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WO1999042545A1 - Method for producing microcrystals of vegetable and animal fats - Google Patents

Method for producing microcrystals of vegetable and animal fats Download PDF

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Publication number
WO1999042545A1
WO1999042545A1 PCT/BE1999/000026 BE9900026W WO9942545A1 WO 1999042545 A1 WO1999042545 A1 WO 1999042545A1 BE 9900026 W BE9900026 W BE 9900026W WO 9942545 A1 WO9942545 A1 WO 9942545A1
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WIPO (PCT)
Prior art keywords
fat
water
separation
ejector
vegetable
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.)
Ceased
Application number
PCT/BE1999/000026
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French (fr)
Other versions
WO1999042545A8 (en
Inventor
Etienne Deffense
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Crystallisation & Degumming Sprl
Original Assignee
Crystallisation & Degumming Sprl
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Publication date
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Priority to EP99934298A priority Critical patent/EP1056820A1/en
Publication of WO1999042545A1 publication Critical patent/WO1999042545A1/en
Publication of WO1999042545A8 publication Critical patent/WO1999042545A8/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B15/00—Solidifying fatty oils, fats, or waxes by physical processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/20—Jet mixers, i.e. mixers using high-speed fluid streams
    • B01F25/21—Jet mixers, i.e. mixers using high-speed fluid streams with submerged injectors, e.g. nozzles, for injecting high-pressure jets into a large volume or into mixing chambers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/30—Injector mixers
    • B01F25/31—Injector mixers in conduits or tubes through which the main component flows
    • B01F25/312—Injector mixers in conduits or tubes through which the main component flows with Venturi elements; Details thereof
    • B01F25/3121—Injector mixers in conduits or tubes through which the main component flows with Venturi elements; Details thereof with additional mixing means other than injector mixers, e.g. screens, baffles or rotating elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/30—Injector mixers
    • B01F25/31—Injector mixers in conduits or tubes through which the main component flows
    • B01F25/312—Injector mixers in conduits or tubes through which the main component flows with Venturi elements; Details thereof
    • B01F25/3124—Injector mixers in conduits or tubes through which the main component flows with Venturi elements; Details thereof characterised by the place of introduction of the main flow
    • B01F25/31243—Eductor or eductor-type venturi, i.e. the main flow being injected through the venturi with high speed in the form of a jet
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40—Static mixers
    • B01F25/42—Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
    • B01F25/43—Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction
    • B01F25/433—Mixing tubes wherein the shape of the tube influences the mixing, e.g. mixing tubes with varying cross-section or provided with inwardly extending profiles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40—Static mixers
    • B01F25/42—Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
    • B01F25/43—Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction
    • B01F25/433—Mixing tubes wherein the shape of the tube influences the mixing, e.g. mixing tubes with varying cross-section or provided with inwardly extending profiles
    • B01F25/4335—Mixers with a converging-diverging cross-section
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B7/00—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils
    • C11B7/0091—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils non-solvents, e.g. water wherein the fat or oil is dispersed account a more washing out of fractions is not taken into
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/50—Circulation mixers, e.g. wherein at least part of the mixture is discharged from and reintroduced into a receptacle

