Process of esterification
16 claims: 16 independent, 0 dependent
- 1Le temps de séjour dans le réacteur est de 1,15 minute. 7 On détermine le degré d’interestérification par mesure de la dilatation · à 20°C (^20)· Le produit quittant le réacteur tubulaire a une D 20 de plus de 610, ce qui signifie que l’estérification est complète. Le produit - interestérifié est alors débarrassé des résidus de catalyseur par lavage au moyen de 10% en poids d’eau fraîche. Le savon formé au cours de la réaction est éliminé dans un appareil centrifuge et le produit interestérifié est séché par pulvérisation dans une chambre où est entretenue une dépression. EXEMPLE 4 Pour illustrer le fait que le procédé de l’invention peut avantageusement .s’appliquer à l’interestérification continue d’huiles neutralisées, on prépare deux mélanges (a et b) d’huile de palme et • d’huile de coprah prises dans le même rapport pondéral dans l’exemple 3. On sèche les deux mélanges dans les mêmes conditions comme décrit dans l’exemple 3,mais on ne neutralise que le mélange a). Les propriétés les plus importantes du mélange d’huile sont les suivantes:a b teneur en eau 0,01% 0,01% indice d’acide 0,
- 22 2,0 indice de peroxyde 0,8 0,8 dilatation à 20°C 2/0 240 On dose du sodium de manière continue dans chaque mélange d’huiles à l’état solide au moyen de l’appareil que représente la Fig. et on répartit ce sodium au moyen d’un Willemsreactron. On introduit alors les mélanges d’huiles dans un réacteur tubulaire comme indiqué à la Fig. 3· On exécute les réactions d’inter· estérification dans les conditions suivantes:> a. b huile admise,tonnes/heure 6 6 sodium en % 0,05 0,10 sodium en kg/heure 3 6 diamètre du piston d’extrusion en cm 25 25 diamètre des orifices d’extrusion en mm 1,4 1,4 nombre d’orifices d’extrusion 5 5 température du mélange d’huiles en °C 120 120 Le temps de séjour dans le réacteur tubulaire de chacun des mélanges d’huiles est de 2 minutes. Le mélange a) est interestérifié dans l’installation que représente la Fig. 3 pendant 5 jours sans interruption. En raison ds la teneur éLevée en savon di produit formé dans le réacteur tubulaire, l’interestérification du mélange b) est interrompue tous les deux jours pour l’élimination des impuretés du réacteur et des filtres des. pompes. Les échantillons prélevés tout au long des opérations ac35 cusent une dilatation excédant 600, ce qui prouve que les produits ont subi une interestérification totale. On· purifie alors les mélanges d’huiles comme décrit dans l’exemple 3. 1584534 i RE S U Μ Ε La présente invention a pour objet t A) un procédé de préparation de dispersions de métaux alcalins se prêtant au traitement des esters, ce procédé présentant les caractéris— tiques suivantes prises isolément ou en combinaison : 1°) on extrude le métal k travers un orifice d’où il débouche directement dans un liquide de dispersion maintenu à une température supérieure au point de fusion du métal et on répartit le métal fondu intimemenj/ dans le liquide;10, 2°) le wétaÿàlcalin est extrudé dans le liquide dispersé à l'état ! solide de manière à constituer un joint entre le liquide de dispersion et l'alimentation en métal alcalin;
- 33 e ) le métal alcalin est amené à l’état solide par déplacement di ; ;rect du métal solide au moyen d'un piston exerçant sa pression sur le I · 15:îmétal k extruder;1
- 44°) l’alimentation en métal alcalin est constituée par une source de métal alcalin liquide délivrant ce métal sous pression grâce k une 1 pompe k engrenages en vue de l'extrusion;
- 55 e ) le métal alcalii est réparti dans le liquide au moyen d'un ίbroyeur colloïdal;
- 66°) le liquide de dispersion comprend du xylène, du toluène ou une huile minérale;I
- 77°)/lïquide de dispersion comprend une huile de la classe des gly— :I 351 eérides;
- 88°) le métal alcalin est dispersé dans un mélange d'huiles de la ! classe des glycérides dont la teneur en eau est inférieure k 0,05%;
- 99°) l'indice d'acide des huiles de la classe des glycérides est inférieur k 0,3;B) une dispersion de métal alcalin, préparée par le procédé visé sous A;C) un procédé d'interestérification présentant les caractéris tiques suivantes prises isolément ou en combinaison t ί
