EP0535475A2 - Stoffgemischfraktionierung - Google Patents

Stoffgemischfraktionierung Download PDF

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Publication number
EP0535475A2
EP0535475A2 EP92116057A EP92116057A EP0535475A2 EP 0535475 A2 EP0535475 A2 EP 0535475A2 EP 92116057 A EP92116057 A EP 92116057A EP 92116057 A EP92116057 A EP 92116057A EP 0535475 A2 EP0535475 A2 EP 0535475A2
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EP
European Patent Office
Prior art keywords
mixture
substances
crystal
maximum
cooling medium
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.)
Withdrawn
Application number
EP92116057A
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German (de)
English (en)
French (fr)
Other versions
EP0535475A3 (enrdf_load_stackoverflow
Inventor
Werner Dr.-Ing. Sitzmann
Thomas Dipl.-Ing. Willner
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SIG Plastics GmbH and Co KG
Original Assignee
Krupp Maschinentechnik GmbH
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Filing date
Publication date
Application filed by Krupp Maschinentechnik GmbH filed Critical Krupp Maschinentechnik GmbH
Publication of EP0535475A2 publication Critical patent/EP0535475A2/de
Publication of EP0535475A3 publication Critical patent/EP0535475A3/xx
Withdrawn legal-status Critical Current

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    • 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
    • C11B7/0075—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils by differences of melting or solidifying points

