WO2025113960A1 - Method for the cryo-crystallisation of oils and fats for applications in the agri-food, cosmetics or pharmacy fields - Google Patents
Method for the cryo-crystallisation of oils and fats for applications in the agri-food, cosmetics or pharmacy fields Download PDFInfo
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- WO2025113960A1 WO2025113960A1 PCT/EP2024/081751 EP2024081751W WO2025113960A1 WO 2025113960 A1 WO2025113960 A1 WO 2025113960A1 EP 2024081751 W EP2024081751 W EP 2024081751W WO 2025113960 A1 WO2025113960 A1 WO 2025113960A1
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS OR COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings or cooking oils
- A23D9/02—Other edible oils or fats, e.g. shortenings or cooking oils characterised by the production or working-up
- A23D9/04—Working-up
- A23D9/05—Forming free-flowing pieces
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0004—Crystallisation cooling by heat exchange
- B01D9/0009—Crystallisation cooling by heat exchange by direct heat exchange with added cooling fluid
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- 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
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0018—Evaporation of components of the mixture to be separated
- B01D9/0027—Evaporation of components of the mixture to be separated by means of conveying fluid, e.g. spray-crystallisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/005—Selection of auxiliary, e.g. for control of crystallisation nuclei, of crystal growth, of adherence to walls; Arrangements for introduction thereof
Definitions
- the present invention relates to the field of processes and equipment dedicated to the cryo-crystallization of oils and fats and waxes, or other liquid or semi-liquid greasy compounds, with a high melting point, for applications in the fields of agri-food, cosmetics or even pharmacy.
- State-of-the-art cryo-crystallization equipment is known to transform an oil, a grease, a wax or other greasy compound containing a certain proportion of active ingredient into a set of solid particles in the form of powder or beads.
- a cryo-crystallization process then classically consists of atomizing the molten product in a cooled enclosure using a cryogenic fluid, typically liquid nitrogen, which causes a sudden cooling of the particles falling freely in the enclosure, up to the point of crystallization.
- a cryogenic fluid typically liquid nitrogen
- the transformation is irreversible and the collected product remains in the crystallized state in the form of a powder or small beads depending on the spraying technology implemented in the device.
- Figure 1 illustrates by a partial schematic view the different parts of a typical state-of-the-art cryo-crystallization device.
- the first process ((a) - pneumatic injection) is undoubtedly considered less qualitative than the second ((b), injection called “electro-spray”) but allows significant productivity to be achieved, typically of the order of 1000 kg/h.
- the particle size distribution is wide with a non- negligible fine particles requiring careful filtration of the extracted gas flow, or even “ATEX” classification of the production facility.
- monodisperse beads also called monodisperse
- the formation of fine particles is then avoided by the preferred application of the second process, to the detriment of productivity. Indeed, as mentioned, the latter is limited to approximately 200 kg/h, with a growth potential limited to the maximum number of needles implantable in the injection head.
- productivity of the system is sensitive to the surface tension of the product.
- the present invention proposes to replace the electro-spray device conventionally installed until now in cryo-crystallization devices, with a more productive device for generating monodisperse beads, while maintaining a high level of quality of the transformed product.
- Figure 3 illustrates by a partial schematic view the operating principle of such wire cutting, the following elements can be seen in Figure 3:
- the typical range of ball diameters that can be achieved with this process is typically 0.2 mm to 3 mm, the quantity of balls generated per second depends on the rotation frequency of the cutting wire, generally 5000 to 10,000 Hz but can go up to 25,000 Hz.
- productivity can reach 1200 kg/h, a value 5 to 6 times higher than that achievable with electro-spray.
- the cutting device mentioned above is installed in the upper part of a cryo-crystallization apparatus, in particular between the reservoir containing the molten product and the cooling enclosure, or in the upper part of this enclosure.
- Figure 4 illustrates by a partial schematic view an example of implementation of the invention with such an installation of the cutting system within a cryo-crystallizer.
- the nozzle is fed at a constant flow rate from the pressurized liquid product reservoir, ensuring, by the constant speed rotation of the cutting wire 14, a very tight ball size distribution.
