of the active agent makes it possible to limit the irritating effect of the final product in the form of a powder.
  • the particles may be coated or encapsulated by an outer coating layer.
  • Such a solution is expensive and complex to implement.
  • the use of a fatty medium is problematic because of the significant risk of degradation by melting the product obtained according to the ambient temperature. The preservation of such a product is therefore delicate.
  • the invention improves the situation.
  • the invention relates to a method for manufacturing an additive intended for animal feed in the form of a powder of particles containing at least a first substance classified in one of the three categories respectively identified by the Xi codes. , Xn and C, characterized in that it comprises an operation for producing said powder by hot atomization of a solution containing said first substance, the powder produced containing at least 90% of particles of size greater than or equal to 200 m .
  • the invention originates from a problem related to the presence of capsicum oleoresin, which contains irritating active substances, in an animal feed additive.
  • the Applicant intends not to limit the scope of its application to this particular example but to extend it to any food additive containing a substance having an at least irritating effect, especially an irritating and / or harmful and / or corrosive effect.
  • substances having an irritant, harmful or corrosive effect are respectively identified by the symbols Xi or Xn or C according to Directive 1999/45 / EC.
  • an additive in the form of a powder consisting of particles of controlled size and greater than or equal to 200 m makes it possible to very clearly reduce the irritant (or harmful or corrosive) effect of the final product (the additive) containing the irritating substance Xi (or Xn or C).
  • fine particles are likely to form by fraction and / or abrasion of the particles of the finished product.
  • a hot-spray particle formation technique is used which makes it possible to agglomerate particles.
  • composite or agglomerated particles are formed from particles of smaller size.
  • the powder is produced by atomization in a fluidized air bed.
  • the solution containing the first substance is advantageously free of fat.
  • the solution is aqueous.
  • the particles produced are uncoated.
  • the method comprises a step of adjusting at least one operating parameter intended to control the size of the solid particles of the final product obtained, the desired size of the particles being greater than or equal to 200 ⁇ m.
  • the solution may contain at least one aromatic substance having an odor and / or taste substance having a flavor.
  • the solution may contain a sweetener.
  • the solution may also contain an emulsifier.
  • the solution contains:
  • Said first substance may be oleoresin capsicum.
  • the additive contains between 0.1% and 99% by weight of said first substance.
  • the invention also relates to a feed additive intended for animal feed in the form of a powder of particles containing a first substance classified in one of the three categories respectively identified by the codes Xi, Xn and C, characterized in that the said powder comprises at least 90% of particles of size greater than or equal to 200 ⁇ , without fat, having a raspberry-like structure or an onion-layer structure or an intermediate structure between a raspberry-like structure and a layered structure onion.
  • the additive is advantageously obtained according to the previously defined manufacturing method.
  • FIG. 1 shows a flowchart of the manufacturing method according to one embodiment
  • FIG. 2 represents a flowchart of the manufacturing method according to another embodiment
  • FIG. 3 represents a support powder in powder form used by the process of FIG. 1, before mixing
  • FIGS. 7A and 7B show agglomerated particles at different stages of their formation, one having an onion layer structure, the other having a raspberry-like structure.
  • the manufacturing method of the invention aims to produce an animal feed additive in the form of a powder of particles containing a substance, called "first substance", having an at least irritating effect.
  • the additive can be added to the food supplied to animals, especially in breeding.
  • the first substance is here an active substance, that is to say a substance having a physiological effect on the animal.
  • at least irritating effect we mean here designating either an irritating effect
  • the first substance can be classified in one of the three categories of substances referred to as dangerous and respectively identified by the codes or symbols Xi, Xn and C. These codes or symbols refer to the signaling system for hazardous substances as defined by the European Directive 1999/45 / EC. The table below shows the effect and risk definition of each of these three categories of substances:
  • Xn Harmful Substances and preparations which through inhalation, ingestion or skin penetration may cause death or health damage either acutely or chronically.
  • the method for manufacturing an animal food additive of the invention comprises an operation for producing a particle powder, which comprises the formation of composite or agglomerated particles, obtained by agglomeration of particles of smaller size (that is, -size smaller than the composite particles).
  • a "composite" particle is an agglomerate of several particles, in other words a particle formed by the agglomeration of other particles.
  • the powder produced by the process of the invention contains at least 90% of particles of size greater than or equal to 200 ⁇ .
  • the operation for producing the powder is carried out by atomization (that is to say, spraying) while hot of a solution containing the first substance, for example by atomization in a fluidized air bed.
  • the operation for producing the powder comprises the steps E1 1 to E14 described below with reference to FIG.
  • the hot atomized solution is free of fat.
  • the solution is aqueous.
  • step E1 a solution to be sprayed (or atomized), denoted "SP m ", containing the active substance, in this case oleoresin capsicum.
  • the active substance which can be initially in liquid or solid form (for example in powder form) is solubilized in a solvent.
  • aqueous solution is prepared. The solvent used is therefore water.
  • step E1 1 (as well as during step E2) of preparation of the solution, it is also possible to add all or part of the following components to the mixture of active substance and solvent:
  • taste substance being a substance providing a salty, sweet, sour, bitter or umami flavor, in particular one or more sweetener (s);
  • a spraying medium for example sodium chloride or maltodextrin, which is preferably soluble or dispersible (for example wheat flour).
  • the emulsifier may be gum arabic. Gum arabic also makes it possible to solubilize aromatic compounds that are insoluble in water and also serves as a support.
  • the solution to be atomized contains:
  • a charging agent may be added additionally in this solution.
  • sputtering solution SP m are given in the following tables ("m" corresponding to the index of the example under consideration). he here aqueous solutions, only the components of the solution other than water being indicated.
  • step E1 the various components indicated in the tables relating to Examples 1 .1 to 1 .4 are mixed and solubilized in water.
  • the ratio between water and components to be solubilized is between 0.5 and 5, preferably between 0.6 and 1.
  • the amount of water must be sufficient to allow the solubility of the various ingredients in the water.
  • Step E1 1 is followed by a step E12 of spraying or atomizing the SP m solution in a fluidized air bed. During this atomization step E12, the solution SP m is sprayed into fine droplets in a fluidized air bed.
  • the process continues with a step E13 of particle formation within the fluidized air bed of the production facility.
  • the minimum size of the particles allowed to be evacuated from the fluidized air bed is regulated by an operating parameter of the installation, the particles smaller than this minimum size being kept in suspension in the fluidized air bed. In the embodiment described here, the minimum size is 200 m.
  • the particles smaller than the minimum size set, especially the fine particles are not allowed to leave and are held in suspension in the fluidized air bed.
  • An operator adjusts certain parameters, such as the spray rate, the air bed temperature, the air flow, and ..., on the production plant during an initial adjustment step E10. This makes it possible to control the size of the solid particles of the final product obtained (that is to say the finished product leaving the production facility).
  • the E12 spray is triggered before the particle formation step E13 and continues concomitantly with this step E13, until total consumption of the spray solution.
  • the spraying is carried out continuously (but could be carried out discontinuously over a given period).
  • the first spray droplets are dried and form fine particles.
  • part of the newly formed droplets are fixed on the particles already formed, especially on the particles "primers", thereby forming composite or agglomerated particles (or agglomerates). These composite particles are dried.
  • Their moisture content is advantageously less than 20%, preferably less than 10%.
  • Composite particles of larger size than the fine "primer” particles directly formed from the fine atomized droplets are thus obtained.
  • the other part of the newly sprayed droplets which are not agglomerated with other particles, form fine particles constituting new primers.
  • the moving particles meet and, in case of contact with a still aqueous surface, these particles agglomerate.
  • the agglomerated or composite particles thus formed in the fluidized air bed may have an onion-layer structure as shown in FIG. 7A, thus forming compact granules having a generally spherical outer surface, or a "raspberry" type structure As shown in Figure 7B.
  • FIG. 7A shows from top to bottom (schematically on the left side and in photo on the right side) a granule having an onion layer structure at different stages of formation: an initial nucleus or particle ( e) 1, a core 2 with two coating layers and the final product 3 comprising the core and several superposed coating layers.
  • FIG. 7A shows from top to bottom (schematically on the left side and in photo on the right side) a granule having an onion layer structure at different stages of formation: an initial nucleus or particle ( e) 1, a core 2 with two coating layers and the final product 3 comprising the core and several superposed coating layers.
  • FIG. 7B shows from left to right a granule having a raspberry structure at different stages of formation: a first initial particle 4, a second initial particle 5, an agglomerated particle 6 obtained by agglomeration of the first and second initial particles 4, 5 and the final product 7 comprising a set of agglomerated particles in a cluster.
  • the particles of size greater than or equal to 200 ⁇ are removed from the installation and, at the outlet thereof, the finished product is obtained, namely the food additive in powder form.
  • a sieve may be placed at the outlet of the installation to remove too large particles, for example larger than 2000 m. These removed particles can then be crushed, then used as primers for next production or re-introduced (in milled form) into the current production. Finally, they can be solubilized again and atomized.
  • the particles thus produced are without coating.
  • the final product obtained by the process of the invention is therefore in the form of a powder of particles devoid of protective coating or protective layer.
  • the formation of particles within a fluidized air bed is carried out without primer.
  • the fluidized air bed initially contains, before triggering the E12 sputtering, already formed particles constituting primers. These particles are generally the particles remaining in the fluidized air bed at the end of production or too large particles that have been crushed or too fine formed.
  • These primers may also be composed of any type of powder or solid whose size will preferably be less than 2000 m.
  • the final product obtained from the solution of Example 1 (containing 10% by weight of capsicum oleoresin, excluding water) has a controlled particle size, the size of 90% of the particles being greater than 200. m. In addition, the product is non-irritating.
  • the final product obtained from the solution of Example 1 .2 (containing 20% by weight of capsicum oleoresin, excluding water) has properties similar to those of the product obtained from the solution of the invention. Example 1 .1.