Definitions

  • the invention relates to a process for the fractionation of meltable, high molecular weight, organic substance mixtures, such as e.g. Fats and oils, di- and triglycerides, fatty acids and waxes and higher hydrocarbons by crystallization in the melt and subsequent separation of the crystal-containing suspension into a solid and a liquid fraction, e.g. a stearin fraction and a liquid olein fraction and on a plant for carrying out the process.
  • meltable, high molecular weight, organic substance mixtures such as e.g. Fats and oils, di- and triglycerides, fatty acids and waxes and higher hydrocarbons
  • Solvent fractionation is suitable for the production of all types of cocoa butter substitutes and generally delivers very good product qualities.
  • the selectivity is to be improved by interactions of the solvent with the triglycerides.
  • the wetting agent fractionation generally gives poor CBR qualities with the exception of cocoa butter substitute (CBS) production based on palm kernel oil (PKO). It is also well suited for the first stage of palm oil fractionation (palm oil production).
  • CBS cocoa butter substitute
  • PKO palm kernel oil
  • the wetting agent fractionation Compared to the dry fractionation, the wetting agent fractionation, apart from the fact that there is no fire risk and the crystallization temperatures are changed only slightly, has the same basic disadvantages as the solvent fractionation.
  • FR 2 369 800 The purpose of the process described in FR 2 369 800 is, starting from palm oil with an iodine number of 50-55, to produce a substitute which is partially miscible with cocoa butter by means of a two-stage conventional dry fractionation, carried out in stirred crystallizers, as the palm middle fraction.
  • CH 658 163 A5 describes a dry fractionation process in which a palm middle fraction of iodine number 36-38 is generated by two-stage fractionation, starting from palm oil.
  • GB 2 220 672 A explicitly points out that the method described there is not suitable for processing lauric fats, since lauric fats form crystal suspensions which, after substep 2), cannot be converted into a pumpable consistency by comminution.
  • Step 1) serves to eliminate the thermal history of any undesired crystals that may be present.
  • Step 2) is used either only for pre-cooling of the material, the actual nucleation taking place in step 3), or both for pre-cooling and for crystal nucleation.
  • step 2) is only used for pre-cooling, this is expediently carried out in a stirred tank or in a heat exchanger. It is important that the temperatures of the cooling surface do not fall significantly below the nucleation temperatures, since otherwise crystals of undesired modification can form on the cooling surfaces. Apart from this limit condition, step 2) can be carried out as quickly as desired in this case by measures to improve the heat transfer.
  • step 2 If both the precooling and the nucleation are carried out in step 2), this must be done in such a way that defined heat transfer ratios are set for the controlled formation of crystal nuclei with a high degree of order.
  • the temperature difference between the interior of the substance mixture to be processed and the cooling medium is preferably limited to a maximum of 5 ° C., the specific heat flow from the substance mixture into the cooling medium being preferably limited to a maximum of 5 W / kg substance mixture as an additional condition.
  • step 2 Carrying out pre-cooling and nucleation in step 2) increases the duration of this process step, but shortens the duration of step 3).
  • the duration of step 3) is extended accordingly if only pre-cooling takes place in step 2).
  • the optimal one The procedure depends on the product. According to the invention, both variants are available.
  • step 3 the crystals are ripened, either after the nucleation, if this was carried out in step 2), or together with the nucleation, if step 2) was only used for pre-cooling.
  • crystallization with a stearance content of the suspension above about 30% is difficult or impossible to carry out in stirred crystallizers due to the high viscosities.
  • the manufacture e.g. of cocoa butter substitutes due to the dry fractionation based on palm oil and palm kernel oil, however, there is necessarily a stearing content of more than 30%. For this reason, such crystallization processes are carried out in such a way that the material to be crystallized is poured out in flat layers and allowed to crystallize out in a non-stirred state, that is to say at rest.
  • the crystals resulting from such tempering are of moderate pressure stability, generally have a reduced ß-crystal content and are not suitable for high-pressure press filtration at pressures of the order of 50 bar.
  • the temperature difference between the interior of the substance mixture and the cooling medium is preferably limited to a maximum of 2 ° C., the specific heat flow from the substance mixture into the cooling medium being preferably limited to a maximum of 0.5 W / kg of substance mixture as an additional condition.
  • stage 2 the temperature difference between the interior of the mixture of substances and the cooling medium is increased, but preferably remains limited to a maximum of 5 ° C., the specific heat flow from the mixture of substances into the cooling medium preferably being limited to a maximum of 2 W / kg of mixture of substances.
  • the heat dissipation can be implemented in two variants:
  • step 3 In contrast to step 2), ie the moving pre-crystallization, for example in the stirred tank, it is surprisingly found in static crystallization in step 3) that the entry of certain, approximately constant shear rates is advantageous, but the entry of approximately constant shear stresses.
  • the shear stress is the mathematical product of dynamic toughness and shear rate.
  • these shear shear stresses should be dimensioned such that as crystallization proceeds and the viscosity of the medium increases, the specific one Energy input remains so low that there is no mechanical or thermal disturbance of the crystal formation.
  • the shear forces introduced should be such that the shear rates decrease towards zero with increasing viscosity in the final phase of crystallization. Such conditions can be realized, for example, by means of a rake moved through the material mixture with low driving forces.
  • step 4 the crystal suspension matured in step 3) is transferred gently into the filtration unit.
  • the procedure according to the invention in steps 2) and 3) results in a material consistency despite high stearing contents of 30% and more, which in the case of non-lauric or slightly lauric as well as in the case of lauric and hardened fats leads to problem-free conveying of the substance mixture through pipes without special mechanical pretreatment.
  • This broad applicability of the method according to the invention and this simple handling of the mature material is a decisive advantage over the procedure described in patent application GB 2 220 672 A, which requires a physical breakup of the crystallized material and is not applicable to lauric fats.
