CN105462685A - Oil fractionation method and oil fractionation equipment - Google Patents
Oil fractionation method and oil fractionation equipment Download PDFInfo
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- CN105462685A CN105462685A CN201410236611.6A CN201410236611A CN105462685A CN 105462685 A CN105462685 A CN 105462685A CN 201410236611 A CN201410236611 A CN 201410236611A CN 105462685 A CN105462685 A CN 105462685A
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Abstract
The present invention relates to an oil fractionation method and oil fractionation equipment. The method comprises that gas bubbles are introduced into a raw material oil under a condition of making of the raw material oil being in a metastable state, wherein the gas bubbles have a diameter of about 200 [mu]m or less than 200 [mu]m. With the method and the equipment of the present invention, the crystal nucleation at the oil fractionation early stage can be accelerated so as to obtain the high crystallization efficiency and/or soft fat yield.
Description
Technical field
The present invention relates to the processing of grease, relate more specifically to carry, particularly for the method and apparatus of grease dry fractionation dividing of grease.
Background technology
The working method of grease is divided into two classes: refining and modification.Dividing carries as a kind of oil and fat modification technology, utilize the difference in the mutual solubility of fatty acid triglycercides different in grease under fusing point or differing temps, by crystallisation by cooling and solid-liquid separation, realize the technology of the separation of different fatty acid triglycercide in grease.By point to carry grease can be separated into have compared with low melting point liquid portion (hereafter also referred to as palmitin) and there is the solid part (hereafter also referred to as tristearin) of higher melt.Point to carry solvent can be divided into again to divide according to the medium difference used carrying, tensio-active agent divides and carries and dry fractionation.Solvent divides to be carried owing to needing to use a large amount of solvent, and the cost of investment of factory and running cost are all higher, and just use point carrying in process of the higher product of some added values and difficult separate substance, use range is relatively little.Tensio-active agent divides to carry and needs to introduce external tensio-active agent, and as sodium lauryl sulphate, therefore product is inevitably by the pollution of these materials, uses and is also placed restrictions on gradually.Although it is slightly poor that dry fractionation compares first two method separating effect, along with the use of multistep fractionation technology and autoclave diaphragm pressure filter applying industrially, the separating effect of dry fractionation obtains remarkable improvement.The significant advantages such as further, it is low that dry fractionation has energy consumption, and production process environmental protection, process are reversible, its application presents trend more and more widely.But dry fractionation still needs further improvement in crystalline rate and control.
Dry fractionation is widely used in the modification of various grease, include but not limited to, Oleum Gossypii semen, plam oil, rapeseed oil, haco oil, tallow, cream, soybean oil, safflower oil, sunflower seed oil, sesame oil, Fructus Maydis oil, sweet oil, peanut oil, Oleum Cocois, palm-kernel oil, lard, fish oil etc., wherein most popular or palmitic dry fractionation.
Plam oil is a kind of widely used vegetables oil, and the main place of production is positioned at the countries such as South East Asia Indonesia, Malaysia.Plam oil containing the unsaturated fatty acids of 50% and the saturated fatty acid of about 50% of having an appointment, the food raw material that this comparatively special fatty acid ratio makes plam oil become to be most widely used.
Plam oil can be divided into 33 degree of plam oils, 24 degree of plam oils, 10 degree of palm wet goods according to the difference point carrying rear fusing point, and what be wherein most widely used at home is 10 degree of plam oils, how as the main raw material of frying oil, mixed oil.10 degree of plam oils are removed dystectic stearic part primarily of 24 degree of plam oils and obtain after dry fractionation, in 24 degree of palmitic crystallisation processs, (wherein S represents saturated fatty acid for the saturated triglyceride level of a small amount of SSS tri-and SSU/SUS cholesterol triglyceride level, U represents unsaturated fatty acids) meeting crystallization gradually, in remaining liq, the relative content of the polyunsaturated triglyceride such as SUU/USU and UUU can increase, the fusing point of final gained liquid oils is reduced, and winter hardiness improves.