  • the final product obtained from the solution of Example 1 .3 has a particle size greater than or equal to 200 m and is very mildly irritating. Similar results are obtained with the solution of Example 1 .4. Another test was carried out by simple atomization (with flow of heat but without fluidized air bed) from this same solution of Example 1 .3. The final product obtained is a very dusty powder containing 100% fine particles smaller than 100 ⁇ , which has a very irritating effect.
  • the operation for producing the powder comprises the steps E1 to E3 described below with reference to FIG. 1 and for various embodiment examples. .
  • step E1 it is equipped with a support S in powder form which contains at least 90% by weight of solid particles of size greater than or equal to 200 m.
  • the carrier powder S can be chosen from vegetable or mineral compounds, for example from one of the compounds of the group comprising almond shell, corn cob, coal, salt, silica, sepiolite, clay, diatomaceous earth and calcium carbonate.
  • the support powder S is the commercial support Diamol Dl 20KF ⁇ , containing diatomaceous earth.
  • the carrier powder has a capacity of sorption (that is to say of absorption and adsorption) of liquid at least greater than or equal to 1% of its weight, preferably greater than or equal to 10% of its weight, advantageously greater than or equal to 50% of its weight, or advantageously still greater than 100% of its weight.
  • step E2 it is provided with at least one liquid, denoted “L n " (n corresponding to the index of an embodiment), containing the first substance classified Xi, Xn or C.
  • this first substance used has an irritating effect. It is therefore classified Xi.
  • This is oleoresin capsicum, containing the active substances capsaicin and dihydrocapsaicin.
  • the oleoresin capsicum is in the form of a viscous liquid.
  • the liquid L n may contain only the first substance, or a mixture containing the first substance and:
  • one or more other substance chosen, for example, from aromatic substances (having an odor) and / or taste substances (that is to say substances that provide a salty, sweet flavor); acid, bitter or umami), and / or
  • Step E2 comprises the preparation of the mixture.
  • Step E2 may comprise a sub-step of dissolving the active substance in a liquid solvent, in particular a solvent of the group comprising water, ethanol and an oil, in order to obtain said liquid containing the active substance .
  • the liquid used, noted L-i contains only the first substance, namely oleoresin capsicum.
  • a liquid denoted L 2 , is prepared by mixing:
  • the irritating active substance namely here the oleoresin of capsicum
  • aromatic substances which here consist of phytonutrients, in this case carvacrol and cinnamaldehyde, and water.
  • a liquid, denoted L 3 is prepared by mixing:
  • the irritating active substance namely here the oleoresin of capsicum
  • a sweetener in this case saccharin
  • a liquid, noted L 4 is prepared by mixing:
  • the irritating active substance namely here the oleoresin of capsicum
  • aromatic substances which consist here of phytonutrients, in this case eugenol and cinnamaldehyde, and
  • a sweetener in this case saccharin
  • the carrier powder in this case Diamol® 20KF
  • the liquid L n being equal to 1, 2, 3 or 4.
  • the relative proportions of carrier powder S and liquid L n (in other words the liquid / carrier ratio) in the mixture produced are adapted so that that the liquid L n penetrates by absorption inside the solid particles of the carrier powder and forms by adsorption an outer envelope on the surface of said particles.
  • This liquid envelope acts as a link interface between particles.
  • composite particles can be formed by agglomeration of smaller size particles bonded together by their outer liquid envelopes which play a role of binding phase or binding interface.
  • the relative proportions of liquid and solid carrier powder in the mixture are adapted so as to obtain an end product (that is to say at the end of the mixture of the carrier powder S and the liquid L n ). which is in the form of a free flow powder and without caking.
  • This final product contains agglomerates of particles, the percentage of agglomerates having a size of less than or equal to 2 mm reaching at least 90%, advantageously 95%, advantageously still 99%.
  • the particles of the support S absorb the liquid L n and, the liquid L n being added to the support in slight excess, the support S becomes slightly oversaturated. This results in the formation of an envelope (or "layer”, or “film") of liquid L n at the surface of the support particles S.
  • This liquid L n at the surface of the support particles S makes it possible, in particular, to retain particles "Fines" potentially present in the support S.
  • the "fine particles” are particles less than or equal to 100 m in size.
  • these fine particles are troublesome because they may produce an irritating effect. Thanks to the liquid envelope L n at the surface of the particles of the support S "charged" (that is to say having absorbed and adsorbed the liquid L n ), these fine particles agglomerate with other particles of the support S, in particular to support particles of size greater than or equal to 200 ⁇ , so as to form composite particles, or agglomerates, of size greater than or equal to 200 m. Thus, the fine particles are retained, trapped by the liquid envelopes particles of the support S. These liquid envelopes play the role of binder phase.
  • a range of support ratios S / liquid L n in other words, respective proportions of support S and liquid L n , which is suitable for mixing in step E3 in order to obtain a final product in the form of a powder which is free from flow and without caking. More precisely, the final product must be in the form of a powder which contains agglomerates of particles, or composite particles, all the agglomerates having a size of less than or equal to 2 mm.
  • FIG 3 there is shown a carrier powder "not loaded", before being mixed with a liquid L n .
  • the step E0 was carried out for a support S consisting of Diamol Dl 20KF ⁇ and for a reference liquid (for example water), denoted L 0
  • FIG. 4A shows the final product obtained by mixing 65% by weight of the support powder S and 35% by weight of the reference liquid L 0 .
  • the final product is "unsaturated". It is in the form of a powder of particles having absorbed all the liquid L 0 The particles obtained at the end of the mixing step E3 are not covered with a liquid envelope L 0 . The powder is free from flow.
  • FIG. 4B the trace left by the resulting powder which has been deposited and then removed from the bottom in a glass cup is shown. We see that the product leaves very little trace. This indicates that the amount of liquid on the surface is not sufficient to form a bonding surface. The absence or the too small bonding surface formed does not therefore make it possible to fix the fine particles. Therefore the product is potentially irritating.
  • FIG. 5A shows the final product obtained by mixing 62% by weight of the carrier powder S and 38% by weight of the reference liquid L 0.
  • the final product is slightly "oversaturated". It is in the form of a particle powder having absorbed all the liquid L 0 and covered with a liquid envelope L 0 .
  • the powder is free from flow.
  • Figure 5B there is shown the trace left by the resulting powder which was deposited in a glass cup and removed. We see that the product leaves a slightly larger trace than in Figure 4B, but this is still limited.
  • the final product obtained thus has a layer of liquid capable of forming a connecting surface allowing part of the product to adhere to the walls of the container.
  • This bonding surface is able to bind to the fine particles present in the product, which therefore limits the risk of irritation.
  • the proportion of liquid L 0 in the mixture produced is sufficient to retain the fine particles and is not excessive so that the product remains free from flow and without caking.
  • the product obtained contains agglomerates of particles smaller than 2 mm, so that this does not alter the flow of the product.
  • FIG. 6A shows the final product obtained by mixing 57% by weight of the carrier powder S and 43% by weight of the reference liquid L 0.
  • the final product is clearly "oversaturated”. It is mottant and not free of flow.
  • Figure 6B shows the trace left by the resulting powder which has been deposited in a glass cup and removed. We see that the product leaves an important trace in the cup (the bottom of the cup remains covered almost entirely product).
  • the proportion of liquid L 0 in the mixture produced is in this case excessive.
  • the product obtained contains agglomerates of particles greater than 2 mm in size which indicate the start of caking and have the effect of greatly reducing the flow properties of the product. The three tests carried out make it possible to conclude that the proportion of liquid
  • L 0 in the carrier-liquid mixture must be greater than 35% and less than 43%.
  • the invention also relates to an animal feed additive in the form of a particle powder containing a substance classified in one of the three categories respectively identified by the codes Xi, Xn and C.
  • the powder comprises at least 90% of particles without material. fat, greater than or equal to 200 m. It is advantageously obtained by implementing the manufacturing method described above. The particles are advantageously without coating.
  • all particles larger than or equal to 200 m have a particle agglomerate structure of smaller size (i.e., less than 200 m). These particles may have a raspberry type structure, or an onion layer structure or an intermediate structure between these two structures.
  • the particles having an agglomerate structure, or composite particles comprise a particle of a support material and a liquid incorporated in the support material particle and forming an envelope on the surface of the support material. This envelope on the surface of the support material allows the particle to bind to the fine particles contained in the product.

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  • Polymers & Plastics (AREA)
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Abstract

The invention relates to an additive in the form of a powder of particles containing at least one first substance classified in one of the three categories respectively identified by the codes Xi, Xn and C. The method comprises an operation of producing said powder by thermal-spraying a solution containing said first substance, at least 90% of the particles in the powder produced being larger than or equal to 200 μm.

Description

Titre : Procédé de fabrication d'un additif destiné à l'alimentation animale et un additif correspondant  Title: Process for the production of an additive for animal feed and a corresponding additive
La présente invention concerne un procédé de fabrication d'un additif destiné à l'alimentation animale et un additif correspondant. The present invention relates to a method of manufacturing an additive for animal feed and a corresponding additive.
Dans le domaine de l'alimentation animale, notamment en élevage, l'utilisation de substances actives d'extraits végétaux présente un grand intérêt pour améliorer les performances zootechniques animales, c'est-à-dire améliorer le gain moyen quotidien des animaux et/ou l'indice de consommation des animaux et/ou l'efficacité de la reproduction animale. Les extraits de plantes peuvent être une alternative à certains antibiotiques qui sont couramment employés à titre préventif dans l'alimentation des animaux mais auraient potentiellement des effets secondaires indésirables sur la santé des consommateurs tels que de développer une résistance bactérienne chez l'homme. In the field of animal nutrition, especially in breeding, the use of active substances of plant extracts is of great interest to improve animal zootechnical performance, that is to say, to improve the average daily gain of animals and / or the index of animal consumption and / or the efficiency of animal reproduction. Plant extracts can be an alternative to some antibiotics that are commonly used as a preventative in animal nutrition but could potentially have undesirable side effects on consumer health such as developing bacterial resistance in humans.