Definitions

  • the present invention relates to a process for the continuous crystallization of fats and oils, more particularly of vegetable and animal origin, and of the corresponding fatty acids.
  • compositions can be generically designated by the expression "fatty substances”.
  • - fats with a very high percentage of triglycerides with a high melting point such as vegetable tallows generally called exotic fats, cocoa butters, palm-mid-fractions, palm kernel and hydrogenated oils,
  • fats with a high percentage of low-melting triglycerides such as, for example, partially hydrogenated palm, butter, bacon and fish fats,
  • fractionation of fats with a high melting point requires small crystallizers with a very large exchange surface in order to eliminate the latent heat of crystallization released suddenly by the fat.
  • a recent patent application (PCT / BE96 / 00106) describes the same principle of separation but instead of introducing the palm kernel in the liquid, or semi-solid or even pasty state, it is introduced in the form of a ball in a aqueous solution previously refrigerated.
  • the process is characterized in that it consists in melting the fat, in dividing the melt into the most homogeneous balls possible and of the most regular dimensions possible, and to introduce these beads into an aqueous solution. ".
  • the whole art lies in dividing the melted fat into beads using perforated plates.
  • the present invention in fact uses a dynamic system comprising a venturi as present in a liquid ejector or hydro-ejector.
  • the invention more generally provides a method which consists in crystallizing the fat, preferably continuously, and in separating it either by centrifugation or by filtration depending on the type of fat.
  • the separation of the crystals can be done directly or after tempering depending on the polymorphic form required.
  • a melted fat is used which is then sucked into a hydro-ejector, generally located at an upper part of the installation, and brought into a reactor equipped with an agitator and an exchanger to control the reactor temperature.
  • Hot grease in contact with cold water excellent cold conductor, directly
  • instantly forms a mixture of micro-crystals in water can be in the form of a suspension of micro-crystals in water (palm kernel) or oil-water-crystal emulsions (case of palm fat or liquid fats), the crystals being in the oil phase.
  • the invention can therefore be applied to the three categories of fat defined in the introduction to this description.
  • the water temperature of one hydro-ejector can be adjusted between 2 and 35 ° C depending on the fat, for example preferably about 8 ° C for palm fat. Only triglycerides with a high melting point crystallize, the others remain liquid.
  • the resulting crystal-oil-liquid-water emulsion separates fairly quickly in the reactor into an upper phase consisting of crystals in suspension in the oil, and an aqueous phase which settles in the lower part.
  • the upper phase (crystal-oil) is separated immediately or after tempering with stirring and controlled temperature.
  • the separation can be carried out either by centrifugation or by filtration through a membrane filter press.
  • the aqueous phase it can be recycled in the hydro-ejector after adjusting the temperature.
  • the crystals formed float in the water at the top of the reactor.
  • the aqueous phase settles in the lower part and can be advantageously recycled.
  • the suspension of the crystals is kept under stirring for a certain time, for example from 2 to 5 hours between 10 and 22 ° C., before being pumped into a membrane filter.
  • the water entrained with the crystals is first removed, then the crystals are compacted, e.g. for at least 30 minutes at minimum 20 bar.
  • the palm kernel thus produces a liquid phase, olein, with an iodine index of 24.5.
  • a solid fraction is obtained, in the form of a stearin cake, the iodine index of 7 starting from palm kernel of 17.5 of iodine index.
  • the process can be applied to crude or refined fats, which may or may not still contain water.
  • a melted (18% water) and homogenized butter can be crystallized immediately by giving an aqueous phase and triglyceride crystals with high melting point, present in suspension in an oil with low Fusion point.
  • oils rich in waxes such as sunflower oil, subjected to the process of the invention generate an oily phase containing wax crystals in suspension.
  • Fig. 1 illustrates a hydro-ejector suitable for practicing the invention.
  • the fluid sucked into one hydro-ejector is, for example, the molten palm kernel which comes into contact with the working fluid, namely water, at the outlet of the driving nozzle.
  • the hot fluid (palm kernel) mixed with the cold fluid (water) is instantly cooled by turbulence and sprayed at high speed in the form of a stable dispersion of water-fat micro-crystals.
  • This emulsion is pumped directly into the high pressure membrane filter press or can be previously tempered or matured (stirred) at the desired temperature before being filtered.
  • the hydro-ejector is located at the top of a reactor. However, it can be found elsewhere and even be submerged in a reactor.
  • the reactor can also be equipped with a multi-hydro-ejector (ejector with several outlets).
  • the invention is illustrated by the following example.
  • a 2 liter crystallizer cooled to 10 ° C. is prepared using a double jacket and provided with an agitator and a hydro-ejector (water pump) supplied with water at 10 ° C. at a flow rate of 15 1 / minute.
  • 500 g palm nut 17.5 of iodine value, liquefied at 70 ° C is sucked from a tank in the crystallizer at a rate of 4 1 / minute via the water pump.
  • Palm kernel fat crystals varying in size from 5 to 800 microns are immediately formed. These remain perfectly suspended in water in the upper part of the crystallizer.
  • the lower part of the crystallizer - that is 3/4 of the total volume - is occupied by decanted water. This can be pumped by a bottom valve and then recycled to the water pump supply tank whose temperature is maintained at 10 ° C.
  • the supernatant part of the crystallizer composed of crystals suspended in water is stirred for 3 to 10 hours at 10 ° C and then pumped to a membrane press filter. During the feeding of the filter, the water used as a means of transport is also eliminated and recycled.
  • a stearin cake with an iodine index of 7 is collected with a yield of approximately 37%.
  • the iodine index of the olein collected is 24-25.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Fats And Perfumes (AREA)
  • Edible Oils And Fats (AREA)

Abstract

The invention invention concerns a method for continuously crystallising fats and oils, more particularly of vegetable and animal origin, and of the corresponding fatty acids. The method comprises a step wherein the previously melted fat is sucked up by a hydro-ejector thereby producing a mixture of microcrystals, which is separated either by centrifuging, or by filtering depending on the type of fat. The separation of the crystals can be done by phase separation and filtering, preferably by membrane filtration.