- the system can be equipped with one, two or more nozzles for producing a jet 12 of liquid to be treated (to be cut), preferably supplied with the same flow rate, a system of multiple nozzles thereby increasing the number of balls generated per unit of time. productivity thus obtained can be high even for a ball diameter of less than 3 mm.
- the refrigerating power provided by the use of a liquid cryogen such as liquid nitrogen allows the complete crystallization of the product over a reduced height, typically around 2 m on state-of-the-art devices, compared to prior art systems equipped with conventional vapor compression refrigeration circuits whose height can reach 5 to 10 meters.
- the present invention then relates to a method for manufacturing solid particles, from a liquid or semi-liquid composition, in particular from a composition of oil, a grease, a wax or another greasy compound, using at least one device for forming a liquid or semi-liquid jet of the product, for example such as from a nozzle or a syringe, then a step of total or partial freezing or crystallization of the jet thus formed, characterized by the implementation of the following measures: one or more streams of the composition are produced using the forming device(s), entering the upper part of a reaction chamber and circulating within this reaction chamber from top to bottom; the reaction chamber is supplied with cryogenic liquid, for example liquid nitrogen, to create a cold gas atmosphere within the reaction chamber; the particles formed are recovered in the lower part of the chamber; characterized in that an apparatus is used for cutting said product stream(s) using a wire or disc rotating at a given and chosen speed, the apparatus being positioned downstream of the outlet of said product stream(s) from said forming device(s), preferably positioned in the upper
- the present invention also relates to an installation for manufacturing solid particles, from a liquid or semi-liquid composition, in particular from a composition of oil, a grease, a wax or another greasy compound, comprising: a reaction chamber; at least one device for forming a liquid or semi-liquid jet of the composition, for example such as from a nozzle or a syringe, a device capable of producing one or more streams of the composition, entering the upper part of the reaction chamber and circulating within this reaction chamber from top to bottom; means for supplying the reaction chamber with cryogenic liquid, for example liquid nitrogen, to create a cold gas atmosphere within the reaction chamber and thus allow the total or partial freezing or crystallization of the stream(s) thus formed to be carried out; means for recovering the particles formed in the lower part of the chamber; characterized in that the installation comprises a device for cutting said product stream(s), using a wire or disc capable of rotating at a given and chosen speed, device positioned downstream of the outlet of said product stream(s) from said forming device(s), preferably positioned in
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Crystallography & Structural Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Edible Oils And Fats (AREA)
- Fats And Perfumes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
PROCEDE DE CRYO-CRISTALLISATION D'HUILES ET DE GRAISSES POUR DES APPLICATIONS DANS LES DOMAINESPROCESS FOR THE CRYO-CRYSTALLIZATION OF OILS AND FATS FOR APPLICATIONS IN THE FIELDS
DE L'AGRO-ALIMENTAIRE, DE LA COSMETIQUE OU ENCORE DE LA PHARMACIE FOOD, COSMETICS OR PHARMACY
La présente invention concerne le domaine des procédés et équipements dédiés à la cryo-cristallisation des huiles et graisses et cires, ou autre composés liquides ou semi- liquides graisseux, à haut point de fusion, pour des applications dans les domaines de l’agro-alimentaire, de la cosmétique ou encore de la pharmacie. The present invention relates to the field of processes and equipment dedicated to the cryo-crystallization of oils and fats and waxes, or other liquid or semi-liquid greasy compounds, with a high melting point, for applications in the fields of agri-food, cosmetics or even pharmacy.
On s’intéresse également ici à la fabrication de principes actifs mais aussi à la fabrication d’excipients, intervenant dans de telles applications industrielles. We are also interested here in the manufacture of active ingredients but also in the manufacture of excipients, involved in such industrial applications.
Les équipements de cryo-cristallisation de l’état de l’art permettent, on le sait, de transformer une huile, une graisse, une cire ou autre composé graisseux contenant une certaine proportion de principe actif, en un ensemble de particules solides se présentant sous la forme de poudre ou de billes. State-of-the-art cryo-crystallization equipment is known to transform an oil, a grease, a wax or other greasy compound containing a certain proportion of active ingredient into a set of solid particles in the form of powder or beads.