L'un des extraits végétaux présentant un grand intérêt zootechnique est l'oléorésine de capsicum. Cet extrait de plante contient notamment deux substances actives : la capsaïcine et la dihydrocapsaïcine. Il se présente généralement sous la forme d'un liquide visqueux. On sait que l'utilisation d'oléorésine de capsicum permet de modifier le comportement alimentaire, notamment la prise d'aliments, d'améliorer la digestibilité de certains nutriments tels que les carbohydrates et les graisses et de moduler la réponse immunitaire, chez les animaux ruminants et/ou monogastriques. One of the vegetable extracts of great zootechnical interest is the oleoresin of capsicum. This plant extract contains in particular two active substances: capsaicin and dihydrocapsaicin. It is generally in the form of a viscous liquid. The use of oleoresin capsicum is known to modify dietary behavior, including food intake, to improve the digestibility of certain nutrients such as carbohydrates and fats and to modulate the immune response in animals. ruminants and / or monogastrics.
Cependant, la capsaïcine et la dihydrocapsaïcine sont des substances extrêmement irritantes lorsqu'elles entrent en contact avec la muqueuse nasale. Elles ne sont toutefois pas volatiles. Par conséquent, utilisées sous forme liquide, elles ne présentent pas de risque d'irritation des muqueuses nasales, même à une distance faible, dans la mesure où on évite tout contact direct avec la muqueuse. Afin de limiter le risque d'irritation, notamment pour les utilisateurs qui doivent manipuler ces substances afin de les incorporer dans l'alimentation animale, la capsaïcine et la dihydrocapsaïcine sont donc usuellement utilisées sous forme liquide. Toutefois, l'utilisation d'un additif alimentaire sous forme liquide est contraignante et mal adaptée. Dans le cas où l'additif doit être mélangé à une poudre avant d'être fourni à l'animal, le mélange final obtenu peut présenter certains inconvénients : distribution non homogène des substances actives, formation d'agrégats, caractère irritant. However, capsaicin and dihydrocapsaicin are extremely irritating substances when they come into contact with the nasal mucosa. They are not volatile, however. Therefore, used in liquid form, they do not present a risk of irritation of the nasal mucosa, even at a small distance, insofar as it avoids any direct contact with the mucosa. In order to limit the risk of irritation, especially for users who must handle these substances in order to incorporate them into the animal feed, capsaicin and dihydrocapsaicin are therefore usually used in liquid form. However, the use of a food additive in liquid form is restrictive and poorly adapted. In the case where the additive must be mixed with a powder before being supplied to the animal, the final mixture obtained may have certain disadvantages: non-homogeneous distribution of the active substances, formation of aggregates, irritancy.
L'utilisation d'un additif alimentaire sous forme de poudre, incorporant les substances actives de capsaïcine et de dihydrocapsaïcine, permettrait d'éviter certains de ces inconvénients, notamment de faciliter une distribution homogène de l'additif dans le mélange et d'éviter la formation d'agrégats. Toutefois, dans ce cas, il convient de trouver une solution pour que le produit final sous forme de poudre ne soit pas irritant. The use of a food additive in powder form, incorporating the active substances of capsaicin and dihydrocapsaicin, would make it possible to avoid some of these drawbacks, in particular to facilitate a homogeneous distribution of the additive in the mixture and to avoid the aggregate formation. However, in this case, it is necessary to find a solution so that the final product in powder form is not irritating.
Une solution connue consiste à mélanger l'oléorésine de capsicum avec de la graisse, par exemple une huile végétale, et de former des particules en forme de billes. Par exemple, FR 2 908 600 décrit un procédé de fabrication d'un additif alimentaire pour animal sous forme de poudre par atomisation à froid d'un mélange liquide contenant une matière grasse d'encapsulation et un agent actif tel que des capsaïcinoïdes. L'utilisation d'un support graisseux d'encapsulation de l'agent actif permet de limiter l'effet irritant du produit final sous forme de poudre. Pour réduire davantage l'effet irritant, les particules peuvent être enrobées ou encapsulées par une couche de revêtement extérieur. Une telle solution s'avère coûteuse et complexe à mettre en œuvre. En outre, l'utilisation d'un support graisseux est problématique en raison du risque important de dégradation par fonte du produit obtenu selon la température ambiante. La conservation d'un tel produit est donc délicate. A known solution is to mix the oleoresin capsicum with fat, for example a vegetable oil, and form particles in the form of beads. For example, FR 2,908,600 discloses a method of manufacturing a powdered animal feed additive by cold atomization of a liquid mixture containing an encapsulating fat and an active agent such as capsaicinoids. The use of a fatty support for encapsulation of the active agent makes it possible to limit the irritating effect of the final product in the form of a powder. To further reduce the irritant effect, the particles may be coated or encapsulated by an outer coating layer. Such a solution is expensive and complex to implement. In addition, the use of a fatty medium is problematic because of the significant risk of degradation by melting the product obtained according to the ambient temperature. The preservation of such a product is therefore delicate.
La présente invention vient améliorer la situation. A cet effet, l'invention concerne un procédé de fabrication d'un additif destiné à l'alimentation animale sous forme d'une poudre de particules contenant au moins une première substance classée dans l'une des trois catégories respectivement identifiées par les codes Xi, Xn et C, caractérisé en ce qu'il comprend une opération de production de ladite poudre par atomisation à chaud d'une solution contenant ladite première substance, la poudre produite contenant au moins 90% de particules de taille supérieure ou égale à 200 m. L'invention tire son origine d'un problème lié à la présence d'oléorésine de capsicum, qui contient des substances actives irritantes, dans un additif alimentaire animal. La demanderesse entend toutefois ne pas limiter la portée de sa demande à cet exemple particulier mais l'étendre à tout additif alimentaire contenant une substance ayant un effet au moins irritant, notamment un effet irritant et/ou nocif et/ou corrosif. De telles substances ayant un effet irritant, nocif ou corrosif sont respectivement identifiées par les symboles Xi ou Xn ou C selon la directive 1999/45/CE. The present invention improves the situation. For this purpose, the invention relates to a method for manufacturing an additive intended for animal feed in the form of a powder of particles containing at least a first substance classified in one of the three categories respectively identified by the Xi codes. , Xn and C, characterized in that it comprises an operation for producing said powder by hot atomization of a solution containing said first substance, the powder produced containing at least 90% of particles of size greater than or equal to 200 m . The invention originates from a problem related to the presence of capsicum oleoresin, which contains irritating active substances, in an animal feed additive. However, the Applicant intends not to limit the scope of its application to this particular example but to extend it to any food additive containing a substance having an at least irritating effect, especially an irritating and / or harmful and / or corrosive effect. Such substances having an irritant, harmful or corrosive effect are respectively identified by the symbols Xi or Xn or C according to Directive 1999/45 / EC.
La fabrication d'un additif sous forme d'une poudre constituée de particules de taille contrôlée et supérieure ou égale à 200 m permet de réduire très nettement l'effet irritant (ou nocif ou corrosif) du produit final (l'additif) contenant la substance irritante Xi (ou Xn ou C). En outre, lors de la fabrication de la poudre, des particules fines sont susceptibles de se former par fraction et/ou abrasion des particules du produit fini. Selon le procédé de l'invention, pour produire l'additif sous forme de poudre, on utilise une technique de formation de particules par atomisation à chaud qui permet de réaliser une agglomération de particules. Autrement dit, on forme des particules composites ou agglomérées à partir de particules de taille inférieure. En raison du phénomène d'agglomération qui se produit durant le processus de formation des particules, les éventuelles particules fines s'agglomèrent à d'autres particules. Il en résulte une forte réduction de l'effet irritant du produit final obtenu. Dans un mode de réalisation particulier, la poudre est produite par atomisation en lit d'air fluidisé. La solution contenant la première substance est avantageusement dépourvue de matière grasse. Avantageusement encore, la solution est aqueuse. The manufacture of an additive in the form of a powder consisting of particles of controlled size and greater than or equal to 200 m makes it possible to very clearly reduce the irritant (or harmful or corrosive) effect of the final product (the additive) containing the irritating substance Xi (or Xn or C). In addition, during the manufacture of the powder, fine particles are likely to form by fraction and / or abrasion of the particles of the finished product. According to the process of the invention, in order to produce the additive in the form of a powder, a hot-spray particle formation technique is used which makes it possible to agglomerate particles. In other words, composite or agglomerated particles are formed from particles of smaller size. Due to the agglomeration phenomenon that occurs during the particle formation process, any fine particles agglomerate with other particles. This results in a strong reduction of the irritating effect of the final product obtained. In a particular embodiment, the powder is produced by atomization in a fluidized air bed. The solution containing the first substance is advantageously free of fat. Advantageously, the solution is aqueous.
De préférence, les particules produites sont sans enrobage. Avantageusement, le procédé comprend une étape de réglage d'au moins un paramètre opératoire destiné à contrôler la taille des particules solides du produit final obtenu, la taille souhaitée des particules étant supérieure ou égale à 200 pm. La solution peut contenir au moins une substance aromatique ayant une odeur et/ou une substance gustative ayant une saveur. Preferably, the particles produced are uncoated. Advantageously, the method comprises a step of adjusting at least one operating parameter intended to control the size of the solid particles of the final product obtained, the desired size of the particles being greater than or equal to 200 μm. The solution may contain at least one aromatic substance having an odor and / or taste substance having a flavor.
La solution peut contenir un édulcorant. La solution peut également contenir un émulsifiant. The solution may contain a sweetener. The solution may also contain an emulsifier.
Avantageusement, la solution contient : Advantageously, the solution contains:
• entre 0,1 % et 100% en poids de ladite première substance ; Between 0.1% and 100% by weight of said first substance;
• entre 0% et 99,9% en poids d'un édulcorant ; Between 0% and 99.9% by weight of a sweetener;
· entre 0% et 99,9% en poids d'un émulsifiant et/ou d'un solvant.  Between 0% and 99.9% by weight of an emulsifier and / or a solvent.
