EP3946709A1 - Methods for producing powder by spray drying - Google Patents

Methods for producing powder by spray drying

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Publication number
EP3946709A1
EP3946709A1 EP20712997.4A EP20712997A EP3946709A1 EP 3946709 A1 EP3946709 A1 EP 3946709A1 EP 20712997 A EP20712997 A EP 20712997A EP 3946709 A1 EP3946709 A1 EP 3946709A1
Authority
EP
European Patent Office
Prior art keywords
liquid
composition
tank
gas
nitrogen
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP20712997.4A
Other languages
German (de)
French (fr)
Inventor
Dominique Ibarra
Carlos Aviles
Mohammed Youbi-Idrissi
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Air Liquide SA, LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical Air Liquide SA
Publication of EP3946709A1 publication Critical patent/EP3946709A1/en
Pending legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
    • B01J2/04—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a gaseous medium
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C1/00—Concentration, evaporation or drying
    • A23C1/04—Concentration, evaporation or drying by spraying into a gas stream

Definitions

  • the present invention relates to the field of powders used in the formulation of food and / or cosmetic products and relates in particular to the problem of preservation of these powders.
  • Such powders can for example be produced from “oil in water” or “water in oil” or “water in oil in water” emulsions.
  • the oily fraction may contain compounds of interest sensitive to oxidation, such as, for example, vitamin E. It is therefore essential to avoid any contact with oxygen.
  • US-4,180,593 which describes a process for manufacturing beads by drying a liquid containing a product capable of forming an edible film. Drying is carried out with a gas which may be present in the formulation of the liquid before the drying step. The gas is added with the aim of causing expansion during drying, in order to ensure good flowability and a controlled bulk density.
  • US Pat. No. 4,368,100 which proposes the atomization of an aqueous soluble coffee extract with a liquid flow rate undergoing controlled fluctuations and an upstream injection of an inert gas at constant pressure.
  • the liquid / gas mixture feeds a nozzle atomization in a drying tower.
  • the purpose of the flow fluctuations is to produce droplets of different sizes during atomization to promote the creation of coffee agglomerates as the small droplets collide with the larger droplets inside the drying tower. .
  • US-5,882,717 which describes injecting a gas into a coffee extract to create a foam with a controlled bubble size.
  • the operating conditions of temperature and pressure are defined so as to incorporate and trap small gas bubbles in the powder during spray drying, in order to replace the empty spaces inside the powder particles with gas.
  • the invention is primarily aimed at drying emulsions which foam, in general, although the invention can also be applied to other liquid matrices which do not foam.
  • the final objective of the injection of the gas is to modulate the properties of the powder particles produced, but no provision is proposed to allow the gas to be removed from the liquid and therefore to allow that oxygen can escape from the liquid.
  • the product is therefore always in the presence of trapped oxygen and available to oxidize the compounds of interest.
  • One of the objectives of the present invention is therefore to provide a process for the production of powders free from oxygen trapped in the particles.
  • FIG. 1 According to one of the embodiments of the invention (which will be detailed later in connection with appended FIG. 1), the production of powders from a liquid produced from a mixture of various ingredients (liquid and / or solid) in water and the injection of a neutral gas (7) (such as nitrogen or argon for example) into the water of the mixture , upstream, in the tank (1), so as to deoxygenate the water.
  • a neutral gas (7) such as nitrogen or argon for example
  • the injection into the tank is then stopped and replaced by a continuous inerting of the tank during all or part of the phase of adding solid ingredients (6) (powder for example) and mixing of the ingredients.
  • An oxygen sensor (5) can be placed in the tank and the dissolved oxygen level compared to a set point (0.5 ppm for example).
  • a homogenization step may be necessary before drying / atomization. It is preferable to ensure inerting of the surface of the liquid by continuous sweeping in order to avoid any uptake of oxygen.
  • the liquid is ready to be sent to the drying / atomization step (2).
  • the neutral gas can then be optionally injected (20) into the drying tower itself in order to intercept the drying zone.
  • the nozzle (3) used uses a compressed gas, which is usually air, it is preferable to replace this air with an inert gas (8), for example nitrogen.
  • the flow of inert gas and its pressure are adjusted so that the entire zone of the development of the jet and of the formation of powder particles is inert.
  • an oxygen probe can be placed in said zone, for example in the top of the drying tower or in the cone of the atomization jet, and slaved to the injection of inert gas to control the inerting of the said area.
  • the water is deoxygenated upstream, then the ingredients intended to make the desired mixture (composition) are added, the tank is preferably continuously inerted during this mixing, l
  • the mixing operation allows the whole to be degassed, the mixture is then directed to the drying tower, and if the atomization nozzle used uses air then it is advantageously preferred to replace the air with an inert gas such as nitrogen.