Les documents suivants illustrent la littérature très abondante et parfois ancienne, qui a été consacrée à cette question : EP-919 279, EP-0393 963, US-4 655 047, GB-2 092 880, WO99/33555, ou US-4 982 577, ou encore EP-1 285 584. The following documents illustrate the very abundant and sometimes old literature which has been devoted to this question: EP-919 279, EP-0393 963, US-4 655 047, GB-2 092 880, WO99/33555, or US-4 982 577, or EP-1 285 584.
On s’intéresse dans le cadre de la présente invention aux particules dites « mono- dispersées » ou « monodisperses », c'est-à-dire dont la taille est sensiblement la même, ne donnant pas lieu à la production d’agrégations, de particules doubles ou triples, ou encore de particules trop petites (« satellites »), particules trop petites qui sont un inconvénient majeur pour certaines applications, notamment pharmaceutiques, et dont l’élimination constitue alors un enjeu majeur. In the context of the present invention, we are interested in so-called "mono-dispersed" or "monodisperse" particles, that is to say those whose size is substantially the same, not giving rise to the production of aggregations, double or triple particles, or even particles that are too small ("satellites"), particles that are too small which are a major drawback for certain applications, particularly pharmaceutical ones, and the elimination of which then constitutes a major challenge.
Cette transformation physique (de fluides en particules) évoquée ci-dessus est recherchée dans de nombreux domaines tels que la nutrition, l’alimentation animale, les cosmétiques ou encore les produits pharmaceutiques. Elle offre de nombreux avantages tels que : This physical transformation (of fluids into particles) mentioned above is sought after in many fields such as nutrition, animal feed, cosmetics and pharmaceutical products. It offers many advantages such as:
• un dosage plus aisé des produits composant une recette industrielle, • un meilleur écoulement du produit, • easier dosage of the products making up an industrial recipe, • better product flow,
• un stockage facilité, • easy storage,
• une meilleure résistance à la compaction et à la reprise en masse, • better resistance to compaction and mass recovery,
• ainsi qu’une augmentation de la durée de vie. • as well as an increase in lifespan.
Un procédé de cryo-cristallisation consiste alors classiquement à atomiser le produit fondu dans une enceinte refroidie à l’aide d’un fluide cryogénique, typiquement de l’azote liquide, ce qui provoque un refroidissement brutal des particules en chute libre dans l’enceinte, jusqu’au point de cristallisation. La transformation est irréversible et le produit recueilli reste à l’état cristallisé sous forme d’une poudre ou de petites billes selon la technologie d’aspersion mise en place dans l’appareil. A cryo-crystallization process then classically consists of atomizing the molten product in a cooled enclosure using a cryogenic fluid, typically liquid nitrogen, which causes a sudden cooling of the particles falling freely in the enclosure, up to the point of crystallization. The transformation is irreversible and the collected product remains in the crystallized state in the form of a powder or small beads depending on the spraying technology implemented in the device.
La [Figure 1] annexée illustre par une vue schématique partielle les différentes parties d’un appareil de cryo-cristallisation typique de l’état de l’art. The attached [Figure 1] illustrates by a partial schematic view the different parts of a typical state-of-the-art cryo-crystallization device.
Expliquons le fonctionnement de cet équipement : les produits préalablement fondus et contenus dans le réservoir 1 sont acheminés dans l’équipement d’injection 2 situé dans la partie supérieure d’une enceinte 3 refroidie à l’aide d’un spray d’azote liquide 4, sous forme atomisée ou sous forme de gouttes selon la méthode qui a été choisie pour fractionner le produit à transformer. Let us explain how this equipment works: the products previously melted and contained in tank 1 are conveyed into the injection equipment 2 located in the upper part of an enclosure 3 cooled using a liquid nitrogen spray 4, in atomized form or in the form of drops depending on the method chosen to fractionate the product to be transformed.