Ladite première substance peut être l'oléorésine de capsicum. Said first substance may be oleoresin capsicum.
Avantageusement, l'additif contient entre 0,1 % et 99% en poids de ladite première substance. L'invention concerne aussi un additif alimentaire destiné à l'alimentation animale sous forme d'une poudre de particules contenant une première substance classée dans l'une des trois catégories respectivement identifiées par les codes Xi, Xn et C, caractérisé en ce que ladite poudre comprend au moins 90% de particules de taille supérieure ou égale à 200 μηπ, sans matière grasse, présentant une structure de type framboise ou une structure en couches d'oignon ou une structure intermédiaire entre une structure de type framboise et une structure en couches d'oignon. L'additif est avantageusement obtenu selon le procédé de fabrication précédemment défini. Advantageously, the additive contains between 0.1% and 99% by weight of said first substance. The invention also relates to a feed additive intended for animal feed in the form of a powder of particles containing a first substance classified in one of the three categories respectively identified by the codes Xi, Xn and C, characterized in that the said powder comprises at least 90% of particles of size greater than or equal to 200 μηπ, without fat, having a raspberry-like structure or an onion-layer structure or an intermediate structure between a raspberry-like structure and a layered structure onion. The additive is advantageously obtained according to the previously defined manufacturing method.
L'invention sera mieux comprise à l'aide de la description suivante de deux modes de réalisation particulier du procédé de fabrication d'un additif alimentaire animale selon l'invention, en référence aux dessins annexés sur lesquels : The invention will be better understood with the aid of the following description of two particular embodiments of the process for manufacturing an animal feed additive according to the invention, with reference to the appended drawings in which:
- La figure 1 représente un organigramme du procédé de fabrication selon un mode de réalisation ;  - Figure 1 shows a flowchart of the manufacturing method according to one embodiment;
- La figure 2 représente un organigramme du procédé de fabrication selon un autre mode de réalisation ;  FIG. 2 represents a flowchart of the manufacturing method according to another embodiment;
- La figure 3 représente un poudre support sous forme de poudre utilisé par le procédé de la figure 1 , avant mélange ;  FIG. 3 represents a support powder in powder form used by the process of FIG. 1, before mixing;
- Les figures 4A et 4B représentent  - Figures 4A and 4B represent
o le produit final obtenu par mélange de la poudre support sous forme de poudre de la figure 3 et d'un liquide dans des proportions respectives de 65% et de 35% en poids,  the final product obtained by mixing the powdery carrier powder of FIG. 3 and a liquid in respective proportions of 65% and 35% by weight,
o la trace laissée au fond d'un récipient en verre ayant contenu ce mélange ;  o the trace left in the bottom of a glass container that has contained this mixture;
- Les figures 5A et 5B représentent  - Figures 5A and 5B represent
o le produit final obtenu par mélange de la poudre support sous forme de poudre de la figure 3 et d'un liquide dans des proportions respectives de 62% et de 38% en poids, o la trace laissée au fond d'un récipient en verre ayant contenu ce mélange ; the final product obtained by mixing the powdery carrier powder of FIG. 3 and a liquid in respective proportions of 62% and 38% by weight, o the trace left in the bottom of a glass container that has contained this mixture;
- Les figures 6A et 6B représentent  - Figures 6A and 6B represent
o le produit final obtenu par mélange de la poudre support sous forme de poudre de la figure 3 et d'un liquide dans des proportions respectives de 57% et de 43% en poids,  the final product obtained by mixing the powdery carrier powder of FIG. 3 and a liquid in respective proportions of 57% and 43% by weight,
o la trace laissée au fond d'un récipient en verre ayant contenu ce mélange.  o the trace left at the bottom of a glass container that has contained this mixture.
- Les figures 7A et 7B représentent des particules agglomérées à différents stade de leur formation, l'une ayant une structure en couches d'oignon, l'autre ayant une structure de type framboise.  - Figures 7A and 7B show agglomerated particles at different stages of their formation, one having an onion layer structure, the other having a raspberry-like structure.
Le procédé de fabrication de l'invention vise à produire un additif alimentaire animal sous forme d'une poudre de particules contenant une substance, dite « première substance », ayant un effet au moins irritant. L'additif peut être ajouté aux aliments fournis à des animaux, notamment en élevage. La première substance est ici une substance active, c'est-à-dire une substance ayant un effet physiologique sur l'animal. Par effet « au moins irritant », on entend ici désigner soit un effet irritantThe manufacturing method of the invention aims to produce an animal feed additive in the form of a powder of particles containing a substance, called "first substance", having an at least irritating effect. The additive can be added to the food supplied to animals, especially in breeding. The first substance is here an active substance, that is to say a substance having a physiological effect on the animal. By "at least irritating" effect, we mean here designating either an irritating effect
(par exemple irritant pour la peau, les muqueuses, les yeux et/ou les voies respiratoires), soit un effet nocif, soit un effet corrosif. En d'autres termes, la première substance peut être classée dans l'une des trois catégories de substances dites dangereuses et respectivement identifiées par les codes ou symboles Xi, Xn et C. Ces codes ou symboles font référence au système de signalisation des substances dangereuses tel que défini par la Directive européenne 1999/45/CE. Le tableau ci-dessous indique l'effet et la définition du risque de chacune de ces trois catégories de substances : (eg irritating to skin, mucous membranes, eyes and / or respiratory tract), either a harmful effect or a corrosive effect. In other words, the first substance can be classified in one of the three categories of substances referred to as dangerous and respectively identified by the codes or symbols Xi, Xn and C. These codes or symbols refer to the signaling system for hazardous substances as defined by the European Directive 1999/45 / EC. The table below shows the effect and risk definition of each of these three categories of substances:
Symbole Effet Identification (définition du danger) Symbol Effect Identification (definition of danger)
Xi Irritant substances et préparations non corrosives qui par contact immédiat, prolongé ou répété avec la peau ou les muqueuses peuvent entraîner une réaction inflammatoire. Xi Irritant substances and non-corrosive preparations which by immediate contact, prolonged or repeated with the skin or mucous membranes may cause an inflammatory reaction.
Xn Nocif Substances et préparations qui par inhalation, ingestion ou pénétration cutanée peuvent entraîner la mort ou nuire à la santé de manière aiguë ou chronique.  Xn Harmful Substances and preparations which through inhalation, ingestion or skin penetration may cause death or health damage either acutely or chronically.
C Corrosif Substances et préparations qui en contact avec des tissus vivants, peuvent exercer une action destructrice sur ces derniers.  C Corrosive Substances and preparations that come into contact with living tissues may have a destructive effect on them.
Le procédé de fabrication d'un additif alimentaire animal de l'invention comprend une opération de production d'une poudre de particules, qui comporte la formation de particules composites ou agglomérées, obtenues par agglomération de particules de taille inférieure (c'est-à-dire de taille inférieure à celle des particules composites). Par définition, une particule « composite » est un agglomérat de plusieurs particules, autrement dit une particule formée par l'agglomération d'autres particules. La poudre produite par le procédé de l'invention contient au moins 90% de particules de taille supérieure ou égale à 200 μιτι. The method for manufacturing an animal food additive of the invention comprises an operation for producing a particle powder, which comprises the formation of composite or agglomerated particles, obtained by agglomeration of particles of smaller size (that is, -size smaller than the composite particles). By definition, a "composite" particle is an agglomerate of several particles, in other words a particle formed by the agglomeration of other particles. The powder produced by the process of the invention contains at least 90% of particles of size greater than or equal to 200 μιτι.
Selon un premier mode de réalisation du procédé de fabrication de l'additif alimentaire de l'invention, l'opération de production de la poudre est réalisée par atomisation (c'est-à-dire pulvérisation) à chaud d'une solution contenant la première substance, par exemple par atomisation en lit d'air fluidisé. L'opération de production de la poudre comporte les étapes E1 1 à E14 décrites ci-après en référence à la figure 2. According to a first embodiment of the method for manufacturing the food additive of the invention, the operation for producing the powder is carried out by atomization (that is to say, spraying) while hot of a solution containing the first substance, for example by atomization in a fluidized air bed. The operation for producing the powder comprises the steps E1 1 to E14 described below with reference to FIG.
La solution atomisée à chaud est dépourvue de matière grasse. Dans l'exemple de réalisation décrit ici, la solution est aqueuse. The hot atomized solution is free of fat. In the embodiment described here, the solution is aqueous.
Lors de l'étape E1 1 , on prépare une solution à pulvériser (ou atomiser), notée « SPm », contenant la substance active, en l'espèce l'oléorésine de capsicum. A cet effet, on solubilise la substance active qui peut être initialement sous forme liquide ou solide (par exemple sous de forme de poudre) dans un solvant. Dans le mode de réalisation décrit ici, on prépare une solution aqueuse. Le solvant utilisé est donc de l'eau. In step E1 1, a solution to be sprayed (or atomized), denoted "SP m ", containing the active substance, in this case oleoresin capsicum. For this purpose, the active substance which can be initially in liquid or solid form (for example in powder form) is solubilized in a solvent. In the embodiment described herein, an aqueous solution is prepared. The solvent used is therefore water.
Lors de l'étape E1 1 (ainsi que lors de l'étape E2) de préparation de la solution, on peut également ajouter au mélange de substance active et de solvant tout ou partie des composants suivants : During step E1 1 (as well as during step E2) of preparation of the solution, it is also possible to add all or part of the following components to the mixture of active substance and solvent:
- un ou plusieurs autres solvant(s) ;  one or more other solvent (s);
- un ou plusieurs émulsifiant(s) ;  - one or more emulsifier (s);
- une ou plusieurs substance(s) aromatique(s) ;  - one or more aromatic substance (s);
- une ou plusieurs substance(s) gustative(s) (une substance gustative étant une substance apportant une saveur salée, sucrée, acide, amer ou umami), notamment un ou plusieurs édulcorant(s) ;  - one or more taste substance (s) (a taste substance being a substance providing a salty, sweet, sour, bitter or umami flavor), in particular one or more sweetener (s);
- un support de pulvérisation, par exemple du chlorure de sodium ou de la maltodextrine, qui est de préférence soluble ou dispersible (par exemple de la farine de blé).  a spraying medium, for example sodium chloride or maltodextrin, which is preferably soluble or dispersible (for example wheat flour).