  • examples of products treated here include powdered fruit juice made from concentrate mixed in water and in which maltodextrin is also added as a support material.
  • FIG. 2 According to another of the embodiments of the invention (which will be detailed below in conjunction with FIG. 2 appended), the case of liquid products resulting from a mixture or else naturally complex is addressed. , but which do not foam.
  • the liquid then leaves the buffer tank (11) to feed the drying / atomization tower (2).
  • Neutral gas can then be optionally injected into the drying tower itself (20) in order to intercept the drying zone.
  • the nozzle (3) used uses a compressed gas, which is usually air, it is preferable to replace this air with an inert gas (8), for example nitrogen.
  • the flow of inert gas and its pressure are adjusted so that the entire zone of the development of the jet and of the formation of powder particles is inert.
  • an oxygen probe can be placed in said zone and slaved to the injection of inert gas to control the inerting of said zone.
  • Examples of products treated here include liquids containing a molecule of pharmaceutical interest to which a lactose-type carrier material is added.
  • the invention therefore relates to a process for manufacturing solid particles, from a liquid or semi-liquid composition, using a drying tower provided with an atomization nozzle into which the composition is injected as well as a drying tower.
  • compressed gas according to which one proceeds according to one of the following two variants:
  • An inert gas such as nitrogen or argon is injected into the water entering into the constitution of said composition, into an upstream tank;
  • One proceeds, in the water of the tank, to a phase of addition of the ingredients entering into the constitution of said required composition, and to the mixture of the whole, and one injects a neutral gas such as nitrogen or argon in the tank during all or part of the phase of adding and mixing the ingredients, the injection preferably being made into the head space of the tank;
  • a neutral gas such as nitrogen or argon
  • An inert gas such as nitrogen or argon is injected into the buffer tank, the injection being preferably made into the head space of the tank or into the liquid phase;
  • the nozzle 3 in both cases can be of different types, and in particular: A dual-fluid nozzle: the compressed air and the liquid (supplied by a pump) arrive by two different routes and mix at the nozzle outlet, at the orifice.
  • the role of compressed air is to break the flow of liquid into fine droplets.
  • a mono-fluid nozzle compressed air is injected into the liquid upstream of the nozzle.
  • the role of compressed air is twofold: to create the pressure necessary to force the liquid to pass through the orifice, and to break the flow of liquid into fine droplets.
  • a pressure nozzle the liquid is supplied by a pump at a pressure high enough to force its passage through the orifice and break the flow into fine droplets.
  • centrifugal nozzle the compressed air and the liquid (supplied by a pump) arrive by two different routes and mix at the nozzle outlet.
  • the role of compressed air is twofold: to rotate the nozzle at a speed high enough to eject the liquid through the multiple ports and break the flow of liquid into fine droplets by shearing.
  • the compressed air is preferably replaced by an inert compressed gas of nitrogen or argon type.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Medicinal Preparation (AREA)
  • Glanulating (AREA)
  • Formation And Processing Of Food Products (AREA)
  • Freezing, Cooling And Drying Of Foods (AREA)
  • General Preparation And Processing Of Foods (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Storage Of Fruits Or Vegetables (AREA)

Abstract

A method for producing solid particles, from a liquid or semi-liquid composition, using a drying tower (2) provided with a spray nozzle (3) into which the composition and a compressed gas are injected, in which method a neutral gas such as nitrogen or argon is injected (7) into the water which forms part of the composition, in an upstream tank (1), the composition alternatively being stored in line in an upstream tank (10) in a line connecting the upstream tank to a buffer tank (11).

Description

Procédés de production de poudre par séchage par atomisation Spray drying powder production processes
La présente invention concerne le domaine des poudres utilisées dans la formulation de produits alimentaires et/ou cosmétiques et concerne notamment la problématique de conservation de ces poudres. The present invention relates to the field of powders used in the formulation of food and / or cosmetic products and relates in particular to the problem of preservation of these powders.
De telles poudres peuvent par exemple être produites à partir d’émulsions « huile dans eau » ou « eau dans huile » ou « eau dans huile dans eau ». La fraction huileuse peut contenir des composés d’intérêt sensibles à l’oxydation, tels que par exemple la vitamine E. Il est alors indispensable d’éviter tout contact avec l’oxygène. Such powders can for example be produced from "oil in water" or "water in oil" or "water in oil in water" emulsions. The oily fraction may contain compounds of interest sensitive to oxidation, such as, for example, vitamin E. It is therefore essential to avoid any contact with oxygen.