- 1010°) un mélange d’esters est interestérifié en présence d'un mé;tal alcalin sous la forme d'une dispersion;
- 1111°) l'interestérification est exécutée simultanément avec l'extrusion du métal alcalin ia sity dans le mélange d'esters;D) un procédé d’interestérification continue d'huiles comestibles de la classe des glycérides, en présence d’un métal alcalin, ce procédé présentant les caractéristiques suivantes prises isolément ou en combinaison j
- 1212°) on admet les huiles préchauffées dans un réacteur d’interestérification maintenu k une température de 100 k 275°C et on soutire le produit interestérifié de ce réacteur, la quantité de métal alcalin dans le réacteur étant maintenue k une concentration, exprimée par rapport .. t ' à la quantité totale d'huiles dans le réacteur, qui est au moins équivalente à la concentration totale des poisons du catalyseur dans le mélange huileux, mais qui n'excède pas cette concentration de plus de 0,1%}
- 1313°) le métal alcalin est dissous quasi complètement en une minute} 5;j
- 1414°) la réaotion est exécutée dans un réacteur tubulaire dans le! ' ' quel le débit des huiles de la classe des glycérides à interestérifier ‘est ajusté de manière è. assurer un temps de séjour du mélange dans le réacteur de 1 à 10 minutes}
- 1515 e ) le sodium est dispersé dans le mélange d'huiles dont la tempé10 rature est de 100 à, 140°C}
- 1616°) la réaction est exécutée à une température de 115 à 135°C} E) huiles de la classe des glycérides interestérifiées, obtenues par le procédé visé sous C et denrées alimentaires, y compris les mar:garines contenant de telles huiles'· BREVET N c PL. I - 3 BREVET N° PL. II - 3
Independent claims16
94 paragraphs, as filed
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The present invention relates to methods of interesterification of esters and particularly of edible oils of the glyceride class. The invention also relates to the preparation of dispersions of alkali metals which can be used to promote interesterification processes.
In general, catalytic interesterification, and in particular that of glycerides, can be carried out by means of various catalytic reagents among which mention should be made of hydroxides and alkali metal alcoholates, but the precise nature of the active catalyst for the reaction has not yet been fully elucidated.
Under the usual conditions of interesterification, the catalytic reagents mentioned have a certain number of drawbacks.
Alcoholates, such as sodium methylate and sod ium ethylate lea d to. the formation of methyl and ethyl esters, which results in an increase in losses of products to be interesterified. In addition, these methyl and ethyl esters generally cannot be removed quantitatively during subsequent conventional deodorization processes. Hydroxides, such as scdium hydroxide, have generally been introduced in the form of an aqueous solution, but at current reaction temperatures, use of these compounds leads to considerable losses by saponification of the esters.
It has also been proposed to carry out the interesterification in the presence of an alkali metal dispersed beforehand in an inert liquid, such as a mineral oil or an aromatic hydrocarbon, such. than xylene.
The present invention relates to a process for the preparation of dispersions of alkali metals which are suitable for the interesterification processes. According to the invention, dispersions of alkali metals suitable for treating esters are prepared. extraditing the metal through an orifice from which it emerges directly into a dispersion liquid maintained at a temperature above the melting point of the alkali metal which is distributed uniformly in the liquid.
The dispersions provided by the process of the invention are particularly suitable for promoting the interesterification of mixtures of esters, but they are also suitable for many other processes requiring the presence of dispersions of an alkali metal.
When alkali metals have to be introduced into liquids in metered quantities, there are in principle two possibilities for introducing them by extrusion, namely indirect dosing and direct dosing.