De façon remarquable, l’énergie frigorifique développée par l’azote liquide autorise une congélation quasi-immédiate des particules de graisse au cours de leur chute dans la chambre de refroidissement. La poudre ou les billes ainsi constituées sont récupérées congelées en partie inférieure de l’enceinte dans un dispositif de collecte 5. Remarkably, the refrigerating energy developed by the liquid nitrogen allows almost immediate freezing of the grease particles as they fall into the cooling chamber. The powder or balls thus formed are recovered frozen in the lower part of the enclosure in a collection device 5.
On distingue généralement deux types de réalisation de l’injection du produit fondu dont le choix dépend du type de transformation souhaitée (types rappelés en [Figure 2] annexée). There are generally two types of injection of the molten product, the choice of which depends on the type of transformation desired (types recalled in [Figure 2] attached).
Le premier procédé ((a) - injection pneumatique) est sans doute considéré comme moins qualitatif que le second ((b), injection appelée « en électro-spray ») mais permet d’atteindre des productivités importantes, typiquement de l’ordre de 1000 kg/h. En revanche, la distribution de tailles de particules est large avec une proportion non négligeable de particules fines nécessitant une filtration soignée du flux gazeux extrait, voire un classement « ATEX » de l’installation de production. The first process ((a) - pneumatic injection) is undoubtedly considered less qualitative than the second ((b), injection called "electro-spray") but allows significant productivity to be achieved, typically of the order of 1000 kg/h. On the other hand, the particle size distribution is wide with a non- negligible fine particles requiring careful filtration of the extracted gas flow, or even “ATEX” classification of the production facility.
Dans les domaines exigeants tels que la pharmacie ou la cosmétologie, la transformation en billes mono-dispersées (on dit aussi monodisperses) est souvent requise. La formation de fines particules est alors évitée par l’application préférée du second procédé, au détriment de la productivité. En effet comme on l’a dit cette dernière est limitée à environ 200 kg/h, avec un potentiel de croissance limité au nombre maximal d’aiguilles implantable dans la tête d’injection. De plus, la productivité du système est sensible à la tension de surface du produit. In demanding fields such as pharmacy or cosmetology, transformation into monodisperse beads (also called monodisperse) is often required. The formation of fine particles is then avoided by the preferred application of the second process, to the detriment of productivity. Indeed, as mentioned, the latter is limited to approximately 200 kg/h, with a growth potential limited to the maximum number of needles implantable in the injection head. In addition, the productivity of the system is sensitive to the surface tension of the product.
Dans le cas de produits à faible tension de surface tels que des tensio-actifs, le débit de produit est limité. Ce type d’injection ne permet pas de transformer des produits ayant une tension de surface supérieure à 0,07 N/m correspondant aux produits très hydratés. Cette sensibilité à la tension de surface du produit implique une configuration et une productivité différentes d'un produit à un autre ce qui peut être très contraignant pour les sites producteurs traitant différents types de produit. In the case of products with low surface tension such as surfactants, the product flow rate is limited. This type of injection does not allow the processing of products with a surface tension greater than 0.07 N/m corresponding to highly hydrated products. This sensitivity to the surface tension of the product implies a different configuration and productivity from one product to another, which can be very restrictive for production sites processing different types of product.
Dans l’art antérieur, la réalisation de billes mono-dispersées avec une productivité supérieure passe alors par l’achat de plusieurs machines, ce qui peut freiner les décisions d’investissement et l’adoption de la technologie par l’industriel. In the prior art, the production of mono-dispersed beads with higher productivity requires the purchase of several machines, which can slow down investment decisions and the adoption of the technology by the manufacturer.
Comme on le verra plus en détails dans ce qui suit, la présente invention propose de remplacer le dispositif d’électro-spray implanté jusqu’ici classiquement dans les appareils de cryo-cristallisation, par un dispositif plus productif de génération des billes monodisperses, tout en conservant un haut niveau de qualité du produit transformé.As will be seen in more detail below, the present invention proposes to replace the electro-spray device conventionally installed until now in cryo-crystallization devices, with a more productive device for generating monodisperse beads, while maintaining a high level of quality of the transformed product.