Description

Procédé de production de micro-cristaux de graisses végétales et animalesProcess for producing micro-crystals of vegetable and animal fats

La présente invention concerne un procédé de cristallisation en continu de graisses et huiles, plus particulièrement d'origine végétale et animale, et des acides gras correspondants.The present invention relates to a process for the continuous crystallization of fats and oils, more particularly of vegetable and animal origin, and of the corresponding fatty acids.

Ces compositions peuvent être génériquement désignées sous l'expression "matières grasses".These compositions can be generically designated by the expression "fatty substances".

On sait que, pour l'application de la purification par cristallisation fractionnée, pour les différentes matières grasses, on distingue trois grandes familles :We know that, for the application of purification by fractional crystallization, for the different fats, there are three main families:

- les graisses à pourcentage très élevé en triglycérides à haut point de fusion tels que les suifs végétaux appelés généralement graisses exotiques, les beurres de cacao, les palm-mid-fractions, le palmiste et les huiles hydrogénées,- fats with a very high percentage of triglycerides with a high melting point such as vegetable tallows generally called exotic fats, cocoa butters, palm-mid-fractions, palm kernel and hydrogenated oils,

les graisses comportant un pourcentage élevé en triglycérides à bas point de fusion telles que, à titre d'exemples, les graisses de palme, de beurre, de lard et de poisson partiellement hydrogénées,fats with a high percentage of low-melting triglycerides such as, for example, partially hydrogenated palm, butter, bacon and fish fats,

- les huiles contenant une faible quantité de matière solide à haut point de fusion (triglycérides ou cires) telles que les huiles de tournesol, mais, coton. Ainsi, la purification de la graisse de palme, qui est une des graisses les plus fractionnées dans le monde, fait appel actuellement à des procédés de cristallisation à sec avec des cristalliseurs dont la capacité varie de 20 à 60 tonnes . La graisse fondue est chauffée puis refroidie progressivement pendant 5 à 18 heures selon le procédé utilisé, avant d'être filtrée à l'aide de filtre à membrane à haute pression. Par comparaison avec le autres techniques utilisées dans le domaine des corps gras, la cristallisation fractionnée reste un procédé lent et exige une place énorme car chaque installation comporte plusieurs cristalliseurs.- oils containing a small amount of solid material with a high melting point (triglycerides or waxes) such as sunflower, corn, cottonseed oils. Thus, the purification of palm fat, which is one of the most fractionated fats in the world, currently uses dry crystallization processes with crystallizers whose capacity varies from 20 to 60 tonnes. The melted fat is heated and then gradually cooled for 5 to 18 hours depending on the process used, before being filtered using a high pressure membrane filter. Compared with the other techniques used in the field of fatty substances, fractional crystallization remains a slow process and requires an enormous space since each installation comprises several crystallizers.

Par ailleurs, le fractionnement des graisses à haut point de fusion (ex. le palmiste) nécessite de petits cristalliseurs à très grande surface d'échange afin d'éliminer la chaleur latente de cristallisation libérée brutalement par la graisse.Furthermore, the fractionation of fats with a high melting point (eg palm kernel) requires small crystallizers with a very large exchange surface in order to eliminate the latent heat of crystallization released suddenly by the fat.

Celles-ci présentent une tendance à figer rapidement en rendant la séparation très difficile.These have a tendency to freeze quickly, making separation very difficult.

Ces graisses à haut point de fusion sont donc cristallisées complètement sous forme de blocs de graisse qui doivent être compressées ensuite à 1 ' aide de presse hydrauliques pour en retirer par fusion partielle, les triglycérides à bas point de fusion. Ces techniques sont coûteuses et nécessitent beaucoup de main d'oeuvre et beaucoup de place . Pour pallier ces inconvénients, le palmiste à l'état liquide peut être introduit dans un filtre presse à membrane, cristallisé dans les chambres du filtre puis compressé pour en retirer une oléine à bas point de fusion (voir p.e. brevet européen 0 256 760, Fuji Oil Co LRD) . Ce procédé bien qu'offrant une plus grande automatisation, immobilise un filtre à presse à membrane à haute pression très coûteux pour réaliser à la fois la cristallisation et la séparation.These high melting point fats are therefore crystallized completely in the form of blocks of fat which must then be compressed using a hydraulic press to remove, by partial melting, the low melting triglycerides. These techniques are expensive and require a lot of manpower and a lot of space. To overcome these drawbacks, the palm kernel in the liquid state can be introduced into a membrane filter press, crystallized in the filter chambers and then compressed to remove an olein with a low melting point (see eg European patent 0 256 760, Fuji Oil Co LRD). This process, although offering greater automation, immobilizes a very expensive high-pressure membrane press filter to carry out both crystallization and separation.