L'émulsifiant peut être de la gomme arabique. La gomme arabique permet en outre de solubiliser des composés aromatiques insolubles dans l'eau et sert également de support. The emulsifier may be gum arabic. Gum arabic also makes it possible to solubilize aromatic compounds that are insoluble in water and also serves as a support.
D'une manière générale, la solution à atomiser contient : In general, the solution to be atomized contains:
• entre 0,1 % et 100% en poids de la première substance ;  Between 0.1% and 100% by weight of the first substance;
• entre 0% et 99,9% en poids d'un édulcorant ;  Between 0% and 99.9% by weight of a sweetener;
• entre 0% et 99,9% en poids d'un émulsifiant et/ou d'un solvant comme l'eau.  Between 0% and 99.9% by weight of an emulsifier and / or a solvent such as water.
Un agent de charge peut être ajouté de façon additionnelle dans cette solution. Différents exemples de solution à pulvériser SPm sont donnés dans les tableaux qui suivent (« m » correspondant à l'indice de l'exemple considéré). Il s'agit ici de solutions aqueuses, seuls les composants de la solution autres que l'eau étant indiqués. A charging agent may be added additionally in this solution. Various examples of sputtering solution SP m are given in the following tables ("m" corresponding to the index of the example under consideration). he here aqueous solutions, only the components of the solution other than water being indicated.
Exemple 1 .1 : Example 1 .1:
Ingrédients % (en poids)  Ingredients% (by weight)
Gomme arabique 63  Gum arabic 63
Maltodextrine 27  Maltodextrin 27
Oléorésine de capsicum 10  Oleoresin Capsicum 10
Exemple 1 .2 : Example 1 .2
Ingrédients % (en poids)  Ingredients% (by weight)
Gomme arabique 56  Arabic gum 56
Maltodextrine 24  Maltodextrin 24
Oléorésine de capsicum 20  Oleoresin Capsicum 20
Exemple 1 .3 : Example 1 .3
Ingrédients kg  Ingredients kg
Sodium de saccharinate 940  Sodium saccharinate 940
Gomme arabique 100  Gum arabic 100
Oléorésine de capsicum 50  Oleoresin Capsicum 50
Exemple 1 .4 : Example 1 .4
Ingrédients kg  Ingredients kg
Sodium de saccharinate 930  Sodium saccharinate 930
Gomme arabique 1 15  Gum arabic 1 15
Oléorésine de capsicum 30 Lors de l'étape E1 1 , les différents composants indiqués dans les tableaux relatifs aux exemples 1 .1 à 1 .4 sont mélangés et solubilisés dans de l'eau. Le ratio entre eau et composants à solubiliser est compris entre 0,5 et 5, préférentiellement entre 0,6 et 1 . On obtient ainsi une solution à pulvériser SPm, avec m égal à 1 , 2, 3 ou 4 selon l'exemple de réalisation correspondant. La quantité d'eau doit être suffisante pour permettre la solubilité des différents ingrédients dans l'eau. L'étape E1 1 est suivie d'une étape E12 de pulvérisation ou d'atomisation de la solution SPm dans un lit d'air fluidisé. Lors de cette étape d'atomisation E12, on pulvérise la solution SPm en fines goutelettes dans un lit d'air fluidisé. Oleoresin Capsicum 30 In step E1 1, the various components indicated in the tables relating to Examples 1 .1 to 1 .4 are mixed and solubilized in water. The ratio between water and components to be solubilized is between 0.5 and 5, preferably between 0.6 and 1. This gives a spray solution SP m , with m equal to 1, 2, 3 or 4 according to the corresponding embodiment. The amount of water must be sufficient to allow the solubility of the various ingredients in the water. Step E1 1 is followed by a step E12 of spraying or atomizing the SP m solution in a fluidized air bed. During this atomization step E12, the solution SP m is sprayed into fine droplets in a fluidized air bed.
Suite à la pulvérisation E12, le procédé se poursuit par une étape E13 de formation de particules au sein du lit d'air fluidisé de l'installation de production. La taille minimale des particules autorisées à être évacuées du lit d'air fluidisé est réglée par un paramètre opératoire de l'installation, les particules de taille inférieure à cette taille minimale étant maintenues en suspension dans le lit d'air fluidisé. Dans le mode de réalisation décrit ici, la taille minimale est égale à 200 m. Ainsi, les particules de taille inférieure à la taille minimale réglée, notamment les particules fines, ne sont pas autorisées à sortir et sont maintenues en suspension dans le lit d'air fluidisé. Un opérateur ajuste certains paramètres, tels que le débit de sprayage, la température du lit d'air, le flux d'air, et..., sur l'installation de production lors d'une étape initiale de réglage E10. Cela permet de contrôler la taille des particules solides du produit final obtenu (c'est-à-dire du produit fini sortant de l'installation de production). Following the E12 spraying, the process continues with a step E13 of particle formation within the fluidized air bed of the production facility. The minimum size of the particles allowed to be evacuated from the fluidized air bed is regulated by an operating parameter of the installation, the particles smaller than this minimum size being kept in suspension in the fluidized air bed. In the embodiment described here, the minimum size is 200 m. Thus, the particles smaller than the minimum size set, especially the fine particles, are not allowed to leave and are held in suspension in the fluidized air bed. An operator adjusts certain parameters, such as the spray rate, the air bed temperature, the air flow, and ..., on the production plant during an initial adjustment step E10. This makes it possible to control the size of the solid particles of the final product obtained (that is to say the finished product leaving the production facility).
Notons que la pulvérisation E12 est déclenchée avant l'étape E13 de formation de particules et se poursuit de façon concomitante à cette étape E13, jusqu'à consommation totale de la solution à pulvériser. La pulvérisation est réalisée en continu (mais pourrait être réalisée de façon discontinue sur une période donnée). Lors de cette étape E13, les premières gouttelettes pulvérisées sont séchées et forment des particules fines. Progressivement, au fil de la pulvérisation E12, une partie des gouttelettes nouvellement formées viennent se fixer sur les particules déjà formées, notamment sur les particules « amorces », en formant ainsi des particules composites ou agglomérées (ou agglomérats). Ces particules composites sont séchées. Leur taux d'humidité est avantageusement inférieur à 20%, de préférence inférieur à 10%. On obtient ainsi des particules composites de taille supérieure à celle des particules fines « amorces » directement formées à partir des fines gouttelettes atomisées. L'autre partie des gouttelettes nouvellement pulvérisées, qui ne sont pas agglomérées à d'autres particules, forment des particules fines constituant de nouvelles amorces. D'autre part, dans le lit d'air fluidisé, les particules en mouvement se rencontrent et, en cas de contact avec une surface encore aqueuse, ces particules s'agglomèrent. Note that the E12 spray is triggered before the particle formation step E13 and continues concomitantly with this step E13, until total consumption of the spray solution. The spraying is carried out continuously (but could be carried out discontinuously over a given period). During this step E13, the first spray droplets are dried and form fine particles. Gradually, over the spraying E12, part of the newly formed droplets are fixed on the particles already formed, especially on the particles "primers", thereby forming composite or agglomerated particles (or agglomerates). These composite particles are dried. Their moisture content is advantageously less than 20%, preferably less than 10%. Composite particles of larger size than the fine "primer" particles directly formed from the fine atomized droplets are thus obtained. The other part of the newly sprayed droplets, which are not agglomerated with other particles, form fine particles constituting new primers. On the other hand, in the fluidized air bed, the moving particles meet and, in case of contact with a still aqueous surface, these particles agglomerate.
Les particules agglomérées ou composites ainsi formées dans le lit d'air fluidisé peuvent avoir une structure en couches d'oignon comme représenté sur la figure 7A, formant ainsi des granules compacts ayant une surface extérieure globalement sphérique, ou bien une structure de type « framboise » comme représenté sur la figure 7B. Sur la figure 7A, on a représenté de haut en bas (de façon schématique sur la partie gauche et en photo sur la partie droite) un granule ayant une structure en couches d'oignon à différents stades de formation : un noyau ou particule initial (e) 1 , un noyau 2 avec deux couches d'enrobage et le produit final 3 comportant le noyau et plusieurs couches d'enrobage superposées. Sur la figure 7B, on a représenté de la gauche vers la droite un granule ayant une structure de framboise à différents stades de formation : une première particule initiale 4, une deuxième particule initiale 5, une particule agglomérée 6 obtenue par agglomération des première et deuxième particules initiales 4, 5 et le produit final 7 comportant un ensemble de particules agglomérées en grappe. Lors d'une étape E14, les particules de taille supérieure ou égale à 200 μηπ sont évacuées de l'installation et, en sortie de celle-ci, on obtient le produit fini, à savoir l'additif alimentaire sous forme de poudre. Un tamis peut être placé en sortie de l'installation afin de retirer les particules de taille trop importante, par exemple de taille supérieure à 2000 m. Ces particules retirées peuvent ensuite être broyées, puis servir d'amorces pour une prochaine production ou être introduites de nouveau (sous forme broyée) dans la production en cours. Enfin, elles peuvent être solubilisées à nouveau et atomisées. Les particules ainsi produites sont sans enrobage. Le produit final obtenu par le procédé de l'invention est donc sous la forme d'une poudre de particules dépourvues de revêtement protecteur ou de couche protectrice. The agglomerated or composite particles thus formed in the fluidized air bed may have an onion-layer structure as shown in FIG. 7A, thus forming compact granules having a generally spherical outer surface, or a "raspberry" type structure As shown in Figure 7B. FIG. 7A shows from top to bottom (schematically on the left side and in photo on the right side) a granule having an onion layer structure at different stages of formation: an initial nucleus or particle ( e) 1, a core 2 with two coating layers and the final product 3 comprising the core and several superposed coating layers. FIG. 7B shows from left to right a granule having a raspberry structure at different stages of formation: a first initial particle 4, a second initial particle 5, an agglomerated particle 6 obtained by agglomeration of the first and second initial particles 4, 5 and the final product 7 comprising a set of agglomerated particles in a cluster. During a step E14, the particles of size greater than or equal to 200 μηπ are removed from the installation and, at the outlet thereof, the finished product is obtained, namely the food additive in powder form. A sieve may be placed at the outlet of the installation to remove too large particles, for example larger than 2000 m. These removed particles can then be crushed, then used as primers for next production or re-introduced (in milled form) into the current production. Finally, they can be solubilized again and atomized. The particles thus produced are without coating. The final product obtained by the process of the invention is therefore in the form of a powder of particles devoid of protective coating or protective layer.