In 24 degree of dry fractionation of palm oil processes of routine, due to more difficult crystallizations of symmetry triglyceride level such as SUS, make crystallization consuming time longer, and produced by the undercooling of raw material self completely due to crystallization initial stage nucleus, need higher condensate depression and the cooling of long period, and form the more difficult control of process of nucleus, easily produce nucleus tiny in a large number, to follow-up growing the grain, filter generation adverse influence.In addition, due to the fluctuation of 24 degree of plam oil raw materials composition, also often can make point to put forward process and become complexity, if temperature control is improper, also may occur rising again, freeze tank, be difficult to the phenomenons such as filtration, have a strong impact on the production efficiency of factory.Therefore 24 degree of palmitic fractionation technologies still have larger room for improvement, at present to the improvement of fractionation technology mainly to the improvement that improvement and the crystallisation process of equipment control.
Desmet etc. improve dry fractionation crystallizer in US0264667A1, using heat exchange pipe simultaneously as agitator, substantially increase heat interchanging area, in crystallisation process, keep uniform linear rate to stir simultaneously, also the growth making crystal in growing the grain process is comparatively even, is beneficial to follow-up filtration and improves the yield of palmitin.
Mainly adopt the method for adding crystal seed to promote crystallization at present to the control of crystallisation process, reach the object of optimizing process control.Such as, the atlapulgite by adding 0.5% in the plam oil after refining in US Patent No. 5231200, introduces heterogeneous nucleus, promotes crystallization, improves the yield of palmitin.U.S. Patent application US20070160739 carries by adding follow-up point in the feed the dystectic tristearin produced in process, regulates the chemical constitution of raw material, makes the easier crystallized abstract of stock oil.US Patent No. 5602265 and US5621125 by adding polymer and dystectic material shortens crystallization induction time in stock oil, thus enhance productivity and palmitin yield.Although but adding foreign matter promotes that the mode of crystallization can improving technique, inevitably bring the pollution of other foreign matter into, have an impact to subsequent product quality.
Chinese patent application CN102229860A and US Patent No. 6630185B2 all adopts ultrasonic wave to accelerate the crystallization of grease, can play the object shortening crystallization time and improve separation efficiency.But it is higher that ultrasonic wave realizes cost, and can heat effect be produced while promotion crystallization, cannot use for a long time.In addition, ultrasonic wave may make the local flavor of grease change, and has a certain impact to the quality of subsequent product.
In addition, promote that crystal nucleation is known in chemical industry by bubble, such as conventional bubble column crystallizer.But these means are generally used for realizing Crystallization Separation from the low viscosity materials such as solvent system, for the grease that system viscosity is larger, if use bubble column crystallizer to carry out dry fractionation can produce a large amount of foams, be unfavorable for follow-up product separation.
To sum up, the technology and equipment being applicable to grease particularly palmitic dry fractionation of higher crystalline rate and palmitin yield is still needed to have.
Summary of the invention
In order to resolve at least one or more of the problems as set forth in the prior art, the invention provides the novel method and equipment that are applicable to grease, particularly palmitic dry fractionation, the crystal nucleation time in advance that it accelerating point by the bubble with micron order or following diameter, thus achieve higher crystalline rate and/or palmitin yield.
In one aspect, the invention provides oil fractionation method, it passes into the step of bubble wherein under being included in and raw oil material being in be situated between the condition of steady state, wherein said bubble has about 200 μm or following diameter, and for the formation of the gas of described bubble be under residing condition not with the gas of described raw oil material generation chemical reaction.
On the other hand, the invention provides the crystallizer for oil fractionation, it is characterized in that, comprise the container for holding grease, for stirring the whipping appts of grease and the bubble generator for generation of bubble, the bubble exit of this bubble generator is positioned at the bottom of described container, and this bubble generator can produce the bubble with about 200 μm or following diameter.