Dans l’art antérieur, on peut citer de nombreux documents décrivant l’injection de gaz dans un liquide à sécher par atomisation, et notamment les documents suivants : In the prior art, one can cite numerous documents describing the injection of gas into a liquid to be dried by spray drying, and in particular the following documents:
US-1 406 381 qui décrit un procédé où un gaz (sous pression ou non), stérile non-oxydant (le C02 est préféré selon ce document car très soluble dans le produit, est dissous dans du lait liquide. Le lait chargé en gaz est ensuite atomisé dans une cuve d’évaporation. Le produit résultant est du lait en poudre imprégné avec le même gaz. US Pat. No. 1,406,381 which describes a process in which a sterile non-oxidizing gas (pressurized or not) (CO2 is preferred according to this document because it is very soluble in the product, is dissolved in liquid milk. The gas laden with gas is then atomized in an evaporation tank The resulting product is powdered milk impregnated with the same gas.
US-3 222 193 qui propose la dispersion d’un gaz inerte relativement insoluble dans un liquide (lait, petit-lait, jus de fruit, jus de tomate, jus d’orange, ou encore jus de pamplemousse) précédemment pasteurisé et concentré (40- 50 % solides) avant séchage par atomisation, afin d’obtenir une bonne « coulabilité ». US-3,222,193 which proposes the dispersion of an inert gas relatively insoluble in a liquid (milk, whey, fruit juice, tomato juice, orange juice, or grapefruit juice) previously pasteurized and concentrated ( 40-50% solids) before spray drying, in order to obtain good “flowability”.
US-4 180 593 qui décrit un procédé de fabrication de billes par séchage d’un liquide contenant un produit capable de former un film comestible. Le séchage est réalisé avec un gaz qui peut être présent dans la formulation du liquide avant l’étape de séchage. Le gaz est ajouté avec le but de provoquer une expansion lors du séchage, afin d’assurer une bonne coulabilité et une masse volumique apparente contrôlée. US-4,180,593 which describes a process for manufacturing beads by drying a liquid containing a product capable of forming an edible film. Drying is carried out with a gas which may be present in the formulation of the liquid before the drying step. The gas is added with the aim of causing expansion during drying, in order to ensure good flowability and a controlled bulk density.
US-4 368 100 qui propose l’atomisation d’un extrait aqueux de café soluble avec un débit de liquide subissant des fluctuations contrôlées et une injection en amont d’un gaz inerte à pression constante. Le mélange liquide/gaz alimente une buse d’atomisation dans une tour de séchage. Les fluctuations de débit ont pour but de produire des gouttelettes de tailles différentes pendant l’atomisation afin de favoriser la création d’agglomérats de café lorsque les petites gouttelettes entrent en collision avec les gouttelettes de taille supérieure à l’intérieur de la tour de séchage. US Pat. No. 4,368,100 which proposes the atomization of an aqueous soluble coffee extract with a liquid flow rate undergoing controlled fluctuations and an upstream injection of an inert gas at constant pressure. The liquid / gas mixture feeds a nozzle atomization in a drying tower. The purpose of the flow fluctuations is to produce droplets of different sizes during atomization to promote the creation of coffee agglomerates as the small droplets collide with the larger droplets inside the drying tower. .
US-5 882 717 qui décrit l’injection d’un gaz dans un extrait de café afin de créer une mousse avec une taille contrôlée de bulle. Les conditions opératoires de température et pression sont définies de manière à incorporer et piéger des petites bulles de gaz dans la poudre lors du séchage par atomisation, afin de remplacer les espaces vides à l’intérieur des particules de poudre avec du gaz. US-5,882,717 which describes injecting a gas into a coffee extract to create a foam with a controlled bubble size. The operating conditions of temperature and pressure are defined so as to incorporate and trap small gas bubbles in the powder during spray drying, in order to replace the empty spaces inside the powder particles with gas.
Tous ces documents proposent donc l’injection d’un gaz directement dans un liquide. Ce type de solution ne convient pas dès lors pour les applications où les émulsions précitées sont, de par leur composition, des liquides moussants. All these documents therefore propose the injection of a gas directly into a liquid. This type of solution is therefore not suitable for applications where the aforementioned emulsions are, by their composition, foaming liquids.
Et on notera ici que l’invention vise prioritairement le séchage d’émulsions qui moussent, en général, même si l’invention peut aussi s’appliquer à d’autres matrices liquides qui ne moussent pas. And it will be noted here that the invention is primarily aimed at drying emulsions which foam, in general, although the invention can also be applied to other liquid matrices which do not foam.
En fait dans tous les documents précités, l’objectif final de l’injection du gaz est de moduler les propriétés des particules de poudre produites, mais aucune disposition n’est proposée pour permettre d’éliminer le gaz du liquide et donc pour permettre que l’oxygène puisse s’échapper du liquide. Le produit est donc toujours en présence d’oxygène piégé et disponible pour oxyder les composés d’intérêt. In fact in all the aforementioned documents, the final objective of the injection of the gas is to modulate the properties of the powder particles produced, but no provision is proposed to allow the gas to be removed from the liquid and therefore to allow that oxygen can escape from the liquid. The product is therefore always in the presence of trapped oxygen and available to oxidize the compounds of interest.