In the case of indirect dosing, a container is used which is completely filled with the alkali metal and which is provided at its top with a closed lid comprising an inlet for the liquid and at its base a calibrated spring valve. The alkali metal is then moved from the container through the calibrated spring valve, by introducing "a metered amount of an inert liquid with a density lower than that of the alkali metal, such as a mineral oil, this inert liquid being taken in an amount equivalent to the amount of alkali metal to pass through the valve. When small quantities of alkali metal, up to 10 kg / hour, have to be metered, the valve opening under the effect of the desired overpressure of atmospheric atmospheres must be very small and it has been found during many experiments that small amounts of oxides or other impurities greatly affect the accuracy of the assay. Sn further, due. static friction and incalculable pulses during the dosing of mineral oil, which can even bring the entire dosing system into resonance, the quantity of alkali metal to be dosed per unit of time is subject to a standard error from $ 24 to $ 65. For this reason, in the process which is the subject of the invention, the alkali metals are preferably brought in by direct displacement by means of a source of pressure mechanically stressed, for example a piston.
When the alkali metal is extruded in the molten state into the dispersion liquid, its very high surface tension causes a significant contraction and the interface of the metal with the liquid forms a very convex meniscus. Consequently, the dispersed liquid, probably due to capillarity, enters the cylinder and can therefore have a detrimental effect on the precision of the metering of the alkali metal.
According to a process which is the subject of the invention, the alkali metal is, for this reason, extradited in the liquid dispersed in the solid state, so as to form a seal between the liquid and the source of alkali metal, after whereby the alkali metal is dispersed in the liquid in the molten state preferably under the effect of shear forces.
Since the alkali metal is solid at the interface with the liquid, a natural seal is formed between this liquid and the extrusion unit, so that the liquid cannot penetrate into the dosing cylinder used for the alkali metal intake. In the metering cylinder, the alkali metal can be brought into the liquid state, but it is preferably brought by direct displacement in the solid state by means of a piston which adapts precisely in the metering cylinder or else, in case the admission takes place in the liquid state, by means of an electromagnetic or rotary pump, especially a gear pump.
When the liquid alkali metals are conveyed by means of a rotary pump, it is important to choose a pump of this kind whose jams do not react with the alkali metal, or else to use a rotary gear pump fitted with metallic seals. 'es.
Regardless of the state in which the alkali metal is brought into the metering cylinder, it is essential, according to a preferred aspect of the invention, that the alkali metal be in the solid state at the point where the cylinder enters the dispersion liquid. When the alkali metal is brought to the liquid state, it must for this reason be cooled at least at the point where it is admitted into the liquid to a temperature below its melting point under pressure prevailing in the system. When the alkali metal is brought to the solid state, the cylinder must be sufficiently thermally insulated, or else provided with a similar cooling device in order to also keep the alkali metal in the solid state at place where it comes into contact with the dispersion liquid.
The alkali metal must be extruded into the dispersion liquid through one or more orifices mounted in the dosing cylinder. ·
Preferably, the solid rod of an alkali metal extruded in the pipe does not extend in a straight line through the latter. The choice of the number and the diameter of the orifices of the metering cylinder must therefore be determined according to the diameter of the pipe in which the alkali metal is metered as well as according to the flow of liquid in this line, metal alca- ;. flax is dispersed more easily · when the holes are narrow than when they are wide.
When the alkali metal is brought to the solid state, the cylinder may have previously been filled with alkali metal in the molten state, the tube being cooled to a temperature below the melting point of the alkali metal before extrusion.
For the execution of continuous processes by the process of the invention, it is therefore preferred to alternately use two or more metering rolls, the alkali metal being introduced continuously into the dispersion liquid from one or more of these metering rolls, while the other cylinder (s) are filled or cooled.
Although the existence of a solid alkali metal in the metering cylinder at the place where this metal comes into contact with the liquid prevents infiltration of any type of dispersion fluid towards the admission of alkali metal, the invention is particularly advantageous when it is necessary to prepare dispersions of an alkali metal in mixtures of esters for an interesterification reaction? .cation, because the natural seal formed by the solid alkali metal also prevents the formation of undesirable reaction products in the cylinder, which would result in a decrease in the effective internal diameter of this cylinder, so that the metering accuracy would be affected. r
The process of the invention can advantageously be applied to the interesterification of a mixture of esters or else of esters and of a f <sup>-</sup> · Or several alcohols. Suitable esters can be derived from higher alcohols such as glycerol, from glycols such as ethylene glycol? col, propylene glycol and polyalkylene glycols, cellulose, sorbitol, mannitol, pentaerythritol and polyvinyl alcohol, or monovalent alcohols, such as methanol, ethanol, propanol / and butanol.<sub>;</sub>.