Afin de ne pas immobiliser le filtre pendant des heures pour la cristallisation proprement dite, certains industriels essaient de pré-cristalliser le palmiste avant de l'introduire dans le filtre. Cette technique soulève deux problèmes : d'une part la masse cristalline pâteuse est difficile à introduire dans le filtre presse à membrane et d'autre part si celle-ci doit rester partiellement cristallisée pour en favoriser l'introduction, sa cristallisation doit être parachevée dans le filtre. On notera que la masse cristalline pâteuse introduite de cette façon subit une fusion partielle qui diminue le rendement de la fraction solide recherchée .In order not to immobilize the filter for hours for the actual crystallization, some manufacturers try to pre-crystallize the palm kernel before introducing it into the filter. This technique raises two problems: on the one hand the pasty crystalline mass is difficult to introduce into the membrane press filter and on the other hand if the latter has to remain partially crystallized to encourage its introduction, its crystallization must be completed in the filter. It will be noted that the pasty crystalline mass introduced in this way undergoes partial melting which reduces the yield of the desired solid fraction.

Une demande de brevet récent (PCT/BE96/00106) décrit le même principe de séparation mais au lieu d'introduire le palmiste à l'état liquide, ou semi-solide voire pâteux, celui-ci est introduit sous forme de bille dans une solution aqueuse préalablement réfrigérée. le procédé est caractérisé en ce qu'il consiste à fondre les matières grasses, à diviser la masse fondue en billes les plus homogènes possibles et de dimension les plus régulières possibles, et à introduire ces billes dans une solution aqueuse..". Selon ce procédé, tout l'art réside à diviser la matière grasse fondue en billes à l'aide de plaques perforées .A recent patent application (PCT / BE96 / 00106) describes the same principle of separation but instead of introducing the palm kernel in the liquid, or semi-solid or even pasty state, it is introduced in the form of a ball in a aqueous solution previously refrigerated. the process is characterized in that it consists in melting the fat, in dividing the melt into the most homogeneous balls possible and of the most regular dimensions possible, and to introduce these beads into an aqueous solution. ". According to this process, the whole art lies in dividing the melted fat into beads using perforated plates.

Il a maintenant été constaté que, selon un procédé plus avantageux et plus rapide, on peut produire à l'aide d'un hydro-éjecteur un mélange de micro-cristaux, composé de matière grasse et d'eau.It has now been found that, according to a more advantageous and faster process, a mixture of micro-crystals, composed of fat and water, can be produced using a hydro-ejector.

Le présente invention recourt en effet à un système dynamique comprenant un venturi tel que présent dans un éjecteur de liquide ou hydro-éjecteur.The present invention in fact uses a dynamic system comprising a venturi as present in a liquid ejector or hydro-ejector.

L'invention propose plus généralement un procédé qui consiste à cristalliser la matière grasse, de préférence en continu, et à la séparer soit par centrifugation, soit par filtration selon le type de matière grasse. La séparation des cristaux peut se faire directement ou après tempérage selon la forme polymorphique requise.The invention more generally provides a method which consists in crystallizing the fat, preferably continuously, and in separating it either by centrifugation or by filtration depending on the type of fat. The separation of the crystals can be done directly or after tempering depending on the polymorphic form required.

Selon un mode de réalisation de l'invention, on utilise une matière grasse fondue qui est ensuite aspirée dans un hydro-éjecteur , localisé généralement à une partie supérieure de l'installation, et amenée dans un réacteur muni d'un agitateur et d'un echangeur pour contrôler la température du réacteur. La graisse chaude au contact de l'eau froide (excellent conducteur de froid, en direct) forme instantanément un mélange de micro-cristaux dans 1 ' eau. Ce dernier mélange, selon notamment la nature de la matière grasse et la température de l'eau, peut se présenter sous la forme de suspension de micro-cristaux dans l'eau (cas du palmiste) ou d'émulsions huile-eau- cristaux (cas de la graisse de palme ou des matières grasses liquides) , les cristaux se trouvant dans la phase huile .According to one embodiment of the invention, a melted fat is used which is then sucked into a hydro-ejector, generally located at an upper part of the installation, and brought into a reactor equipped with an agitator and an exchanger to control the reactor temperature. Hot grease in contact with cold water (excellent cold conductor, directly) instantly forms a mixture of micro-crystals in water. This latter mixture, depending in particular on the nature of the fat and the temperature of the water, can be in the form of a suspension of micro-crystals in water (palm kernel) or oil-water-crystal emulsions (case of palm fat or liquid fats), the crystals being in the oil phase.