Dans ce domaine de l’art antérieur on peut également citer tous les travaux effectués par la société MESSER, qui a expérimenté de nombreuses situations, avec l’utilisation de N2 ou CO2, gazeux, liquide, ou encore supercritique, avec généralement la mise en contact du gaz ou cryogène liquide et du produit au niveau de la buse d’atomisation (on pourra consulter les documents DE-10233864, US-6 284 302, EP-1 027 144, EP- 1 677 903...). L’un des travaux propose la charge préalable du produit avec du CO2 gazeux avant l’envoi vers l’atomisation. On notera néanmoins que le CO2 est soluble dans l’eau, il ne désorbe donc pas et donc ne peut pas entraîner l’oxygène hors du liquide. In this field of the prior art, mention may also be made of all the work carried out by the company MESSER, which has experimented with numerous situations, with the use of N2 or CO2, gaseous, liquid, or even supercritical, generally with the setting in contact of the gas or liquid cryogen and of the product at the level of the atomization nozzle (documents DE-10233864, US-6 284 302, EP-1 027 144, EP-1 677 903, etc. may be consulted). One of the works proposes the preliminary charge of the product with gaseous CO2 before sending it to atomization. Note, however, that CO2 is soluble in water, it therefore does not desorb and therefore cannot carry oxygen out of the liquid.
On peut également citer le document US2010/215818 (Nestec) : l'objectif de ce document est de sur-saturer le liquide en gaz, par exemple en azote , pour avoir une poudre très "foisonnée" (contenant beaucoup de gaz), pour cela ils soumettent le liquide à une pression très élevée, typiquement de 50 à 400 bars, le liquide arrive donc dans la tour de séchage avec beaucoup d'azote dissous. We can also cite document US2010 / 215818 (Nestec): the objective of this document is to over-saturate the liquid with gas, for example with nitrogen, to have a very "expanded" powder (containing a lot of gas), for that they subject the liquid to a very high pressure, typically 50 to 400 bars, the liquid therefore arrives in the drying tower with a lot of dissolved nitrogen.
Comme on le verra ci-dessous ce n’est pas du tout l’approche suivie par la présente invention dont l’objectif n’est pas de saturer le liquide en gaz, mais d'enlever l'oxygène, en travaillant à pression atmosphérique et en s’attachant à procéder à une étape de séparation gaz/liquide avant l'arrivée dans la tour de séchage, de manière à ce que l'azote injecté, chargé en oxygène, puisse sortir du liquide. As will be seen below, this is not at all the approach followed by the present invention, the objective of which is not to saturate the liquid with gas, but to remove the oxygen, working at atmospheric pressure. and by focusing on carrying out a gas / liquid separation step before entering the drying tower, so that the injected nitrogen, loaded with oxygen, can exit the liquid.
Un des objectifs de la présente invention est alors de proposer un procédé de production de poudres exemptes d’oxygène piégé dans les particules. One of the objectives of the present invention is therefore to provide a process for the production of powders free from oxygen trapped in the particles.
Comme on le verra plus en détails dans ce qui suit, la solution technique proposée selon la présente invention permet l’obtention des résultats suivants : As will be seen in more detail in what follows, the technical solution proposed according to the present invention enables the following results to be obtained:
- le procédé produit des poudres dont les particules ne contiennent pas de gaz dissous, et donc pas d’oxygène piégé au sein de la particule. Ainsi, l’oxydation des molécules sensibles est réduite ou évitée. - the process produces powders whose particles do not contain dissolved gas, and therefore no oxygen trapped within the particle. Thus, oxidation of sensitive molecules is reduced or avoided.
- puisque le liquide alimentant la buse d’atomisation ne contient pas de gaz dissous, le moussage est évité lors du séchage. - since the liquid supplied to the atomization nozzle does not contain dissolved gas, foaming is avoided during drying.