The acid radicals can be radicals of carboxylic acids of 2 to 26 carbon atoms, both saturated and unsaturated.
By applying the process of the invention, it is possible to interesterify edible oils without appreciable saponification of the glycerides, so that the interesterified products are practically free of by-products.
By oils is meant for the purposes of the invention both the glycerides of fatty acids solid at room temperature and generally called fats or butters as liquid glycerides with <sup>v</sup>'. Room temperature.
The alkali metal can be dispersed in a liquid ...
inert as an aromatic solvent, such as scylene or toluene, and the dispersion can be incorporated into the mixture of esters to be inter-> esterified. Inert liquids can be removed during subsequent deodorization by treatment with live steam. Preferably, however, the alkali metal is dispersed directly in the mixture of esters to be interesterified, the extrusion and interesterification being able to be carried out simultaneously.
According to a preferred aspect of the invention, an alkali metal dispersion is prepared in situ by extruding the metal into the mixture of esters maintained under the interesterification conditions.
The alkali metal is preferably added to the mixture to be interesterified in an amount equal to or greater than that consumed by
I the poisons of the catalyst, so that the presence in the mixture to be interester of the poisons or catalyst is compensated for by an equivalent amount to the alkali metal, expressed in equivalent grams. Many substances can be catalyst poisons, for example water, fatty acids and peroxides, but these poisons have in common a tendency to combine with the alkali metal into a substance which is catalytically inert or only slightly active under the reaction conditions. Following numerous experiments, it has been discovered that for the interesterification of edible oils, water should not be considered as a poison of the catalyst if it is present in an amount less than 0.01%. In addition, metal soaps should be considered to be catalytically inert at a reaction temperature below 180 ° C.<sub>;</sub>
Before being admitted to the reactor, the mixture of oils and alkali metals must be subjected to intense shearing to form a microdispersion of the catalytic reagent in the oil.
It has been found that the reaction can be carried out in the presence of optimal amounts of catalytic reactants when the alkali metals are dispersed with such violence that at the reaction temperature they dissolve in 1 minute and preferably in 20 seconds. A particularly suitable device for the formation of dispersions is a colloid mill which is known under the name of Willensreactron and which is described in particular in the patent of the German Federal Republic No. 1,152,003 "
The interesterification can be carried out, for example, in a number of cascaded agitator tanks, but preferably in a tubular reactor.
Depending on the concentration of the catalyst, the reaction temperature and the nature of the mixture to be treated, the interification can be completed in 1 to 10 minutes. On leaving the reactor, the reaction product is freed from any hydrogen which may have formed, then soaps and the components of the catalyst by vigorous stirring<sub>t</sub>with 5 to 30% by weight of water, after which the aqueous phase is separated from the reaction product. .
Completely or partially interesterified products can be prepared by acting on the residence time in the reactor and on the quantity of active catalyst used.
The degree of interesterification of a mixture of edible oils can be measured for example by dilatometry. For example, for a mixture of palm oil and coconut oil, the expansion to 20 ° C, represented by the symbol ï'20 '<sup>idiots</sup>^ i '<sup>kill</sup> an appropriate measure of the degree of interesterification. The expansion is determined as described in Analysis and characterization of oils, fats and fat products,
HA Boekenoogen, 1964, Interscience Publishers, London, pages I43 et seq.
The interesterification can be carried out at any temperature. at which the catalyst is formed in situ with sufficient activity, temperatures of 100 to 275 ° C being suitable. The temperature chosen depends on the nature of the catalyst and the properties of the mixture to be interesterified, but is higher than the melting point of the alkali metal.
. Good results have been obtained using sodium at temperatures of 100 to 140 ° C and preferably 115 to 135 ° C.