On propose alors ici de mettre en œuvre un procédé de découpe d’un jet liquide issu par exemple d’une buse ou encore d’une seringue de production de ce jet, à l’aide d’un fil ou disque rotatif tournant à grande vitesse (on parle parfois dans l’industrie de « jet cutting »). We then propose to implement a process for cutting a liquid jet coming for example from a nozzle or a syringe producing this jet, using a wire or rotating disc rotating at high speed (in the industry we sometimes speak of "jet cutting").
La [Figure 3] annexée illustre par une vue schématique partielle le principe de fonctionnement d’une telle découpe au fil, on reconnaît sur la Figure 3 les éléments suivants : The attached [Figure 3] illustrates by a partial schematic view the operating principle of such wire cutting, the following elements can be seen in Figure 3:
10 : l’arrivée de produit (composition) liquide de graisse à traiter 11 : un moteur 10: arrival of liquid grease product (composition) to be treated 11: an engine
12 : le jet/courant de liquide produit 12: the jet/stream of liquid produced
13 : les particules produites en aval du disque ou fil (14) de coupe. 13: particles produced downstream of the cutting disc or wire (14).
Le passage du fil ou disque (14) au niveau du jet liquide de produit, provoque la découpe de cylindres qui se transforment en billes sphériques au cours de leur chute.The passage of the wire or disc (14) at the level of the liquid jet of product causes the cutting of cylinders which transform into spherical balls during their fall.
L’étendue typique des diamètres de billes envisageables avec ce procédé va typiquement de 0,2 mm à 3 mm, la quantité des billes générées par seconde dépend de la fréquence de rotation du fil de découpe, généralement de 5000 à 10 000 Hz mais pouvant aller jusqu’à 25 000 Hz. The typical range of ball diameters that can be achieved with this process is typically 0.2 mm to 3 mm, the quantity of balls generated per second depends on the rotation frequency of the cutting wire, generally 5000 to 10,000 Hz but can go up to 25,000 Hz.
A titre d’exemple, pour un diamètre de 3 mm et à la fréquence maximale de 25 000 Hz, la productivité peut atteindre 1200 kg/h, valeur 5 à 6 fois supérieure à celle atteignable en électro-spray. For example, for a diameter of 3 mm and at the maximum frequency of 25,000 Hz, productivity can reach 1200 kg/h, a value 5 to 6 times higher than that achievable with electro-spray.
Par ailleurs, cette productivité n’est pas affectée par la tension de surface du produit, ni par sa densité ou sa viscosité dynamique. Les performances annoncées peuvent ainsi être atteintes même pour des produits présentant une très faible tension de surface, inférieure à 20 mN/m par exemple pour des tensio-actifs. Furthermore, this productivity is not affected by the surface tension of the product, nor by its density or dynamic viscosity. The announced performances can therefore be achieved even for products with a very low surface tension, less than 20 mN/m for example for surfactants.
Selon un mode de mise en œuvre de l’invention qui est préféré, le dispositif de coupage évoqué ci-dessus est implanté en partie supérieure d’un appareil de cryo cristallisation, notamment entre le réservoir contenant le produit fondu et l’enceinte de refroidissement, ou encore dans la partie haute de cette enceinte. According to a preferred embodiment of the invention, the cutting device mentioned above is installed in the upper part of a cryo-crystallization apparatus, in particular between the reservoir containing the molten product and the cooling enclosure, or in the upper part of this enclosure.
La [Figure 4] annexée illustre par une vue schématique partielle un exemple de mise en œuvre de l’invention avec une telle implantation du système de découpe au sein d’un cryo-cristalliseur. The attached [Figure 4] illustrates by a partial schematic view an example of implementation of the invention with such an installation of the cutting system within a cryo-crystallizer.
La buse est alimentée à débit constant à partir du réservoir de produit liquide pressurisé, assurant, par la rotation à vitesse constante du fil de découpe 14, une distribution de taille de bille très resserrée. The nozzle is fed at a constant flow rate from the pressurized liquid product reservoir, ensuring, by the constant speed rotation of the cutting wire 14, a very tight ball size distribution.