- on peut dès lors traiter - we can therefore treat
i. des produits issus de mélanges dans lesquels un solide (poudre par exemple) doit être dissous dans un ou plusieurs liquides (émulsion eau/huile par exemple ou i. products derived from mixtures in which a solid (powder for example) must be dissolved in one or more liquids (water / oil emulsion for example or
ii. des liquides complexes (jus, lait... etc... ) ; il faut noter que pour sécher un liquide alimentaire l’ajout d’un matériau de support (maltodextrine, gomme d’acacia... ) est souvent indispensable. Le mélange résultant est dans la plupart des cas moussant. [Fig. 1] annexée : Selon un des modes de mise en oeuvre de l’invention (que l’on détaillera plus loin en liaison avec la figure 1 annexée), on adresse la production de poudres à partir d’un liquide élaboré issu d’un mélange de divers ingrédients (liquides et/ou solides) dans de l’eau et l’on effectue l’injection d’un gaz neutre (7) (tel l’azote ou l’argon par exemple) dans l’eau du mélange, en amont, en cuve (1 ), de manière à désoxygéner l’eau. L’injection dans la cuve est ensuite arrêtée et remplacée par un inertage continu de la cuve pendant tout ou partie de la phase d’ajout d’ingrédients solides (6) (en poudre par exemple) et de mélange des ingrédients. Une sonde à oxygène (5) peut être placée dans la cuve et le niveau d’oxygène dissous comparé à une valeur de consigne (0.5 ppm par exemple). Dans certains cas, une étape d’homogénéisation peut être nécessaire avant le séchage/atomisation. Il est préférable d’assurer un inertage de la surface du liquide par balayage en continu afin d’éviter toute reprise en oxygène. Après l’étape de mélange et/ou homogénéisation, le liquide est prêt à être envoyé à l’étape de séchage/atomisation (2). ii. complex liquids (juice, milk ... etc ...); it should be noted that in order to dry a food liquid, the addition of a support material (maltodextrin, acacia gum, etc.) is often essential. The resulting mixture is in most cases foaming. [Fig. 1] appended: According to one of the embodiments of the invention (which will be detailed later in connection with appended FIG. 1), the production of powders from a liquid produced from a mixture of various ingredients (liquid and / or solid) in water and the injection of a neutral gas (7) (such as nitrogen or argon for example) into the water of the mixture , upstream, in the tank (1), so as to deoxygenate the water. The injection into the tank is then stopped and replaced by a continuous inerting of the tank during all or part of the phase of adding solid ingredients (6) (powder for example) and mixing of the ingredients. An oxygen sensor (5) can be placed in the tank and the dissolved oxygen level compared to a set point (0.5 ppm for example). In some cases, a homogenization step may be necessary before drying / atomization. It is preferable to ensure inerting of the surface of the liquid by continuous sweeping in order to avoid any uptake of oxygen. After the mixing and / or homogenization step, the liquid is ready to be sent to the drying / atomization step (2).
Le gaz neutre peut alors être optionnellement injecté (20) dans la tour de séchage elle- même afin d’inerter la zone de séchage. The neutral gas can then be optionally injected (20) into the drying tower itself in order to intercept the drying zone.
Il est préférable d’éviter toute reprise d’oxygène par le liquide avant sa transformation en poudre. Aussi dans le cas où la buse (3) utilisée met en oeuvre un gaz comprimé, qui est habituellement de l’air, il est préférable de remplacer cet air par un gaz inerte (8), par exemple de l’azote. It is preferable to avoid any absorption of oxygen by the liquid before it is transformed into powder. Also in the case where the nozzle (3) used uses a compressed gas, which is usually air, it is preferable to replace this air with an inert gas (8), for example nitrogen.
Avantageusement, le débit de gaz inerte et sa pression sont réglés de sorte que toute la zone du développement du jet et de la formation de particules de poudre est inerte. Avantageusement, une sonde d'oxygène peut être placée dans ladite zone, par exemple dans le haut de la tour de séchage ou dans le cône du jet d’atomisation, et asservie à l'injection de gaz inerte pour contrôler l’inertage de la dite zone. Advantageously, the flow of inert gas and its pressure are adjusted so that the entire zone of the development of the jet and of the formation of powder particles is inert. Advantageously, an oxygen probe can be placed in said zone, for example in the top of the drying tower or in the cone of the atomization jet, and slaved to the injection of inert gas to control the inerting of the said area.
Donc en résumé selon ce premier mode de mise en oeuvre, on désoxygène l’eau en amont, puis on ajoute les ingrédients destinés à faire le mélange (composition) voulu(e), on inerte préférentiellement en continu la cuve durant ce mélange, l’opération de mélange permet de dégazer l’ensemble, le mélange est alors dirigé vers la tour de séchage, et si la buse d’atomisation utilisée met en oeuvre de l’air alors on préfère avantageusement remplacer l’air par un gaz inerte tel l’azote. Parmi les exemples de produits traités ici on peut citer le jus de fruit en poudre fabriqué à partir de concentré mélangé dans de l’eau et dans lequel est aussi rajouté de la maltodextrine comme matériau de support. So in summary according to this first mode of implementation, the water is deoxygenated upstream, then the ingredients intended to make the desired mixture (composition) are added, the tank is preferably continuously inerted during this mixing, l The mixing operation allows the whole to be degassed, the mixture is then directed to the drying tower, and if the atomization nozzle used uses air then it is advantageously preferred to replace the air with an inert gas such as nitrogen. Examples of products treated here include powdered fruit juice made from concentrate mixed in water and in which maltodextrin is also added as a support material.