  • step 5 the mixture of substances introduced into the filtration unit is mechanically separated into a liquid phase (olein) and a solid phase (stearin).
  • Carrying out step 5) according to the invention requires press filtration, for example carried out in a membrane filter press, at press pressures which e.g. in the case of the production of palm middle fraction or palm kernel stearin, preferably between 45 and 70 bar.
  • the procedure according to the invention is not only based on the fractionation of fats and oils, but also on the fractionation of numerous other meltable, high molecular weight, organic substance mixtures, such as e.g. Mono-, di- and triglycerides, fatty acids and waxes and higher hydrocarbons can be used. From the broad field of application, only two examples are given here: the de-oiling of mixtures of substances that occur during paraffin or paraffin grease processing, and the separation of glycerol from mixtures of substances that arise during the enzymatic production of monoglycerides.
  • crystal ripening can be influenced to a certain extent by inoculation if the seed crystals of the desired crystal form are added in a low concentration during the nucleation phase.
  • the improvement effect of vaccination is comparative low, since the crystals produced according to the invention are of very good quality even without vaccination.
  • the terms used here are to be understood as follows:
  • the temperature at the start of crystallization also called the crystallization temperature, is understood here to mean the temperature at which the first visible crystals are formed or a first turbidity of the material is visible.
  • the temperature at the start of crystallization is synonymous with the beginning of the process phase of crystal ripening.
  • the crystal ripening phase is understood here to mean that temperature range which is below the temperature at the start of crystallization. It is synonymous with the phase of crystal growth.
  • the temperature range of the nucleation phase also called the nucleation phase, is understood to be the temperature range within which the material is optically clear, ie no crystals are visible to the eye, but very small crystal nuclei are formed.
  • Evidence of the nucleation phase is usually successful if comparative tests are carried out at different cooling temperatures and it is found that the crystals that become visible later mature differently, even if they are subjected to completely identical conditions after they become visible. From a certain minimum size, crystal nuclei can also be detected microscopically.
  • the nucleation temperature here means the upper temperature limit of the crystal nucleation phase.
  • the pre-cooling phase is the temperature range above the nucleation phase.
  • the shear rate in a process container with moving built-in parts is understood here to mean the mathematical quotient, formed from the speed of the respective moving built-in part in the numerator and the distance to the nearest fixed built-in part, possibly to the container wall or to the container bottom, in the denominator.
  • the specific heat flow Q from the mixture of substances into the cooling medium, specified in W / kg of mixture of substances, in words Watts per kilogram of mixture of substances, is determined in a time period t from the change in temperature T, below which is the difference between the average material temperature at the beginning and at the end of each understood period of time, and the specific heat capacity C of the material, specified in J / (kg ° C), in words Joule per kilogram of substance mixture and degrees Celsius temperature change (for fats, for example, it is known that here about 2150 J / (kg ° C) ), as well as the increase in crystal content X in the time period t, given in kg crystal per kg substance mixture, and the latent specific heat of crystallization H released, given in J / kg crystal (for fat crystals, for example, it is known to be of the order of 100,000 to 200,000 J / kg), using the following formula:
  • the following examples serve to illustrate the procedure according to the invention and are not to be understood as a limitation of the invention.
  • a stearin with an increased POP content and a double-fractionated palmolein with a high iodine number are produced according to the following variant of the fractionation process according to the invention:
  • the palm olein is heated to 70 ° C. in a stirred kettle in accordance with step 1).
  • the material is then cooled down as quickly as possible to 30-35 ° C during the pre-cooling phase at an increased stirrer speed of over 40 revolutions per minute.
  • a liquid cooling medium in this example water, is used. The temperature of the cooling medium must not fall significantly below the nucleation temperature of 19-29 ° C.
  • the subsequent phase of nucleation within the stirred tank is initiated by reducing the stirrer speed in such a way that shear rates of 10 l / s are not exceeded. In the present case, this corresponds to a stirrer speed of 11 revolutions per minute.
  • the further cooling of the oil is controlled by regulating the temperature difference between the cooling medium and oil in such a way that the specific heat flow from the initial oil temperature of 30-35 ° C to the crystallization temperature of 14-20 ° C is approximately linear in time from about 4. 0 to about 0.2 W / kg of oil reduced.
  • the Coolant flow is 5 - 15 l / min.
  • the heat transfer conditions in the stirred tank are designed so that a temperature difference between the cooling medium and the oil of 0.5 ° C is not exceeded at the end of the nucleation phase.
  • the still free-flowing suspension is poured into a stainless steel trough in which the ripening of the crystals is carried out in accordance with step 3).
  • the fill level of the material is 45 mm in the present example. This filling level is chosen such that it is ensured during the entire ripening process that the temperature difference between the respective maximum temperature in the material and the surface temperature of the material does not exceed 3 ° C.
  • air is used as the cooling medium, which flows around the tub on all sides.
  • the further cooling of the oil is achieved by regulating the temperature difference between the cooling medium and the oil in such a way that the specific heat flow increases approximately linearly from about 0.2 to about 1.0 W / kg of oil within the first 5 hours of crystal ripening.
  • the heat flow is then kept at about 1.0 W / kg until the end of crystallization.
  • the cooling air flow is about 200 m3 / h.
  • the heat transfer conditions are designed so that a maximum temperature difference of 5 ° C is not exceeded between the interior of the crystallizing material layer and the cooling air.
  • the crystal ripening phase is ended by transferring the suspension into the filtration unit immediately after reaching a desired iodine number of 69 in the liquid residual oil still between the crystals, the so-called oleic phase.
  • test filtrations of suspension samples are carried out during crystal ripening.