L'invention peut donc s'appliquer aux trois catégories de matière grasse définie dans l'introduction de cet exposé .The invention can therefore be applied to the three categories of fat defined in the introduction to this description.

La température de l'eau de 1 ' hydro-éjecteur peut être ajustée entre 2 et 35°C selon la matière grasse, par exemple de préférence à environ 8°C pour la graisse de palme. Seuls les triglycérides à haut point de fusion cristallisent, les autres restent liquides.The water temperature of one hydro-ejector can be adjusted between 2 and 35 ° C depending on the fat, for example preferably about 8 ° C for palm fat. Only triglycerides with a high melting point crystallize, the others remain liquid.

Dans le cas où il y a trois phases, soit pour les deux dernières catégories susmentionnées à température ordinaire, l'émulsion résultante cristaux-huile liquide-eau se sépare assez rapidement dans le réacteur en une phase supérieure constituée de cristaux en suspension dans l'huile, et une phase aqueuse qui décante dans la partie inférieure.In the case where there are three phases, i.e. for the last two categories mentioned above at ordinary temperature, the resulting crystal-oil-liquid-water emulsion separates fairly quickly in the reactor into an upper phase consisting of crystals in suspension in the oil, and an aqueous phase which settles in the lower part.

La phase supérieure (cristaux-huile) est séparée aussitôt ou après tempérage sous agitation et température contrôlée. La séparation peut être menée soit par centrifugation ou par filtration sur filtre presse à membranes . La phase aqueuse quant à elle peut être recyclée dans la 1 ' hydro-éjecteur après ajustement de la température.The upper phase (crystal-oil) is separated immediately or after tempering with stirring and controlled temperature. The separation can be carried out either by centrifugation or by filtration through a membrane filter press. As for the aqueous phase, it can be recycled in the hydro-ejector after adjusting the temperature.

Dans le cas du palmiste, les cristaux formés surnagent dans l'eau, dans la partie supérieure du réacteur. La phase aqueuse décante dans la partie inférieure et peut être avantageusement recyclée.In the case of palm kernel, the crystals formed float in the water at the top of the reactor. The aqueous phase settles in the lower part and can be advantageously recycled.

Toujours dans le cas du palmiste, de préférence, la suspension des cristaux est maintenue sous agitation pendant un certain temps, par exemple de 2 à 5 heures entre 10 et 22°C, avant d'être pompée dans un filtre à membrane. L'eau entraînée avec les cristaux est d'abord éliminée, puis les cristaux sont compactés, p.e. pendant minimum 30 minutes à minimum 20 bar.Still in the case of palm kernel, preferably, the suspension of the crystals is kept under stirring for a certain time, for example from 2 to 5 hours between 10 and 22 ° C., before being pumped into a membrane filter. The water entrained with the crystals is first removed, then the crystals are compacted, e.g. for at least 30 minutes at minimum 20 bar.

Le palmiste produit ainsi une phase liquide , l'oléine, d'indice d'iode de 24,5. Après débatissage du filtre, on obtient une fraction solide, sous la forme d'un gâteau de stéarine dont l'indice d'iode est de 7 en partant de palmiste de 17,5 d'indice d'iode.The palm kernel thus produces a liquid phase, olein, with an iodine index of 24.5. After stripping the filter, a solid fraction is obtained, in the form of a stearin cake, the iodine index of 7 starting from palm kernel of 17.5 of iodine index.

Le procédé peut être appliqué à des graisses brutes ou raffinées, contenant ou non encore de l'eau.The process can be applied to crude or refined fats, which may or may not still contain water.

Ainsi, avec le procédé de l'invention, un beurre fondu (18% d'eau) et homogénéisé peut être cristallisé immédiatement en donnant une phase aqueuse et des cristaux de triglycérides à haut point de fusion, présents en suspension dans une huile à bas point de fusion. Par ailleurs, les huiles riches en cires, telle que l'huile de tournesol, soumises au procédé de l'invention génèrent une phase huileuse contenant des cristaux de cires en suspension.Thus, with the process of the invention, a melted (18% water) and homogenized butter can be crystallized immediately by giving an aqueous phase and triglyceride crystals with high melting point, present in suspension in an oil with low Fusion point. Furthermore, oils rich in waxes, such as sunflower oil, subjected to the process of the invention generate an oily phase containing wax crystals in suspension.