[Fig. 2] annexée : Selon un autre des modes de mise en oeuvre de l’invention (que l’on détaillera plus loin en liaison avec la figure 2 annexée), on adresse le cas de produits liquides résultants d’un mélange ou bien naturellement complexes, mais qui ne moussent pas. [Fig. 2] appended: According to another of the embodiments of the invention (which will be detailed below in conjunction with FIG. 2 appended), the case of liquid products resulting from a mixture or else naturally complex is addressed. , but which do not foam.
On propose ici une injection du gaz neutre (azote ou argon par exemple) non pas en amont en cuve mais ici en ligne dans le liquide (i.e le mélange à sécher), stocké dans la cuve 10, injection (7) suffisamment en amont d’une cuve tampon (11 ) inertée (12), où le liquide dans lequel le gaz a été injecté est envoyé, cuve tampon dans laquelle la séparation entre le liquide et le gaz neutre chargé en oxygène va se faire. Expression « suffisamment en amont » car il est important que l’injection soit faite suffisamment en amont de manière à ce que l’échange entre le gaz inerte et l’oxygène dissous ait le temps de se faire. La longueur de canalisation permet préférentiellement un temps de contact après l’injection qui est compris entre 5 et 30s. We propose here an injection of the neutral gas (nitrogen or argon for example) not upstream in the tank but here online in the liquid (ie the mixture to be dried), stored in the tank 10, injection (7) sufficiently upstream of 'an inerted buffer tank (11) (12), where the liquid into which the gas has been injected is sent, a buffer tank in which the separation between the liquid and the neutral gas loaded with oxygen will take place. Expression "sufficiently upstream" because it is important that the injection be made sufficiently upstream so that the exchange between inert gas and dissolved oxygen has time to take place. The length of the pipe preferably allows a contact time after the injection which is between 5 and 30s.
Le liquide quitte ensuite la cuve tampon (11 ) pour alimenter la tour de séchage/atomisation (2). The liquid then leaves the buffer tank (11) to feed the drying / atomization tower (2).
Le gaz neutre peut alors être optionnellement injecté dans la tour de séchage elle- même (20) afin d’inerter la zone de séchage. Neutral gas can then be optionally injected into the drying tower itself (20) in order to intercept the drying zone.
Il est préférable d’éviter toute reprise d’oxygène par le liquide avant sa transformation en poudre. Aussi dans le cas où la buse (3) utilisée met en oeuvre un gaz comprimé, qui est habituellement de l’air, il est préférable de remplacer cet air par un gaz inerte (8), par exemple de l’azote. It is preferable to avoid any absorption of oxygen by the liquid before it is transformed into powder. Also in the case where the nozzle (3) used uses a compressed gas, which is usually air, it is preferable to replace this air with an inert gas (8), for example nitrogen.
Avantageusement, le débit de gaz inerte et sa pression sont réglés de sorte que toute la zone du développement du jet et de la formation de particules de poudre est inerte. Avantageusement, une sonde d'oxygène peut être placée dans ladite zone et asservie à l'injection de gaz inerte pour contrôler l’inertage de la dite zone. Advantageously, the flow of inert gas and its pressure are adjusted so that the entire zone of the development of the jet and of the formation of powder particles is inert. Advantageously, an oxygen probe can be placed in said zone and slaved to the injection of inert gas to control the inerting of said zone.
Donc en résumé selon ce second mode de mise en oeuvre, on procède à l’injection du gaz en ligne directement dans le liquide complexe constitué (pas dans l’eau avant mélange), on envoie le liquide dans une cuve tampon inertée, où s’effectue le dégazage, puis on envoie ce liquide vers la tour de séchage/atomisation. So in summary according to this second mode of implementation, one proceeds to the injection of the gas in line directly into the complex liquid formed (not in the water before mixture), the liquid is sent to an inerted buffer tank, where degassing takes place, then this liquid is sent to the drying / atomization tower.
Parmi les exemples de produits traités ici on peut citer les liquides contenant une molécule d’intérêt pharmaceutique dans lequel on ajoute un matériau de support de type lactose. Examples of products treated here include liquids containing a molecule of pharmaceutical interest to which a lactose-type carrier material is added.