For the interesterification of the glycerides, esters are treated from which, according to the invention, at least most of the poisons of the catalyst present are eliminated beforehand, because the amount of alkali metal necessary for the interesterification depends very much the quantity of catalyst poisons present in the oil On the other hand, the use of larger quantities of alkali metal, to compensate for the presence of significant quantities of catalyst poisons, leads to excessive soap formation which can result in an unacceptably high viscosity of the oil / soap mixture, clogging of the filters with a soap gel, the formation of soap on the internal walls of the reactor and a considerable reduction in lt. reaction rate. Thus, when interesterifying a crude oil mixture having an acid number of 2 to 3 and a water content exceeding 0.05%, a quantity of sodium of at least 0.3% is necessary and can lead to these undesirable results. Since water and free acids are the main poisons of the catalyst, it is therefore preferred to carefully neutralize the mixture to be interesterified and reduce its water content to a value less than 0.05% and preferably 0.03 %.
When using deacidification by distillation, drying can be carried out in various ways common in the edible oil industry and additional drying is usually not necessary for the purposes of the invention. Alternatively, the mixture can be dried at an elevated temperature using an inert gas. However, heating is usually carried out by means of an apparatus which maintains, under reduced pressure, for example from 10 to 50 mm Hg and at an elevated temperature, for example from 100 to 140 ° C, the heated mixture of esters which is atomized at the top of a chamber of the device in which a vacuum is maintained allowing the rapid evaporation of most of the water present. The operation can, if desired, be carried out in two or more stages. It has been found that good results are obtained by means of a two-stage vacuum drying apparatus operating at pressures of and ae 10 ma Hg respectively for an oil admitted at a temperature of 125 to 140 ° C.
The temperature of the medium to be sprayed and the value of the vacuum are chosen so that the product to be interesterified reaches -.
the required moisture content, which is less than $ 0.05 by weight. ...
Oils subject to interesterification are preferably deacidified to an acid number of less than 0.3. By "acid number" is meant the number of mg of potassium hydroxide necessary to neutralize 1 g of the mixture to be interesterified. This acidity is determined according to the method described by HABoekenoogen / in Analysis and characterization of oils, fats and fat products,? volume I, 1964, Interscience'Publishers, London, pages 23-24 · Since> 'this determination is carried out briefly at room temperature, the esters are not saponified, so that an acid index of 0 corresponds the absence of free acids. The mixture to be interesterified ·· 'can be deacidified by means of a vacuum distillation process, but this operation can also be carried out by direct contact with (¾ ··. An alkaline solution, which forms soaps which can be separated due to the difference in density between the oil and the sa->.
see. Such deacidification with an alkali can be carried out with P l using a 0.2 to SN sodium hydroxide solution.
The deacidification can be carried out continuously in a centrifugal device which provides brief contact between the oil and the alkaline solution. In addition, continuous deacidification can also be carried out by rapid mixing of the product with the alkaline solution, then washing of the mixture in a packed column. However, the //; deacidification is preferably carried out by passing the oil through a column packed with current in the same direction or in the opposite direction to that of; / the alkaline solution, if necessary under high pressure and at a temperature of 80 to 160 ° C., the oil constituting the dispersed phase. These deacidification processes are described in the patent applications î / - 'Dutch n ° 6503471 and 6603470.' #
The process of the invention is described below with reference to the accompanying drawings in which: <sup>S;</sup>
Fig · 1 illustrates a process for preparing dispersions of an alkali metal in which the alkali metal is brought to the liquid state • and then solidified before coming into contact with the fluid;
Fig. 2 shows a metering device for alkali metal // · in which the alkali metal is admitted in the solid state; \
Fig. 3 shows a table of a continuous interesterification process in an apparatus where the process which is the subject of the invention is applied.
L ·.
1004584
In Fig. 1, a tank 1 for the liquid alkali metal is provided with an external heating jacket 2. The contents of the container are heated beyond the melting point of the alkali metal by means of a heat exchanger medium admitted at 3 and racked in 4 ·
The liquid alkali metal 5 is covered with a layer of paraffin oil 6 which prevents its oxidation.
Through the valve 8, the pipe 7 and the rotary gear pump 9, the alkali metal is brought into the metering cylinder 12.
* The flow rate of alkali metal is adjusted by means of a variator 10 connected to an electric motor 11 and to the gear pump 9..
The metering cylinder I2 is provided with a heat exchanger 13 which a cooling medium passes through at a temperature such that its passage from the inlet 14 to the outlet 15 causes the alkali metal to solidify in the part of the metering cylinder passing through the exchanger 13.