La fig. 1 illustre un hydroéjecteur approprié pour pratiquer l'invention. Le fluide aspiré dans 1 ' hydro-éjecteur est, par exemple, le palmiste fondu qui entre en contact avec le fluide moteur, à savoir l'eau, à la sortie de la buse motrice.Fig. 1 illustrates a hydro-ejector suitable for practicing the invention. The fluid sucked into one hydro-ejector is, for example, the molten palm kernel which comes into contact with the working fluid, namely water, at the outlet of the driving nozzle.

Le fluide chaud (palmiste) mélangé au fluide froid (l'eau) est refroidi instantanément par effet de turbulence et pulvérisé à grande vitesse sous la formed 'une dispersion stable de micro-cristaux eau-graisse. Cette émulsion est pompée directement dans le filtre presse à membrane à haute pression ou peut être préalablement tempérée ou maturée (agitée) à la température souhaitée avant d'être filtrée.The hot fluid (palm kernel) mixed with the cold fluid (water) is instantly cooled by turbulence and sprayed at high speed in the form of a stable dispersion of water-fat micro-crystals. This emulsion is pumped directly into the high pressure membrane filter press or can be previously tempered or matured (stirred) at the desired temperature before being filtered.

Selon la fig. 2 l 'hydroéjecteur est situé au sommet d'un réacteur. Il peut cependant se trouver ailleurs et même être immergé dans un réacteur. Le réacteur peut d'ailleurs être équipée d'un multi-hydroéjecteur (éjecteur à plusieurs sorties) .According to fig. 2 the hydro-ejector is located at the top of a reactor. However, it can be found elsewhere and even be submerged in a reactor. The reactor can also be equipped with a multi-hydro-ejector (ejector with several outlets).

L'invention est illustrée par l'exemple suivant.The invention is illustrated by the following example.

On prépare un cristalliseur de 2 litres refroidi à 10° C à l'aide d'une double enveloppe et muni d'un agitateur et d'un hydro-éjecteur (pompe à eau) alimenté en eau à 10°C à un débit de 15 1/minute. 500 g de palmiste de 17,5 d' indice d'iode, liquéfiée à 70°C est aspirée à partir d'une cuve dans le cristalliseur à un débit de 4 1/minute via la trompe à eau.A 2 liter crystallizer cooled to 10 ° C. is prepared using a double jacket and provided with an agitator and a hydro-ejector (water pump) supplied with water at 10 ° C. at a flow rate of 15 1 / minute. 500 g palm nut 17.5 of iodine value, liquefied at 70 ° C is sucked from a tank in the crystallizer at a rate of 4 1 / minute via the water pump.

Après 8 secondes, 1 ' hydro-éjecteur est arrêté. Des cristaux de graisse de palmiste de taille variant de 5 à 800 microns sont aussitôt formés. Ceux-ci restent parfaitement en suspension dans l'eau dans la partie supérieure du cristalliseur. La partie inférieure du cristalliseur - c'est à dire les 3/4 du volume total - est occupée par l'eau décantée. Celle-ci peut être pompée par une vanne de fond puis recyclée dans le tank d'alimentation de la trompe à eau dont la température est maintenue à 10 °C.After 8 seconds, the hydro-ejector is stopped. Palm kernel fat crystals varying in size from 5 to 800 microns are immediately formed. These remain perfectly suspended in water in the upper part of the crystallizer. The lower part of the crystallizer - that is 3/4 of the total volume - is occupied by decanted water. This can be pumped by a bottom valve and then recycled to the water pump supply tank whose temperature is maintained at 10 ° C.

La partie surnageante du cristalliseur composée de cristaux en suspension dans l'eau est agitée pendant 3 à 10 heures à 10°C puis pompée vers un filtre presse à membrane. Au cours de l'alimentation du filtre, l'eau servant de moyen de transport, est éliminée et recyclée également .The supernatant part of the crystallizer composed of crystals suspended in water is stirred for 3 to 10 hours at 10 ° C and then pumped to a membrane press filter. During the feeding of the filter, the water used as a means of transport is also eliminated and recycled.