Dans la description qui précède, la formation de particules au sein d'un lit d'air fluidisé est réalisée sans amorce. En variante, on peut envisager d'utiliser un procédé de pulvérisation et de formation de particules par lit d'air fluidisé avec amorce. Dans ce cas, le lit d'air fluidisé contient initialement, avant déclenchement de la pulvérisation E12, des particules déjà formées constituant des amorces. Ces particules sont généralement les particules restant dans le lit d'air fluidisé en fin de production ou des particules de taille trop importante broyées ou trop fines formées. Ces amorces peuvent aussi être composées de tout type de poudre ou solide dont la taille sera préférablement inférieure à 2000 m. On va maintenant décrire les résultats de tests réalisés avec les solutions des exemples 1 .1 à 1 .4, par la mise en œuvre des étapes E12 et E13. In the foregoing description, the formation of particles within a fluidized air bed is carried out without primer. Alternatively, one can consider using a method of spraying and particle formation per primer fluidized air bed. In this case, the fluidized air bed initially contains, before triggering the E12 sputtering, already formed particles constituting primers. These particles are generally the particles remaining in the fluidized air bed at the end of production or too large particles that have been crushed or too fine formed. These primers may also be composed of any type of powder or solid whose size will preferably be less than 2000 m. The results of tests carried out with the solutions of Examples 1 .1 to 1 .4 will now be described, by the implementation of steps E12 and E13.
Le produit final obtenu à partir de la solution de l'exemple 1 .1 (contenant 10% en poids d'oléorésine de capsicum, sans compter l'eau) présente une granulométrie contrôlée, la taille de 90% des particules étant supérieure à 200 m. En outre, le produit est non irritant. Le produit final obtenu à partir de la solution de l'exemple 1 .2 (contenant 20% en poids d'oléorésine de capsicum, sans compter l'eau) présente des propriétés similaires à celles du produit obtenu à partir de la solution de l'exemple 1 .1 . The final product obtained from the solution of Example 1 (containing 10% by weight of capsicum oleoresin, excluding water) has a controlled particle size, the size of 90% of the particles being greater than 200. m. In addition, the product is non-irritating. The final product obtained from the solution of Example 1 .2 (containing 20% by weight of capsicum oleoresin, excluding water) has properties similar to those of the product obtained from the solution of the invention. Example 1 .1.
Le produit final obtenu à partir de la solution de l'exemple 1 .3 présente une granulométrie supérieure ou égale à 200 m et est très peu irritant. On obtient des résultats similaires avec la solution de l'exemple 1 .4. Un autre test a été réalisé par atomisation simple (avec flux de chaleur mais sans lit d'air fluidisé) à partir de cette même solution de l'exemple 1 .3. Le produit final obtenu est une poudre très poussiéreuse, contenant 100% de particules fines de taille inférieure à 100 μηπ, qui a un effet très irritant. Selon un deuxième mode de réalisation du procédé de fabrication de l'additif alimentaire de l'invention, l'opération de production de la poudre comporte les étapes E1 à E3 décrites ci-après en référence à la figure 1 et pour différents exemples de réalisation. Lors de l'étape E1 , on se munit d'un support S sous forme de poudre qui contient au moins 90% en poids de particules solides de taille supérieure ou égale à 200 m. La poudre support S peut être choisie parmi des composés végétaux ou minéraux, par exemple parmi l'un des composés du groupe comportant de la coque d'amande, de la rafle de maïs, du charbon, du sel, de la silice, de la sépiolite, de l'argile, de la terre de diatomée et du carbonate de calcium. Dans l'exemple de réalisation particulier décrit ici, la poudre support S est le support commercial Diamol Dl 20KF©, contenant de la terre de diatomée. La poudre support a une capacité de sorption (c'est-à-dire d'absorption et d'adsorption) de liquide au moins supérieure ou égale à 1 % de son poids, préférentiellement supérieure ou égale à 10% de son poids, avantageusement supérieure ou égale à 50% de son poids, ou avantageusement encore supérieure à 100% de son poids. Lors de l'étape E2, on se munit d'au moins un liquide, noté « Ln » (n correspondant à l'indice d'un exemple de réalisation), contenant la première substance classée Xi, Xn ou C. Dans les exemples de réalisation décrits plus loin, cette première substance utilisée a un effet irritant. Elle est donc classée Xi. Il s'agit en l'espèce de l'oléorésine de capsicum, contenant les substances actives de capsaïcine et de dihydrocapsaïcine. L'oléorésine de capsicum se présente sous forme d'un liquide visqueux. Le liquide Ln peut contenir uniquement la première substance, ou un mélange contenant la première substance et : The final product obtained from the solution of Example 1 .3 has a particle size greater than or equal to 200 m and is very mildly irritating. Similar results are obtained with the solution of Example 1 .4. Another test was carried out by simple atomization (with flow of heat but without fluidized air bed) from this same solution of Example 1 .3. The final product obtained is a very dusty powder containing 100% fine particles smaller than 100 μηπ, which has a very irritating effect. According to a second embodiment of the process for manufacturing the food additive of the invention, the operation for producing the powder comprises the steps E1 to E3 described below with reference to FIG. 1 and for various embodiment examples. . During step E1, it is equipped with a support S in powder form which contains at least 90% by weight of solid particles of size greater than or equal to 200 m. The carrier powder S can be chosen from vegetable or mineral compounds, for example from one of the compounds of the group comprising almond shell, corn cob, coal, salt, silica, sepiolite, clay, diatomaceous earth and calcium carbonate. In the particular embodiment described here, the support powder S is the commercial support Diamol Dl 20KF ©, containing diatomaceous earth. The carrier powder has a capacity of sorption (that is to say of absorption and adsorption) of liquid at least greater than or equal to 1% of its weight, preferably greater than or equal to 10% of its weight, advantageously greater than or equal to 50% of its weight, or advantageously still greater than 100% of its weight. During step E2, it is provided with at least one liquid, denoted "L n " (n corresponding to the index of an embodiment), containing the first substance classified Xi, Xn or C. In examples of embodiments described below, this first substance used has an irritating effect. It is therefore classified Xi. This is oleoresin capsicum, containing the active substances capsaicin and dihydrocapsaicin. The oleoresin capsicum is in the form of a viscous liquid. The liquid L n may contain only the first substance, or a mixture containing the first substance and:
- une ou plusieurs autre(s) substance(s), choisie(s) par exemple parmi des substances aromatiques (ayant une odeur) et/ou des substances gustatives (c'est-à-dire des substances apportant une saveur salée, sucrée, acide, amer ou umami) , et/ou  one or more other substance (s) chosen, for example, from aromatic substances (having an odor) and / or taste substances (that is to say substances that provide a salty, sweet flavor); acid, bitter or umami), and / or
- un solvant organique ou inorganique, par exemple de l'éthanol ou de l'eau, contenant éventuellement un émulsifiant pour homogénéiser la solution. Dans le cas où le liquide Ln est un mélange, tel que défini ci-dessus, l'étape E2 comprend la préparation du mélange. L'étape E2 peut comprendre une sous-étape de dissolution de la substance active dans un solvant liquide, notamment un solvant du groupe comportant de l'eau, de l'éthanol et une huile, afin d'obtenir ledit liquide contenant la substance active. an organic or inorganic solvent, for example ethanol or water, optionally containing an emulsifier for homogenizing the solution. In the case where the liquid L n is a mixture, as defined above, the step E2 comprises the preparation of the mixture. Step E2 may comprise a sub-step of dissolving the active substance in a liquid solvent, in particular a solvent of the group comprising water, ethanol and an oil, in order to obtain said liquid containing the active substance .
Dans un premier exemple de réalisation, le liquide utilisé, noté L-i, contient uniquement la première substance, à savoir de l'oléorésine de capsicum. In a first exemplary embodiment, the liquid used, noted L-i, contains only the first substance, namely oleoresin capsicum.
Dans un deuxième exemple de réalisation, on prépare un liquide, noté L2, en mélangeant : In a second embodiment, a liquid, denoted L 2 , is prepared by mixing:
- la substance active irritante, à savoir ici l'oléorésine de capsicum, des substances aromatiques, qui sont ici constituées par des phytonutriments, en l'espèce du carvacrol et du cinnamaldéhyde, et de l'eau. the irritating active substance, namely here the oleoresin of capsicum, aromatic substances, which here consist of phytonutrients, in this case carvacrol and cinnamaldehyde, and water.
Dans un troisième exemple de réalisation, on prépare un liquide, noté L3, en mélangeant : In a third exemplary embodiment, a liquid, denoted L 3 , is prepared by mixing:
- la substance active irritante, à savoir ici l'oléorésine de capsicum, et the irritating active substance, namely here the oleoresin of capsicum, and
- de l'eau dans laquelle un édulcorant, en l'espèce de la saccharine, a été dissout. water in which a sweetener, in this case saccharin, has been dissolved.