Avantageusement comme on le voit sur la Figure 4, le système peut être équipé de une, deux ou plusieurs buses de production d’un jet 12 de liquide à traiter (à découper), alimentées préférentiellement avec le même débit, système de multiples buses augmentant par là même le nombre de billes générées par unité de temps. La productivité ainsi obtenue peut être élevée même pour un diamètre de bille inférieur à 3 mm. Advantageously, as seen in Figure 4, the system can be equipped with one, two or more nozzles for producing a jet 12 of liquid to be treated (to be cut), preferably supplied with the same flow rate, a system of multiple nozzles thereby increasing the number of balls generated per unit of time. productivity thus obtained can be high even for a ball diameter of less than 3 mm.
L’utilisation, conformément à l’invention ; du coupage au fil ou disque en cryo- cristallisation constitue un progrès notable par rapport à l’état de l’art; elle permet la production des billes monodisperses d’huiles, de graisses, de cires ou autres composés, de diamètre supérieur au mm, en plus grande quantité et dont la qualité est au moins équivalente à celle obtenue avec les procédés antérieurs. The use, in accordance with the invention, of wire or disc cutting in cryo-crystallization constitutes a notable advance compared to the state of the art; it allows the production of monodisperse beads of oils, fats, waxes or other compounds, with a diameter greater than one mm, in greater quantity and the quality of which is at least equivalent to that obtained with the previous processes.
Car en effet, le pouvoir frigorifique apporté par l’utilisation d’une cryogène liquide tel l’azote liquide autorise la cristallisation complète du produit sur une hauteur réduite, typiquement aux alentours de 2 m sur les appareils de l’état de l’art, à comparer aux systèmes de l’art antérieur équipés de circuits frigorifiques conventionnels à compression de vapeur dont la hauteur peut atteindre 5 à 10 mètres. Indeed, the refrigerating power provided by the use of a liquid cryogen such as liquid nitrogen allows the complete crystallization of the product over a reduced height, typically around 2 m on state-of-the-art devices, compared to prior art systems equipped with conventional vapor compression refrigeration circuits whose height can reach 5 to 10 meters.
La présente invention concerne alors un procédé de fabrication de particules solides, à partir d’une composition liquide ou semi-liquide, notamment à partir d’une composition d’huile, d’une graisse, d’une cire ou d’un autre composé graisseux, mettant en œuvre au moins un dispositif de formation d’un jet liquide ou semi-liquide du produit, par exemple tel qu’issu d’un buse ou encore d’une seringue, puis une étape de surgélation ou cristallisation totale ou partielle du jet ainsi formé, se caractérisant par la mise en œuvre des mesures suivantes : on produit à l’aide du ou des dispositifs de formation un ou plusieurs courants de la composition, entrant dans la partie haute d’une chambre de réaction et circulant au sein de cette chambre de réaction de haut en bas ; on alimente la chambre de réaction en liquide cryogénique, par exemple en azote liquide, pour créer une atmosphère de gaz froid au sein de la chambre de réaction ; on récupère dans la partie basse de la chambre les particules formées ; se caractérisant en ce que l’on met en œuvre un appareil de découpe du ou desdits courants de produit, à l’aide d’un fil ou disque tournant à vitesse donnée et choisie, appareil positionné en aval de la sortie desdits courants de produit du ou desdits dispositifs de formation, préférentiellement positionné en partie supérieure de la chambre, le passage du fil ou disque permettant de provoquer la découpe de particules du produit sensiblement cylindriques, se transformant en particules sphérique ou sensiblement sphériques au cours de leur chute au sein de la chambre vers la partie basse de la chambre où s’effectue leur récupération. The present invention then relates to a method for manufacturing solid particles, from a liquid or semi-liquid composition, in particular from a composition of oil, a grease, a wax or another greasy compound, using at least one device for forming a liquid or semi-liquid jet of the product, for example such as from a nozzle or a syringe, then a step of total or partial freezing or crystallization of the jet thus formed, characterized by the implementation of the following measures: one or more streams of the composition are produced using the forming device(s), entering the upper part of a reaction chamber and circulating within this reaction chamber from top to bottom; the reaction chamber is supplied with cryogenic liquid, for example liquid nitrogen, to create a cold gas atmosphere within the reaction chamber; the particles formed are recovered in the lower part of the chamber; characterized in that an apparatus is used for cutting said product stream(s) using a wire or disc rotating at a given and chosen speed, the apparatus being positioned downstream of the outlet of said product stream(s) from said forming device(s), preferably positioned in the upper part of the chamber, the passage of the wire or disc making it possible to cause the cutting of substantially cylindrical particles of the product, transforming into spherical or substantially spherical during their fall within the chamber towards the lower part of the chamber where they are recovered.