  • the liquid phase is pressed through a filter fabric, in which, in the present case, the filter chamber is subjected to a slowly increasing pressing pressure, applied by means of a mechanical volume reduction of the filter chamber, within 45 minutes.
  • the final filtration pressure is 55 bar.
  • Example 12 kg of the stearin obtained in Example 1 are subjected to the dry fractionation process according to the invention for producing a palm middle fraction with a particularly steep melting curve:
  • the material is heated to 70 ° C. in a stirred kettle in accordance with step 1).
  • the material is then cooled as quickly as possible to 35-40 ° C during the pre-cooling phase at an increased stirrer speed of over 40 revolutions per minute.
  • a liquid cooling medium in this example water, is used.
  • the temperature of the cooling medium must not fall significantly below the nucleation temperature of 27-35 ° C.
  • the subsequent phase of nucleation within the stirred tank is initiated by reducing the Stirrer speed in such a way that shear speeds of 10 1 / s are not exceeded. In the present case, this corresponds to a stirrer speed of 11 revolutions per minute.
  • the further cooling of the oil is achieved by regulating the temperature difference between the cooling medium and the oil in such a way that the specific heat flow from the initial oil temperature of 35-40 ° C to the crystallization temperature of approximately 22-28 ° C is approximately linear in time from 3. 2 to 0.2 W / kg oil reduced.
  • the cooling medium flow is 5 - 15 l / min.
  • the heat transfer conditions in the stirred tank are designed so that a temperature difference between the cooling medium and the oil of 0.5 ° C is not exceeded at the end of the nucleation phase.
  • the still free-flowing suspension is poured into a stainless steel trough in which the crystals are ripened in accordance with step 3.
  • the fill level of the material is 45 mm in the present example. This filling level is selected such that it is ensured during the entire ripening process that the temperature difference between the respective maximum temperature in the material and the surface temperature of the material does not exceed 3 ° C.
  • air is used as the cooling medium, which flows around the tub on all sides.
  • the further cooling of the oil is achieved by regulating the temperature difference between the cooling medium and the oil in such a way that the specific heat flow increases approximately linearly from about 0.2 to about 1.0 W / kg of oil within the first 5 hours of crystal ripening.
  • the heat flow is then kept at about 1.0 W / kg until the end of crystallization.
  • the cooling air flow is about 200 m3 / h.
  • the Heat transfer conditions are designed so that a maximum temperature difference of 5 ° C is not exceeded between the interior of the crystallizing material layer and the cooling air.
  • the crystal ripening phase is terminated by transferring the suspension into the filtration unit immediately after reaching a desired iodine number of 50 in the liquid residual oil still between the crystals, the so-called oleic phase.
  • test filtrations of suspension samples are carried out during crystal ripening.
  • the liquid phase is pressed through a filter fabric, in which, in the present case, the filter chamber is subjected to a slowly increasing pressure, applied within 45 minutes, by means of a mechanical volume reduction of the filter chamber.
  • the final filtration pressure is 60 bar.
  • a palm kernel stearin with a particularly low iodine number and a palm kernel oil with a relatively high iodine number are obtained by the following variant of the fractionation process according to the invention.
  • the palm kernel oil is heated up to 60 ° C. in a stirred kettle in accordance with step 1).
  • the material is then cooled as quickly as possible to 32-37 ° C during the pre-cooling phase at an increased stirrer speed of over 40 revolutions per minute.
  • a liquid cooling medium in this example water, is used. The temperature of the cooling medium must not fall significantly below the nucleation temperature of 26-32 ° C.
  • the subsequent phase of nucleation within the stirred tank is initiated by reducing the stirrer speed in such a way that shear rates of 10 l / s are not exceeded. In the present case, this corresponds to a stirrer speed of 11 revolutions per minute.
  • the further cooling of the oil is achieved by regulating the temperature difference between the cooling medium and the oil in such a way that the specific heat flow from the initial oil temperature of 32-37 ° C to the crystallization temperature of 22-28 ° C is approximately linear in time over about 2. 8 to about 0.2 W / kg of oil reduced.
  • the cooling medium flow is 5 - 15 l / min.
  • the heat transfer conditions in the stirred tank are designed so that a temperature difference between the cooling medium and the oil of 0.5 ° C is not exceeded at the end of the nucleation phase.
  • the still free-flowing suspension is poured into a stainless steel trough in which the ripening of the crystals is carried out in accordance with step 3).
  • the fill level of the material is 41 mm in the present example. This fill level is chosen such that during the entire ripening process it is ensured that the temperature difference between the respective maximum temperature in the material and the surface temperature of the material does not exceed 3 ° C.
  • air is used as the cooling medium, which flows around the tub on all sides.
  • the further cooling of the oil is achieved by regulating the temperature difference between the cooling medium and oil in such a way that the specific heat flow increases approximately linearly in time from about 0.2 to about 1.1 W / kg of oil within the first 4 hours of crystal ripening.
  • the heat flow is then kept at about 1.1 W / kg until the end of crystallization.
  • the cooling air flow is about 200 m3 / h.
  • the heat transfer conditions are designed so that a maximum temperature difference of 5 ° C is not exceeded between the interior of the crystallizing material layer and the cooling air.
  • the crystal ripening phase is ended by transferring the suspension into the filtration unit immediately after reaching a desired iodine number of 26 of the liquid residual oil still between the crystals, the so-called oleic phase.
  • test filtrations of suspension samples are carried out during crystal ripening.
  • the liquid phase is pressed through a filter fabric, in which, in the present case, the filter chamber is subjected to a slowly increasing pressing pressure, applied by mechanical volume reduction of the filter chamber, within 60 minutes.
  • the final filtration pressure is 70 bar.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Fats And Perfumes (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
EP92116057A 1991-10-04 1992-09-19 Stoffgemischfraktionierung Withdrawn EP0535475A2 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4132892 1991-10-04
DE4132892A DE4132892A1 (de) 1991-10-04 1991-10-04 Stoffgemischfraktionierung