Après compactage de la masse cristalline à 30 bar et débatissage, on recueille un gâteau de stéarine d'indice d'iode de 7 avec un rendement d'environ 37 %. L'indice d'iode de l'oléine recueillie est de 24-25. After compacting the crystalline mass at 30 bar and deburring, a stearin cake with an iodine index of 7 is collected with a yield of approximately 37%. The iodine index of the olein collected is 24-25.

Claims

Revendications claims 1. Procédé de séparation de matière grasse végétale ou animale caractérisé en ce qu'il comprend une étape dans laquelle la matière grasse est aspirée par un hydro-éjecteur.1. Process for the separation of vegetable or animal fat, characterized in that it comprises a step in which the fat is sucked up by a hydro-ejector. 2. Procédé selon la revendication 1 caractérisé en ce que la matière grasse aspirée par 1 ' hydro-éjecteur est une matière grasse fondue.2. Method according to claim 1 characterized in that the fat aspirated by one hydro-ejector is a melted fat. 3. Procédé selon n'importe laquelle des revendications précédentes caractérisé en ce que la matière grasse et aspirée en continu.3. Method according to any one of the preceding claims, characterized in that the fat is sucked continuously. 4. Procédé selon n'importe laquelle des revendications précédentes caractérisé en ce que le rapport volumique des débits eau/graisse varie entre 2 et 8.4. Method according to any one of the preceding claims, characterized in that the volume ratio of the water / fat flow rates varies between 2 and 8. 5. Procédé selon n'importe laquelle des revendications précédentes caractérisé en ce que la température de l'eau varie entre 1 et 35°, de préférence entre 3 et 15°C.5. Method according to any one of the preceding claims, characterized in that the water temperature varies between 1 and 35 °, preferably between 3 and 15 ° C. 6. Procédé selon n'importe laquelle des revendications précédentes caractérisé en ce qu'il est applicable en continu.6. Method according to any one of the preceding claims, characterized in that it is applicable continuously. 7. Procédé selon n'importe laquelle des revendications précédentes caractérisé en ce que le rapport volumique des débits eau/graisse est d'environ 4. 7. Method according to any one of the preceding claims, characterized in that the volume ratio of the water / fat flow rates is approximately 4. 8. Procédé selon n'importe laquelle des revendications précédentes caractérisé en ce que le mélange eau-graisse est recueilli dans un réacteur et décanté.8. Method according to any one of the preceding claims, characterized in that the water-fat mixture is collected in a reactor and decanted. 9. Procédé selon n'importe laquelle des revendications précédentes caractérisé en ce que la phase supérieure consiste en une suspension cristaux-huile liquide-eau et est séparée puis agité à une température variant de 5 à 20°C durant 1 à 10 heures.9. Method according to any one of the preceding claims, characterized in that the upper phase consists of a crystal-liquid oil-water suspension and is separated and then stirred at a temperature varying from 5 to 20 ° C for 1 to 10 hours. 10. Procédé selon n'importe laquelle des revendications précédentes caractérisé en ce qu'il comprend l'étape supplémentaire de séparation par filtration de ladite phase aqueuse supérieure, la filtration étant de préférence une filtration par membrane, des cristaux contenus dans la phase aqueuse.10. Method according to any one of the preceding claims, characterized in that it comprises the additional step of separation by filtration of said upper aqueous phase, the filtration preferably being a membrane filtration, of the crystals contained in the aqueous phase. 11. Procédé selon la revendication précédente caractérisé en ce que la filtration est effectuée avec une compression, obtenue par une presse, p.e. une presse hydraulique, située entre 2 et 60 bar, de préférence entre 20 et 40 bar.11. Method according to the preceding claim characterized in that the filtration is carried out with compression, obtained by a press, eg a hydraulic press, located between 2 and 60 bar, preferably between 20 and 40 bar. 12. Procédé selon n'importe laquelle des revendications précédentes caractérisé en ce que la graisse est une graisse à haut pourcentage en triglycérides de point de fusion élevée, en particulier le palmiste. 12. Method according to any one of the preceding claims, characterized in that the fat is a fat with a high percentage of triglycerides of high melting point, in particular palm kernel. 13. Procédé de séparation de graisses et huiles végétales ou animales caractérisé en ce que la graisse ou l'huile liquide ou liquéfiée est mise progressivement en contact avec un excès d'eau sous forte agitation et/ou sous forme dispersée. .13. Process for the separation of vegetable or animal fats and oils, characterized in that the liquid or liquefied fat or oil is gradually brought into contact with an excess of water with vigorous stirring and / or in dispersed form. . 14. Procédé de séparation de graisses et huiles végétales ou animales comportant les étapes suivantes : chauffage à une température supérieure au point de fusion de la graisse ou l'huile14. Process for the separation of vegetable or animal fats and oils, comprising the following steps: heating to a temperature above the melting point of the fat or oil - aspiration dans un hydro-éjecteur recueil du mélange résultant dans un réacteur, de préférence thermostatisé et muni d'un agitateur- suction in a hydro-ejector collecting the resulting mixture in a reactor, preferably thermostatically controlled and equipped with an agitator - séparation d'une phase supérieure recyclage d'une phase aqueuse inférieure vers l'alimentation de l'éjecteur ou de la trompe- separation of an upper phase recycling of a lower aqueous phase to the feed to the ejector or the tube - agitation de la phase supérieure séparée pompage de la phase supérieure vers un filtre à membrane- agitation of the separate upper phase pumping of the upper phase to a membrane filter - séparation de l'eau résiduelle résultant du filtrage- separation of residual water resulting from filtering - compactage des cristaux- compacting of crystals - recueils séparés d'une phase liquide organique et d'une fraction solide.- collections separated by an organic liquid phase and a solid fraction. 15. Procédé selon la revendication 2 caractérisé en ce que 1 ' hydroéjecteur est une trompe à eau et l'eau est l'eau débitée par la trompe à eau.15. The method of claim 2 characterized in that one hydroejector is a water pump and the water is the water supplied by the water pump. 16. Procédé de séparation de matière grasse végétale ou animale caractérisé en ce qu'il comprend une étape dans laquelle la matière grasse est violemment éjectée en continu dans un débit d'eau non laminaire pour former une suspension de micro-cristaux dans une phase eau ou huile-eau.16. Process for the separation of vegetable or animal fat, characterized in that it comprises a step in which the fat is violently ejected in continuous in a non-laminar flow of water to form a suspension of micro-crystals in a water or oil-water phase. 17. Procédé selon la revendication 1 caractérisé en ce que la graisse est aspirée par une pompe pour être mise en contact avec le débit d'eau. 17. The method of claim 1 characterized in that the fat is sucked by a pump to be brought into contact with the water flow.
PCT/BE1999/000026 1998-02-19 1999-02-18 Method for producing microcrystals of vegetable and animal fats Ceased WO1999042545A1 (en)