Leaving the metering cylinder, the alkali metal enters line 16 from ds in which a preheated dispersion liquid is pumped and brought from the reservoir 17 equipped with heating devices (not shown) via the valve 18 and by means of the pump 19 The mixture of alkali metal and dispersion liquid '' kept at a temperature higher than the melting point of the metal. /icalin is then transferred to the colloid mill 20 in which the alkali metal is distributed in the dispersion liquid. The dispersed f'-rmée can via line 16 be introduced into containers or be brought continuously a process where it is required.
Instead of feeding the alkali metal in the liquid state by means of a rotary pump as shown in Fig. 1, this operation can be carried out in the solid state by means of an apparatus such as that shown in FIG. 2.
The dosing cylinder 21 is connected at 29 by bolts (not shown) and by a packing ring 28 to the cylinder head 22.
The metering cylinder 21 is provided with a piston 23 actuated hydraulically or mechanically.
The drive mechanism is not shown.
The cylinder head 22 constituting a part of the metering cylinder 21 is provided with an orifice 25 through which the solid alkali metal contained in the tube 24 can be extruded by means of the piston 23 into the liquid flowing in the pipe 26. The line 26 is fitted with equipment similar to that described above, for example a pump and a colloid mill, as shown in FIG. 1 in the case of line 16.
The cylinder head 22 is also equipped with a cooling jacket 27 to prevent the alkali metal from melting inside the orifice 25.
A continuous interesterification process carried out according to the invention is described below with reference to FIG. 3.
An interesterified mixture is introduced at 31 by a pump 32 and brought via a heat exchanger 33, where it is preheated to a temperature of 125-140 ° C, in a vacuum drying apparatus 34 where it is sprayed using a spray head
35. The vacuum drying apparatus 34 is connected at 36 to a vacuum installation (not shown) which makes it possible to maintain a pressure of 10 to 50 mm of Hg in the drying apparatus. The mixture thus brought to a moisture content of less than 0.05% by weight is brought by the spring 37 to the reactor 41. Before the Product to be interested15 to enter the reactor, the required quantity of metal, alkali at 38, is added, this metal being finely distributed in the mixture by a colloidal mill 39 · The mixture then descends into the tubular reactor 41 fitted with thermal insulation and a 4θ heating coil to keep the temperature at the required value. The residence time in the reactor can be adjusted to a value of 1 to 10 minutes by modifying the flow rate of the liquid. The prodvi, -. The esterified jiter is then mixed in the mixer 43 with 5 to 30% by weight of water admitted at 42, with a view to extraction by washing of the soaps formed and of the residues of the catalyst. In the centrifugal device 44 the undesirable by-products are extracted at 45, while the interesterified product ^ is sprayed via the spray head 47 in the drying device 46 which is connected at 48 to a plant for empty. The drying apparatus 46 can be maintained under a pressure of 45 mm of Hg so that the interesterified product is dried to a water content of 1 to 0.1% by weight. The purified and dried interesterified product is then extracted by the pump 49 from the spraying chamber.
The process of the invention is further illustrated by the examples below.
EXAMPLE 1 Lithium dispersions are prepared using, inter alia, the apparatus shown in FIG. 1.
Lithium melting is first heated to T80 ° C under a film of light mineral oil at a temperature of 200 ° C and, by means of a rotary gear pump with a capacity of 220 g / hour, leads to a metering cylinder, the orifice of which opens directly into a shot-blasting bowl.
ίο
The blasting bowl is provided with a heating jacket with a rotating comb for the distribution of lithium under the effect of; rr. these high shear and continuous and metered mineral oil intake devices into the bowl as well as an outlet device for the dispersion of prepared lithium · ·
At the point where the lithium first comes into contact with the oil, the metering cylinder is cooled to a temperature of 50 to 150 ° C.
"The lithium entering the shot-blasting bowl is left in mineral oil at a temperature of 210 to 230 ° C. A good quality product is obtained in which the lithium has a particle size of 15 to 50 microns, when the lithium and the oil are admitted continuously in a weight ratio of 1: 3, the flow rates of lithium and of mineral oil being set so that the average day time is 10 minutes.