L’invention concerne alors un procédé de fabrication de particules solides, à partir d’une composition liquide ou semi-liquide, mettant en oeuvre une tour de séchage munie d’une buse d’atomisation dans laquelle est injectée la composition ainsi qu’un gaz comprimé, selon lequel on procède selon l’une des deux variantes suivantes : The invention therefore relates to a process for manufacturing solid particles, from a liquid or semi-liquid composition, using a drying tower provided with an atomization nozzle into which the composition is injected as well as a drying tower. compressed gas, according to which one proceeds according to one of the following two variants:
i. i.
- on effectue l’injection, dans l’eau entrant dans la constitution de la dite composition, d’un gaz neutre tel l’azote ou l’argon, dans une cuve amont ; - An inert gas such as nitrogen or argon is injected into the water entering into the constitution of said composition, into an upstream tank;
- on procède, dans l’eau de la cuve, à une phase d’ajout des ingrédients entrant dans la constitution de ladite composition requise, et au mélange de l’ensemble, et l’on injecte un gaz neutre tel l’azote ou l’argon dans la cuve pendant tout ou partie de la phase d’ajout et de mélange des ingrédients , l’injection étant préférentiellement faite dans l’espace de tête de la cuve ; - One proceeds, in the water of the tank, to a phase of addition of the ingredients entering into the constitution of said required composition, and to the mixture of the whole, and one injects a neutral gas such as nitrogen or argon in the tank during all or part of the phase of adding and mixing the ingredients, the injection preferably being made into the head space of the tank;
- on dirige la composition ainsi obtenue dans la tour de séchage. - The composition thus obtained is directed into the drying tower.
- on dispose de la dite composition dans une cuve amont ; - We have said composition in an upstream tank;
- on dispose d’une ligne reliant la cuve amont à une cuve tampon ou un autre système de séparation gaz/liquide, et l’on procède à une injection d’un gaz neutre tel l’azote ou l’argon en ligne, dans la composition circulant dans cette ligne entre les deux cuves ; - there is a line connecting the upstream tank to a buffer tank or another gas / liquid separation system, and an injection of a neutral gas such as nitrogen or argon is carried out in line, in the composition circulating in this line between the two tanks;
- on procède à l’injection d’un gaz neutre tel l’azote ou l’argon dans la cuve tampon, l’injection étant préférentiellement faite dans l’espace de tête de la cuve ou dans la phase liquide; - An inert gas such as nitrogen or argon is injected into the buffer tank, the injection being preferably made into the head space of the tank or into the liquid phase;
- on dirige la composition ainsi obtenue dans la tour de séchage. - The composition thus obtained is directed into the drying tower.
La buse 3 dans les deux cas peut être de différents types, et notamment : Une buse bi-fluide : l’air comprimé et le liquide (alimenté par une pompe) arrivent par deux voies différentes et se mélangent en sortie de buse, au niveau de l’orifice. Le rôle de l’air comprimé est de casser le flux de liquide en fines gouttelettes. The nozzle 3 in both cases can be of different types, and in particular: A dual-fluid nozzle: the compressed air and the liquid (supplied by a pump) arrive by two different routes and mix at the nozzle outlet, at the orifice. The role of compressed air is to break the flow of liquid into fine droplets.
Une buse mono-fluide : l’air comprimé est injecté dans le liquide en amont de la buse. Le rôle de l’air comprimé est double : créer la pression nécessaire pour forcer le passage du liquide au travers l’orifice, et casser le flux de liquide en fines gouttelettes. A mono-fluid nozzle: compressed air is injected into the liquid upstream of the nozzle. The role of compressed air is twofold: to create the pressure necessary to force the liquid to pass through the orifice, and to break the flow of liquid into fine droplets.
Une buse pression : le liquide est alimenté par une pompe à une pression suffisamment haute pour forcer son passage à travers l’orifice et casser le flux en fines gouttelettes. A pressure nozzle: the liquid is supplied by a pump at a pressure high enough to force its passage through the orifice and break the flow into fine droplets.
- Une buse centrifuge : l’air comprimé et le liquide (alimenté par une pompe) arrivent par deux voies différentes et se mélangent en sortie de buse. Le rôle de l’air comprimé est double : faire tourner la buse à une vitesse suffisamment haute pour éjecter le liquide par les multiples orifices et casser le flux de liquide en fines gouttelettes par cisaillement. - A centrifugal nozzle: the compressed air and the liquid (supplied by a pump) arrive by two different routes and mix at the nozzle outlet. The role of compressed air is twofold: to rotate the nozzle at a speed high enough to eject the liquid through the multiple ports and break the flow of liquid into fine droplets by shearing.
Dans la présente invention, l’air comprimé est préférentiellement remplacé par un gaz comprimé inerte de type azote ou argon. In the present invention, the compressed air is preferably replaced by an inert compressed gas of nitrogen or argon type.