La présente invention concerne également une installation de fabrication de particules solides, à partir d’une composition liquide ou semi-liquide, notamment à partir d’une composition d’huile, d’une graisse, d’une cire ou d’un autre composé graisseux, comportant : une chambre de réaction ; au moins un dispositif de formation d’un jet liquide ou semi-liquide de la composition, par exemple tel qu’issu d’un buse ou encore d’une seringue, dispositif apte à produire un ou plusieurs courants de la composition, entrant dans la partie haute de la chambre de réaction et circulant au sein de cette chambre de réaction de haut en bas ; des moyens d’alimentation de la chambre de réaction en liquide cryogénique, par exemple en azote liquide, pour créer une atmosphère de gaz froid au sein de la chambre de réaction et ainsi permettre de réaliser la surgélation ou cristallisation totale ou partielle du ou des courants ainsi formé(s); des moyens de récupération dans la partie basse de la chambre des particules formées ; se caractérisant en ce que l’installation comporte un appareil de découpe du ou desdits courants de produit, à l’aide d’un fil ou disque apte à tourner à vitesse donnée et choisie, appareil positionné en aval de la sortie desdits courants de produit du ou desdits dispositifs de formation, préférentiellement positionné en partie supérieure de la chambre, le passage du fil ou disque permettant de provoquer la découpe de particules du produit sensiblement cylindriques, se transformant en particules sphérique ou sensiblement sphériques au cours de leur chute au sein de la chambre vers la partie basse de la chambre où s’effectue leur récupération à l’aide desdits moyens de récupération. The present invention also relates to an installation for manufacturing solid particles, from a liquid or semi-liquid composition, in particular from a composition of oil, a grease, a wax or another greasy compound, comprising: a reaction chamber; at least one device for forming a liquid or semi-liquid jet of the composition, for example such as from a nozzle or a syringe, a device capable of producing one or more streams of the composition, entering the upper part of the reaction chamber and circulating within this reaction chamber from top to bottom; means for supplying the reaction chamber with cryogenic liquid, for example liquid nitrogen, to create a cold gas atmosphere within the reaction chamber and thus allow the total or partial freezing or crystallization of the stream(s) thus formed to be carried out; means for recovering the particles formed in the lower part of the chamber; characterized in that the installation comprises a device for cutting said product stream(s), using a wire or disc capable of rotating at a given and chosen speed, device positioned downstream of the outlet of said product stream(s) from said forming device(s), preferably positioned in the upper part of the chamber, the passage of the wire or disc making it possible to cause the cutting of substantially cylindrical particles of the product, transforming into spherical or substantially spherical particles during their fall within the chamber towards the lower part of the chamber where they are recovered using said recovery means.