EXAMPLE 2. A sodium dispersion is formed in xylene by bringing in liquid sodium, melting at about 98 ° C in a metering cylinder by means of the same rotary gear pump as that of Example 1 and as illustrated in FIG. 1.
The sodium reservoir, the rotary pump and most of the metering cylinder are maintained at a temperature of 105 to 110 ° C.
The dosing cylinder opens directly into a line where xylene flows and is · perpendicular to this line.
The end of the dosing cylinder is cooled to 50-80 ° C just before the place where the sodium comes into contact with the xylene.
The extruded sodium as well as the xylene stream, taken in a weight ratio 1: 3, are admitted continuously at 105-110 ° C in a colloid mill where the sodium is distributed in the xylene.
The product leaving the colloid mill is cooled to room temperature and is packaged in containers or carried out in a process for which a sodium dispersion is necessary for catalytic purposes.
EXAMPLE 3 - ~
This example illustrates the interesterification of a mixture
60:40 palm oil and coconut oil in an installation of the type shown in FIG. 3. Before mixing the oils, they are neutralized using a 0.8N sodium hydroxide solution, then dried by spraying in a chamber where a vacuum of 10 mm Hg is maintained at a temperature of 125 ° C.
The oils are then mixed. -,
The most important properties of the mixture of oils formed are as follows: <sup>vs</sup> ·
Water content: 0.008%
Acid number: 0.13
Peroxide index: 0.8
Expansion at 20 ° C: 240
The mixture of oils is pumped into the apparatus at the rate of 390 kg / hour and the sodium in this mixture is metered by means of the apparatus which is shown in FIG. 2 at a rate of 0.072 kg / hour, that is to say at a rate of 0.0184% by weight.
The amount of sodium introduced, expressed in relation to the total of oils, exceeds the equivalent amount of catalyst poisons by 0.0017 "
The sodium is extruded by means of an extruder fitted with a piston 40 mm in diameter and a die 2 mm in diameter under a pressure of approximately 150 kg / cm 2.
The extruder is sufficiently insulated to keep all of the sodium in a solid state.
The sodium is then distributed in the oil mixture by means of a Willemsreactron type TDLE 3/55 provided with rotors with a diameter of 10 cm arranged at a distance of 2 mm and rotating at the speed of 2910 revolutions / minute. After an average residence time of 4 seconds in this type of colloi d mill, no more s odium particles in dispersion can be detected with the naked eye, which probably means that the fineness of the dispersion is such that the surface sodium is increased to such an extent that the active catalyst is instantly prepared / (· prepared. / l.
The resulting mixture is introduced continuously r into a tubular reactor. . ?
3 sheets
Sheet 1 Sheet 2 Sheet 3
Every citation, both ways
| Document | Relation | Office | Cited during |
|---|---|---|---|
| WO9204117A1 | Cited by | World Intellectual Property Organization (WIPO) | International search |
| US5124301A | Cited by | United States of America | Search report |
17 members in 14 offices
Priority claims2
| Document | Office | Kind | Date |
|---|---|---|---|
| 54108 | Luxembourg | A | |
| 54108 | Luxembourg | A |
Members17
| Document | Office | Kind | |
|---|---|---|---|
| BE718013A | Belgium | A | |
| NL6809796A | Netherlands (Kingdom of the) | A | |
| LU54108A1 | Luxembourg | A1 | |
| ES356091A1 | Spain | A1 | |
| FR1584584AThis record | France | A | |
| AT289143B | Austria | B | |
| GB1236233A | United Kingdom | A | |
| DE1792011A1 | Germany | A1 | |
| IT949223B | Italy | B | |
| NO128022B | Norway | B | |
| SE362069B | Sweden | B | |
| CA943942A | Canada | A | |
| US3852315A | United States of America | A | |
| DE1792011B2 | Germany | B2 | |
| JPS5235684B1 | Japan | B1 | |
| NL157647B | Netherlands (Kingdom of the) | B | |
| DE1792011C3 | Germany | C3 |
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Numbers
- Publication
- 1584584
- Application
- 1584584
Classification
- IPC, 6
- B01J2 06
- B01J2 20
- B01J13 00
- B01J23 00
- B22F9 06
- C11C3 10