Claims

REVENDICATIONS
1. Procédé de fabrication de particules solides, à partir d’une composition liquide ou semi-liquide, mettant en oeuvre une tour de séchage (2) munie d’une buse (3) d’atomisation dans laquelle est injectée la composition ainsi qu’un gaz comprimé, selon lequel on procède selon l’une des deux variantes suivantes : 1. A method of manufacturing solid particles, from a liquid or semi-liquid composition, using a drying tower (2) provided with an atomization nozzle (3) into which the composition is injected as well as a compressed gas, according to which one proceeds according to one of the following two variants:
i. i.
- on effectue l’injection (7), dans l’eau entrant dans la constitution de la dite composition, d’un gaz neutre tel l’azote ou l’argon, dans une cuve amont (1 ); - The injection (7), into the water entering into the constitution of said composition, of a neutral gas such as nitrogen or argon, into an upstream tank (1);
- on procède, dans l’eau de la cuve, à une phase (6) d’ajout des ingrédients entrant dans la constitution de ladite composition requise, et au mélange de l’ensemble, et l’on injecte un gaz neutre tel l’azote ou l’argon dans la cuve pendant tout ou partie de la phase d’ajout et de mélange des ingrédients , l’opération de mélange permettant de dégazer l’ensemble; - One proceeds, in the water of the tank, to a phase (6) of addition of the ingredients entering into the constitution of said required composition, and the mixture of the whole, and one injects a neutral gas such as nitrogen or argon in the tank during all or part of the phase of adding and mixing the ingredients, the mixing operation making it possible to degas the whole;
- on dirige la composition ainsi obtenue dans la tour de séchage. - The composition thus obtained is directed into the drying tower.
- on dispose de la dite composition dans une cuve amont 10) ; - The said composition is available in an upstream tank 10);
- on dispose d’une ligne reliant la cuve amont à une cuve tampon (11 ), et l’on procède à une injection (7) d’un gaz neutre tel l’azote ou l’argon en ligne, dans la composition circulant dans cette ligne entre les deux cuves ; - There is a line connecting the upstream tank to a buffer tank (11), and an injection (7) of a neutral gas such as nitrogen or argon in line, in the circulating composition is carried out in this line between the two tanks;
- on procède à l’injection (12) d’un gaz neutre tel l’azote ou l’argon dans la cuve tampon (11 ), cuve tampon dans laquelle la séparation entre le liquide et le gaz neutre chargé en oxygène, va pouvoir s’effectuer; - One proceeds to the injection (12) of a neutral gas such as nitrogen or argon in the buffer tank (11), buffer tank in which the separation between the liquid and the neutral gas loaded with oxygen, will be able to to perform;
- on dirige la composition ainsi obtenue dans la tour de séchage. - The composition thus obtained is directed into the drying tower.
EP20712997.4A 2019-04-05 2020-03-26 Methods for producing powder by spray drying Pending EP3946709A1 (en)

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FR1903657A FR3094649B1 (en) 2019-04-05 2019-04-05 Spray drying powder production processes
PCT/EP2020/058500 WO2020200994A1 (en) 2019-04-05 2020-03-26 Methods for producing powder by spray drying

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US1406381A (en) 1920-04-12 1922-02-14 Heath Wilfrid Paul Process of manufacturing powdered milk and other food products
US3072486A (en) * 1959-06-30 1963-01-08 Et Oakes Corp Preparation for soluble milk powder
US3222193A (en) 1962-09-12 1965-12-07 Francis P Hanrahan Method of spray drying liquid food products
US4180593A (en) 1977-04-29 1979-12-25 Cohan Allan N Process for producing round spherical free flowing blown bead food products of controlled bulk density
ES481924A1 (en) 1978-06-28 1980-09-01 Gen Foods Ltd Process for producing a spray-dried agglomerated soluble coffee product
US5092959A (en) * 1990-04-27 1992-03-03 Yamato Scientific Co., Ltd. Organic solvent spray dryer device
US5882717A (en) 1996-10-30 1999-03-16 Kraft Foods, Inc. Soluble espresso coffee
DE19748069A1 (en) 1997-10-31 1999-05-06 Messer Griesheim Gmbh Method and device for cooling and atomizing liquid or pasty substances
DE10233864A1 (en) 2002-01-03 2003-07-17 Messer Griesheim Gmbh Apparatus, useful for producing a powdered product in the food and pharmaceutical industries, comprises a relaxation device for an atomizer medium, feeders and a mixer
EP1677903B1 (en) 2003-10-30 2012-08-01 Merck Serono SA Process and apparatus for cooling and atomizing liquid or pasty-like substances
PT2194795E (en) * 2007-09-28 2015-03-04 Nestec Sa Instant drink powder

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AU2020254901A8 (en) 2021-12-09
AU2020254901A1 (en) 2021-11-04

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