Claims
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FRFR2313205 | 2023-11-28 | ||
| FR2313205A FR3155723B1 (en) | 2023-11-28 | 2023-11-28 | Cryogenic crystallization process for oils and fats for applications in the food, cosmetics and pharmaceutical industries |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2025113960A1 true WO2025113960A1 (en) | 2025-06-05 |
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ID=89897352
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/EP2024/081751 Pending WO2025113960A1 (en) | 2023-11-28 | 2024-11-08 | Method for the cryo-crystallisation of oils and fats for applications in the agri-food, cosmetics or pharmacy fields |
Country Status (2)
| Country | Link |
|---|---|
| FR (1) | FR3155723B1 (en) |
| WO (1) | WO2025113960A1 (en) |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2092880A (en) | 1981-01-27 | 1982-08-25 | Boc Ltd | Freezing a liquid |
| US4655047A (en) | 1985-03-25 | 1987-04-07 | I.Q.F. Inc. | Process for freezing or chilling |
| EP0393963A2 (en) | 1989-04-17 | 1990-10-24 | Canadian Oxygen Limited | Method and apparatus for cryogenic crystallization of fats |
| US4982577A (en) | 1990-03-19 | 1991-01-08 | I.Q.F. Inc. | Cryogenic apparatus |
| EP0919279A1 (en) | 1997-11-27 | 1999-06-02 | Messer Griesheim Gmbh | Process and device for pelletizing or granulating liquid or pasty material |
| WO1999033555A1 (en) | 1997-12-24 | 1999-07-08 | Goudsche Machinefabriek B.V. | Method and apparatus for forming granulate from a melt of chemical products |
| EP1285584A2 (en) | 2001-08-23 | 2003-02-26 | The BOC Group plc | Cryogenic crystallisation of fats |
| WO2010063918A1 (en) * | 2008-12-04 | 2010-06-10 | L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Method and equipment for manufacturing deep-frozen beads |
| EP2226062A1 (en) * | 2009-03-06 | 2010-09-08 | Linde AG | Method for making cosmetics |
| WO2010099966A2 (en) * | 2009-03-06 | 2010-09-10 | Linde Aktiengesellschaft | Method for formulating cosmetics |
| EP2345475A1 (en) * | 2010-01-19 | 2011-07-20 | L'AIR LIQUIDE, Société Anonyme pour l'Etude et l'Exploitation des Procédés Georges Claude | Process and installation for the production of solid particles from a liquid or semi-liquid composition |
| WO2012041682A1 (en) * | 2010-09-29 | 2012-04-05 | Unilever Nv | Cyrogenic spray process |
-
2023
- 2023-11-28 FR FR2313205A patent/FR3155723B1/en active Active
-
2024
- 2024-11-08 WO PCT/EP2024/081751 patent/WO2025113960A1/en active Pending
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2092880A (en) | 1981-01-27 | 1982-08-25 | Boc Ltd | Freezing a liquid |
| US4655047A (en) | 1985-03-25 | 1987-04-07 | I.Q.F. Inc. | Process for freezing or chilling |
| EP0393963A2 (en) | 1989-04-17 | 1990-10-24 | Canadian Oxygen Limited | Method and apparatus for cryogenic crystallization of fats |
| US4982577A (en) | 1990-03-19 | 1991-01-08 | I.Q.F. Inc. | Cryogenic apparatus |
| EP0919279A1 (en) | 1997-11-27 | 1999-06-02 | Messer Griesheim Gmbh | Process and device for pelletizing or granulating liquid or pasty material |
| WO1999033555A1 (en) | 1997-12-24 | 1999-07-08 | Goudsche Machinefabriek B.V. | Method and apparatus for forming granulate from a melt of chemical products |
| EP1285584A2 (en) | 2001-08-23 | 2003-02-26 | The BOC Group plc | Cryogenic crystallisation of fats |
| WO2010063918A1 (en) * | 2008-12-04 | 2010-06-10 | L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Method and equipment for manufacturing deep-frozen beads |
| EP2226062A1 (en) * | 2009-03-06 | 2010-09-08 | Linde AG | Method for making cosmetics |
| WO2010099966A2 (en) * | 2009-03-06 | 2010-09-10 | Linde Aktiengesellschaft | Method for formulating cosmetics |
| EP2345475A1 (en) * | 2010-01-19 | 2011-07-20 | L'AIR LIQUIDE, Société Anonyme pour l'Etude et l'Exploitation des Procédés Georges Claude | Process and installation for the production of solid particles from a liquid or semi-liquid composition |
| WO2012041682A1 (en) * | 2010-09-29 | 2012-04-05 | Unilever Nv | Cyrogenic spray process |
Also Published As
| Publication number | Publication date |
|---|---|
| FR3155723A1 (en) | 2025-05-30 |
| FR3155723B1 (en) | 2025-11-14 |
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