Dans un quatrième exemple de réalisation, on prépare un liquide, noté L4, en mélangeant : In a fourth embodiment, a liquid, noted L 4 , is prepared by mixing:
- la substance active irritante, à savoir ici l'oléorésine de capsicum, the irritating active substance, namely here the oleoresin of capsicum,
- des substances aromatiques, qui sont ici constituées par des phytonutriments, en l'espèce de l'eugénol et du cinnamaldéhyde, etaromatic substances, which consist here of phytonutrients, in this case eugenol and cinnamaldehyde, and
- de l'eau dans laquelle un édulcorant, en l'espèce de la saccharine, a été dissout. water in which a sweetener, in this case saccharin, has been dissolved.
Lors de l'étape E3, on mélange la poudre support (ici Diamol© 20KF) avec le liquide Ln, n étant égal à 1 , 2, 3 ou 4. During step E3, the carrier powder (in this case Diamol® 20KF) is mixed with the liquid L n , n being equal to 1, 2, 3 or 4.
Les proportions relatives des différents composants de chacun des mélanges réalisés pour les différents exemples de réalisation sont indiquées dans les tableaux suivants : The relative proportions of the various components of each of the mixtures produced for the various embodiments are indicated in the following tables:
Exemple 2.1 : Example 2.1:
en %  in %
Diamol© 20KF 67 oléorésine de capsicum 33 Exemple 2.2 : Diamol © 20KF 67 capsicum oleoresin 33 Example 2.2:
Figure imgf000017_0001
Figure imgf000017_0001
Les proportions relatives de poudre support S et de liquide Ln (autrement dit le ratio liquide/support) dans le mélange réalisé sont adaptées de sorte à ce que le liquide Ln pénètre par absorption à l'intérieur des particules solides de la poudre support et forme par adsorption une enveloppe extérieure à la surface desdites particules. Cette enveloppe de liquide joue un rôle d'interface de liaison entre particules. Ainsi, des particules composites peuvent se former par agglomération de particules de taille inférieure liées entre elles par leurs enveloppes extérieures de liquide qui jouent un rôle de phase liante ou d'interface de liaison. Plus précisément, les proportions relatives de liquide et de poudre support solide dans le mélange sont adaptées de sorte à obtenir un produit final (c'est-à-dire à l'issue du mélange de la poudre support S et du liquide Ln) qui est sous la forme d'une poudre libre d'écoulement et sans mottage. Ce produit final contient des agglomérats de particules, le pourcentage des agglomérats ayant une taille inférieure ou égale à 2 mm atteignant au moins 90%, avantageusement 95%, avantageusement encore 99%. Ainsi, lors du mélange de l'étape E3, les particules du support S absorbent le liquide Ln et, le liquide Ln étant ajouté au support en léger excès, le support S devient légèrement sursaturé. Cela se traduit par la formation d'une enveloppe (ou « couche », ou « film ») de liquide Ln à la surface des particules de support S. Ce liquide Ln en surface des particules de support S permet notamment retenir des particules « fines » potentiellement présentes dans le support S. Par définition, les « particules fines » sont des particules de taille inférieure ou égale à 100 m. Elles sont susceptibles de se former par abrasion et/ou fraction des particules de taille supérieure du support S, lors de la manipulation et du transport du support sous forme de poudre, ou bien sont initialement présentes en quantité limitée dans la poudre support S produite. En toute hypothèse, ces particules fines sont gênantes car elles risquent de produire un effet irritant. Grâce à l'enveloppe de liquide Ln à la surface des particules du support S « chargé » (c'est-à-dire ayant absorbé et adsorbé le liquide Ln), ces particules fines s'agglomèrent à d'autres particules du support S, notamment à des particules de support de taille supérieure ou égale à 200 μηπ, de sorte à former des particules composites, ou agglomérats, de taille supérieure ou égale à 200 m. Ainsi, les particules fines sont retenues, piégées par les enveloppes liquides des particules du support S. Ces enveloppes liquides jouent le rôle de phase liante. The relative proportions of carrier powder S and liquid L n (in other words the liquid / carrier ratio) in the mixture produced are adapted so that that the liquid L n penetrates by absorption inside the solid particles of the carrier powder and forms by adsorption an outer envelope on the surface of said particles. This liquid envelope acts as a link interface between particles. Thus, composite particles can be formed by agglomeration of smaller size particles bonded together by their outer liquid envelopes which play a role of binding phase or binding interface. More specifically, the relative proportions of liquid and solid carrier powder in the mixture are adapted so as to obtain an end product (that is to say at the end of the mixture of the carrier powder S and the liquid L n ). which is in the form of a free flow powder and without caking. This final product contains agglomerates of particles, the percentage of agglomerates having a size of less than or equal to 2 mm reaching at least 90%, advantageously 95%, advantageously still 99%. Thus, during the mixing of step E3, the particles of the support S absorb the liquid L n and, the liquid L n being added to the support in slight excess, the support S becomes slightly oversaturated. This results in the formation of an envelope (or "layer", or "film") of liquid L n at the surface of the support particles S. This liquid L n at the surface of the support particles S makes it possible, in particular, to retain particles "Fines" potentially present in the support S. By definition, the "fine particles" are particles less than or equal to 100 m in size. They are likely to form by abrasion and / or fraction of the larger particles of the support S, during the handling and transport of the support in powder form, or are initially present in a limited amount in the carrier powder S produced. In any case, these fine particles are troublesome because they may produce an irritating effect. Thanks to the liquid envelope L n at the surface of the particles of the support S "charged" (that is to say having absorbed and adsorbed the liquid L n ), these fine particles agglomerate with other particles of the support S, in particular to support particles of size greater than or equal to 200 μηπ, so as to form composite particles, or agglomerates, of size greater than or equal to 200 m. Thus, the fine particles are retained, trapped by the liquid envelopes particles of the support S. These liquid envelopes play the role of binder phase.
Pour chaque support S et pour chaque liquide Ln, il convient de déterminer, lors d'une étape préalable E0, une plage de ratios support S / liquide Ln, autrement dit de proportions respectives de support S et de liquide Ln, qui convient pour réaliser le mélange à l'étape E3 afin d'obtenir un produit final sous la forme d'une poudre qui est libre d'écoulement et sans mottage. Plus précisément, le produit final doit être sous la forme d'une poudre qui contient des agglomérats de particules, ou particules composites, la totalité des agglomérats ayant une taille inférieure ou égale à 2 mm. For each support S and for each liquid L n , it is necessary to determine, during a prior step E0, a range of support ratios S / liquid L n , in other words, respective proportions of support S and liquid L n , which is suitable for mixing in step E3 in order to obtain a final product in the form of a powder which is free from flow and without caking. More precisely, the final product must be in the form of a powder which contains agglomerates of particles, or composite particles, all the agglomerates having a size of less than or equal to 2 mm.
Sur la figure 3, on a représenté une poudre support « non chargée », avant d'être mélangée à un liquide Ln. A titre d'exemple illustratif, l'étape E0 a été réalisée pour un support S constitué par du Diamol Dl 20KF© et pour un liquide de référence (par exemple de l'eau), noté L0 In Figure 3, there is shown a carrier powder "not loaded", before being mixed with a liquid L n . By way of illustrative example, the step E0 was carried out for a support S consisting of Diamol Dl 20KF © and for a reference liquid (for example water), denoted L 0
Sur la figure 4A, on a représenté le produit final obtenu en mélangeant 65% en poids de la poudre support S et de 35% en poids du liquide de référence L0. Le produit final est « non saturé ». Il se présente sous la forme d'une poudre de particules ayant absorbé la totalité du liquide L0 Les particules obtenues à l'issue de l'étape de mélange E3 ne sont pas recouvertes d'une enveloppe de liquide L0. La poudre est libre d'écoulement. Sur la figure 4B, on a représenté la trace laissée par la poudre obtenue qui a été déposée puis retirée du fond dans une coupelle en verre. On voit que le produit laisse très peu de trace. Cela indique que la quantité de liquide en surface n'est pas suffisante pour former une surface de liaison. L'absence ou la trop faible surface de liaison formée ne permet donc pas de fixer les particules fines. Par conséquent le produit est donc potentiellement irritant. La proportion de liquide L0 dans le mélange réalisé est donc insuffisante. Sur la figure 5A, on a représenté le produit final obtenu en mélangeant 62% en poids de la poudre support S et de 38% en poids du liquide de référence L0 Le produit final est légèrement « sursaturé ». Il se présente sous la forme d'une poudre de particules ayant absorbé la totalité du liquide L0 et recouvertes d'une enveloppe de liquide L0. La poudre est libre d'écoulement. Sur la figure 5B, on a représenté la trace laissée par la poudre obtenue qui a été déposée dans une coupelle en verre puis retirée. On voit que le produit laisse une trace légèrement plus importante que sur la figure 4B, mais cela reste malgré tout limité. Le produit final obtenu dispose donc d'une couche de liquide apte à former une surface de liaison permettant à une partie du produit d'adhérer aux parois du récipient. Cette surface de liaison est apte à se lier aux particules fines présentes dans le produit, ce qui limite par conséquent les risques d'irritation. La proportion de liquide L0 dans le mélange réalisé est suffisante pour retenir les particules fines et n'est pas excessive de sorte que le produit reste libre d'écoulement et sans mottage. Le produit obtenu contient des agglomérats de particules de taille inférieure à 2 mm, de sorte que cela n'altère pas l'écoulement du produit. FIG. 4A shows the final product obtained by mixing 65% by weight of the support powder S and 35% by weight of the reference liquid L 0 . The final product is "unsaturated". It is in the form of a powder of particles having absorbed all the liquid L 0 The particles obtained at the end of the mixing step E3 are not covered with a liquid envelope L 0 . The powder is free from flow. In FIG. 4B, the trace left by the resulting powder which has been deposited and then removed from the bottom in a glass cup is shown. We see that the product leaves very little trace. This indicates that the amount of liquid on the surface is not sufficient to form a bonding surface. The absence or the too small bonding surface formed does not therefore make it possible to fix the fine particles. Therefore the product is potentially irritating. The proportion of liquid L 0 in the mixture produced is therefore insufficient. FIG. 5A shows the final product obtained by mixing 62% by weight of the carrier powder S and 38% by weight of the reference liquid L 0. The final product is slightly "oversaturated". It is in the form of a particle powder having absorbed all the liquid L 0 and covered with a liquid envelope L 0 . The powder is free from flow. In Figure 5B, there is shown the trace left by the resulting powder which was deposited in a glass cup and removed. We see that the product leaves a slightly larger trace than in Figure 4B, but this is still limited. The final product obtained thus has a layer of liquid capable of forming a connecting surface allowing part of the product to adhere to the walls of the container. This bonding surface is able to bind to the fine particles present in the product, which therefore limits the risk of irritation. The proportion of liquid L 0 in the mixture produced is sufficient to retain the fine particles and is not excessive so that the product remains free from flow and without caking. The product obtained contains agglomerates of particles smaller than 2 mm, so that this does not alter the flow of the product.