Publications (2)

Publication Number Publication Date
EP0535475A2 true EP0535475A2 (de) 1993-04-07
EP0535475A3 EP0535475A3 (enrdf_load_stackoverflow) 1994-08-03

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EP92116057A Withdrawn EP0535475A2 (de) 1991-10-04 1992-09-19 Stoffgemischfraktionierung

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US (1) US5401867A (enrdf_load_stackoverflow)
EP (1) EP0535475A2 (enrdf_load_stackoverflow)
DE (1) DE4132892A1 (enrdf_load_stackoverflow)
MY (1) MY115127A (enrdf_load_stackoverflow)

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WO1996005279A1 (en) * 1994-08-17 1996-02-22 Quest International B.V. Oil modification
US5602265A (en) * 1993-07-27 1997-02-11 Van Den Bergh Foods Co., Division Of Conopco, Inc. Fractionation of triglyceride oils

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JP3718113B2 (ja) 2000-07-13 2005-11-16 花王株式会社 油脂組成物の固液分別法
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US7618670B2 (en) * 2004-06-14 2009-11-17 Premium Vegetable Oils Sdn. Bhd. Trans free non-hydrogenated hard structural fat and non-hydrogenated hard palm oil fraction component
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EP1818088A1 (en) * 2006-01-20 2007-08-15 De Smet Engineering N.V. Crystallisers useful in fractionation processes for oils and fats
EP1905815A1 (en) * 2006-09-28 2008-04-02 De Smet Engineering S.A. Phase transfer apparatus and process
EP2028258A1 (en) * 2007-08-01 2009-02-25 N.V. Desmet Ballestra Engineering S.A. Process for equipment for desolventising under reduced pressure
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MY184018A (en) * 2014-12-03 2021-03-17 Sime Darby Plantation Intellectual Property Sdn Bhd Continuous process for dry fractionation of glyceride oils
BR102018011321A2 (pt) * 2018-06-04 2019-12-03 Univ Estadual Campinas Unicamp processo de fabricação de bases lipídicas, bases lipídicas e uso das mesmas

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5602265A (en) * 1993-07-27 1997-02-11 Van Den Bergh Foods Co., Division Of Conopco, Inc. Fractionation of triglyceride oils
WO1996005279A1 (en) * 1994-08-17 1996-02-22 Quest International B.V. Oil modification
US5874599A (en) * 1994-08-17 1999-02-23 Loders Croklaan B.V. Dry fractionation of fat molecules in a pseudo-steady state
AU702761B2 (en) * 1994-08-17 1999-03-04 Unilever Plc Oil modification

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EP0535475A3 (enrdf_load_stackoverflow) 1994-08-03
US5401867A (en) 1995-03-28
DE4132892A1 (de) 1993-04-22
MY115127A (en) 2003-04-30

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