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EP2166072A1 (en) * 2008-07-17 2010-03-24 Contifrac Sprl Method for continuous crystallisation with seeding for body fat
EP1697026A4 (en) * 2003-12-23 2011-06-29 Mi Llc DEVICE AND METHODOLOGY FOR ENHANCED MIXING OF LIQUIDS AND SOLIDS
EP2377505A4 (en) * 2008-12-29 2015-08-05 Evgeny Petrovich Grebennikov Method for producing liposomal drugs and a device for producing a liposome
EP2461898B1 (en) * 2009-08-04 2015-10-07 Solenis Technologies Cayman LP Apparatus, system and method for emulsifying oil and water
CN112138556A (en) * 2020-10-21 2020-12-29 大庆德美特尔能源科技有限公司 Hybrid system for improving solid-liquid-gas mixing performance

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EP0198538A1 (en) * 1985-04-12 1986-10-22 The Procter & Gamble Company Process for preparing pourable solid shortening
JPH03146595A (en) * 1989-11-02 1991-06-21 Noboru Yamada Production of granular solid oil and fat
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1697026A4 (en) * 2003-12-23 2011-06-29 Mi Llc DEVICE AND METHODOLOGY FOR ENHANCED MIXING OF LIQUIDS AND SOLIDS
EP2166072A1 (en) * 2008-07-17 2010-03-24 Contifrac Sprl Method for continuous crystallisation with seeding for body fat
BE1018221A3 (en) * 2008-07-17 2010-07-06 Crystallisation & Degumming Sprl PROCESS FOR CONTINUOUS CRYSTALLIZATION WITH SEEDING FOR BODIES.
EP2377505A4 (en) * 2008-12-29 2015-08-05 Evgeny Petrovich Grebennikov Method for producing liposomal drugs and a device for producing a liposome
EP2461898B1 (en) * 2009-08-04 2015-10-07 Solenis Technologies Cayman LP Apparatus, system and method for emulsifying oil and water
CN112138556A (en) * 2020-10-21 2020-12-29 大庆德美特尔能源科技有限公司 Hybrid system for improving solid-liquid-gas mixing performance

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