Sur la figure 6A, on a représenté le produit final obtenu en mélangeant 57% en poids de la poudre support S et de 43% en poids du liquide de référence L0 Le produit final est nettement « sursaturé ». Il est mottant et non libre d'écoulement. Sur la figure 6B, on a représenté la trace laissée par la poudre obtenue qui a été déposée dans une coupelle en verre puis retirée. On voit que le produit laisse une trace importante dans la coupelle (le fond de la coupelle reste couvert quasi-intégralement de produit). La proportion de liquide L0 dans le mélange réalisé est dans ce cas excessive. Le produit obtenu contient des agglomérats de particules de taille supérieure à 2 mm qui indiquent un début de mottage et ont pour effet de réduire fortement les propriétés d'écoulement du produit. Les trois tests réalisés permettent de conclure que la proportion de liquideFIG. 6A shows the final product obtained by mixing 57% by weight of the carrier powder S and 43% by weight of the reference liquid L 0. The final product is clearly "oversaturated". It is mottant and not free of flow. Figure 6B shows the trace left by the resulting powder which has been deposited in a glass cup and removed. We see that the product leaves an important trace in the cup (the bottom of the cup remains covered almost entirely product). The proportion of liquid L 0 in the mixture produced is in this case excessive. The product obtained contains agglomerates of particles greater than 2 mm in size which indicate the start of caking and have the effect of greatly reducing the flow properties of the product. The three tests carried out make it possible to conclude that the proportion of liquid
L0 dans le mélange support-liquide doit être supérieure à 35% et inférieure à 43%. Une teneur égale, ou sensiblement égale, à 38% en poids, permet d'obtenir un produit final qui est sous forme de poudre libre d'écoulement, non mottant et non irritant. L 0 in the carrier-liquid mixture must be greater than 35% and less than 43%. A content equal to, or substantially equal to, 38% by weight, makes it possible to obtain a final product which is in the form of a free flow, non-caking and non-irritating powder.
L'invention concerne aussi un additif alimentaire animal sous forme d'une poudre de particules contenant une substance classée dans l'une des trois catégories respectivement identifiées par les codes Xi, Xn et C. La poudre comprend au moins 90% de particules sans matière grasse, de taille supérieure ou égale à 200 m. Elle est avantageusement obtenue par la mise en œuvre du procédé de fabrication précédemment décrit. Les particules sont avantageusement sans enrobage. The invention also relates to an animal feed additive in the form of a particle powder containing a substance classified in one of the three categories respectively identified by the codes Xi, Xn and C. The powder comprises at least 90% of particles without material. fat, greater than or equal to 200 m. It is advantageously obtained by implementing the manufacturing method described above. The particles are advantageously without coating.
Dans une première forme de réalisation, toutes les particules de taille supérieure ou égale à 200 m ont une structure d'agglomérat de particules de taille inférieure (c'est-à-dire inférieure à 200 m). Ces particules peuvent avoir une structure de type framboise, ou une structure en couches d'oignon ou bien une structure intermédiaire entre ces deux structures. In a first embodiment, all particles larger than or equal to 200 m have a particle agglomerate structure of smaller size (i.e., less than 200 m). These particles may have a raspberry type structure, or an onion layer structure or an intermediate structure between these two structures.
Dans une deuxième forme de réalisation, les particules ayant une structure d'agglomérat, ou de particules composites, comportent une particule en un matériau support et un liquide incorporé dans la particule en matériau support et formant une enveloppe à la surface du matériau support. Cette enveloppe à la surface du matériau support permet à la particule de se lier aux particules fines contenues dans le produit. Cette première forme de réalisation est obtenue par le mode de réalisation décrit en référence à la figure 1 . In a second embodiment, the particles having an agglomerate structure, or composite particles, comprise a particle of a support material and a liquid incorporated in the support material particle and forming an envelope on the surface of the support material. This envelope on the surface of the support material allows the particle to bind to the fine particles contained in the product. This first embodiment is obtained by the embodiment described with reference to FIG.

Claims

REVENDICATIONS
1 . Procédé de fabrication d'un additif destiné à l'alimentation animale sous forme d'une poudre de particules contenant au moins une première substance classée dans l'une des trois catégories respectivement identifiées par les codes Xi, Xn et C, caractérisé en ce qu'il comprend une opération de production de ladite poudre par atomisation à chaud d'une solution contenant ladite première substance, la poudre produite contenant au moins 90% de particules de taille supérieure ou égale à 200 m. 1. Process for producing an animal feed additive in the form of a particle powder containing at least a first substance classified in one of the three categories respectively identified by the codes Xi, Xn and C, characterized in that it comprises an operation for producing said powder by hot atomization of a solution containing said first substance, the produced powder containing at least 90% of particles of size greater than or equal to 200 m.
2. Procédé selon la revendication 1 , caractérisé en ce que la poudre est produite par atomisation en lit d'air fluidisé. 2. Method according to claim 1, characterized in that the powder is produced by atomization in a fluidized air bed.
3. Procédé selon l'une des revendications précédentes, caractérisé en ce que la solution contenant la première substance est dépourvue de matière grasse. 3. Method according to one of the preceding claims, characterized in that the solution containing the first substance is free of fat.
4. Procédé selon l'une des revendications précédentes, caractérisé en ce que la solution contenant la première substance est une solution aqueuse. 4. Method according to one of the preceding claims, characterized in that the solution containing the first substance is an aqueous solution.
5. Procédé selon l'une des revendications précédentes, caractérisé en ce que les particules produites sont sans enrobage. 5. Method according to one of the preceding claims, characterized in that the particles produced are uncoated.
6. Procédé selon l'une des revendications précédentes, caractérisé en ce qu'il comprend une étape de réglage d'au moins un paramètre opératoire destiné à contrôler la taille des particules solides du produit final obtenu, la taille souhaitée des particules étant supérieure ou égale à 200 m. 6. Method according to one of the preceding claims, characterized in that it comprises a step of adjusting at least one operating parameter for controlling the size of the solid particles of the final product obtained, the desired size of the particles being greater or equal to 200 m.
7. Procédé selon l'une des revendications précédentes, caractérisé en ce que la solution contient au moins une substance aromatique et/ou gustative. 7. Method according to one of the preceding claims, characterized in that the solution contains at least one aromatic substance and / or taste.
8. Procédé selon l'une des revendications précédentes, caractérisé en ce que la solution contient un édulcorant. 8. Method according to one of the preceding claims, characterized in that the solution contains a sweetener.
9. Procédé selon l'une des revendications précédentes, caractérisé en ce que la solution contient un émulsifiant. 9. Method according to one of the preceding claims, characterized in that the solution contains an emulsifier.
10. Procédé selon l'une des revendications précédentes, caractérisé en ce que la solution contient : 10. Method according to one of the preceding claims, characterized in that the solution contains:
• entre 0,1 % et 100% en poids de ladite première substance ; Between 0.1% and 100% by weight of said first substance;
• entre 0% et 99,9% en poids d'un édulcorant ; Between 0% and 99.9% by weight of a sweetener;
• entre 0% et 99,9% en poids d'un émulsifiant et/ou d'un solvant.  Between 0% and 99.9% by weight of an emulsifier and / or a solvent.
1 1 . Procédé selon l'une des revendications précédentes, caractérisé en ce que la première substance est l'oléorésine de capsicum. 1 1. Process according to one of the preceding claims, characterized in that the first substance is oleoresin capsicum.
12. Procédé selon l'une des revendications précédentes, caractérisé en ce que l'additif contient entre 0,1 % et 99% en poids de ladite première substance. 12. Method according to one of the preceding claims, characterized in that the additive contains between 0.1% and 99% by weight of said first substance.
13. Additif destiné à l'alimentation animale sous forme d'une poudre de particules contenant une première substance classée dans l'une des trois catégories respectivement identifiées par les codes Xi, Xn et C, caractérisé en ce que ladite poudre comprend au moins 90% de particules de taille supérieure ou égale à 200 μηπ, sans matière grasse, présentant une structure de type framboise ou une structure en couches d'oignon ou une structure intermédiaire entre une structure de type framboise et une structure en couches d'oignon. 13. Additive for animal feed in the form of a powder of particles containing a first substance classified in one of the three categories respectively identified by the codes Xi, Xn and C, characterized in that said powder comprises at least 90 % of particles greater than or equal to 200 μηπ, without fat, having a raspberry-like structure or an onion-layer structure or an intermediate structure between a raspberry-like structure and an onion-layer structure.
14. Additif selon la revendication précédente, caractérisé en ce que les particules sont sans enrobage. 14. Additive according to the preceding claim, characterized in that the particles are uncoated.
15. Additif selon la revendication 13 ou 14, caractérisé en ce qu'il est obtenu par la mise en œuvre du procédé selon l'une des revendications 1 à 12. 15. Additive according to claim 13 or 14, characterized in that it is obtained by the implementation of the method according to one of claims 1 to 12.
PCT/EP2016/058307 2015-04-16 2016-04-15 Method for producing an additive for animal feed and corresponding additive WO2016166264A1 (en)

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