In another, the invention provides the oil fractionation equipment for oil fractionation, it is characterized in that, comprise crystallizer of the present invention and provide the refrigerating unit of cooling for described crystallizer.
By method and apparatus of the present invention, can promote that oil fractionation is in the crystallization nucleation of the grease of the steady state that is situated between early stage, can crystalline rate be improved on the one hand, shorten crystallization time; On the other hand, the generation of nucleus can be made more lasting and even, and then improve subsequent crystallographic growth quality, be conducive to solid-liquid separation and palmitin yield can be improved.In addition, compare the seed technology of conventional interpolation tristearin, also can significantly improve gained palmitin and stearic quality product.
In addition; method and apparatus of the present invention is simple to operate, be easy to realize; a small amount of gas only can be used to carry out circulating, energy consumption is less; and gases used medium not only can not pollute the finished product; effectively can also protect raw material, make energy consumption cost and Material Cost all lower.
In addition, to compare in chemical industry conventional bubble column crystallizer, crystallizer of the present invention and separating-extracting apparatus forming a large amount of foam for avoiding during oil fractionation in grease, thus are conducive to follow-up solid-liquid separation.
Accompanying drawing explanation
The feature and advantage of the above-mentioned all respects that the present invention may be better understood of detailed description by reference to the accompanying drawings and hereafter and other side, wherein:
Fig. 1 is the schematic diagram of oil fractionation equipment according to an embodiment of the present invention;
Fig. 2 is the diagram of solid fats content with the change of temperature fall time of grease in reference examples 1 and embodiment 1;
Fig. 3 is the crystal habit that when starting rear 6h and 8h, the oil sample of reference examples 1 and embodiment 1 is observed under 40 times of polarizing microscopes of lowering the temperature, wherein the corresponding reference examples 1 of Fig. 3 a is when 6h, the corresponding embodiment 1 of Fig. 3 b is when 6h, and the corresponding reference examples 1 of Fig. 3 c is when 8h, and the corresponding embodiment 1 of Fig. 3 d is when 8h;
Fig. 4 is the diagram of palmitin iodine value with the change of temperature fall time of grease in reference examples 2 and embodiment 2.
Embodiment
In order to understand technical scheme of the present invention and beneficial effect better, hereafter the preferred embodiment of the present invention is illustrated in greater detail in conjunction with the embodiments.Should be appreciated that these explanations are only exemplary, and should not be construed as and by any way the present invention is construed as limiting.
" scope " disclosed herein, with the form of lower limit and the upper limit, such as the form of one or more lower limit and one or more upper limit provides.Given range limits by selecting a lower limit and a upper limit, and selected lower limit and the upper limit define the border of given range.All scopes limited by this way comprise and may be combined with, and namely any lower limit can be combined to form a scope with any upper limit.Such as, list the scope of 60-110 and 80-120 for special parameter, be interpreted as that the scope of 60-120 and 80-110 also can expect.In addition, if the lower limit listed is 1 and 2 upper limits listed is 3,4 and 5, then the scope below all can expect: 1-3,1-4,1-5,2-3,2-4 and 2-5.
In this article, unless otherwise indicated, the breviary of any real combinings that numerical range " a-b " represents between a to b represents, wherein a and b is real number.Such as numerical range " 0-5 " represents the whole real numbers all listed between " 0-5 " herein, and the breviary of " 0-5 " just these combinations of values represents.
In this article, unless otherwise indicated, the arbitrary combination of each selection key element listed by term " its combination " or " their combination " represent, such as two kinds, three kinds, four kinds and until the combination of selection key element of most probable number, as mixture.
If do not particularly not pointed out, this specification sheets term used " a kind of (individual) " refers to " at least one (individual) ".
In this article, unless otherwise indicated, all embodiments mentioned in this article and preferred implementation can be combined to form new technical scheme mutually.
In this article, unless otherwise indicated, all technical characteristics mentioned in this article and preferred feature can be combined to form new technical scheme mutually.
In this article, unless otherwise indicated, term " comprises ", " comprising ", " containing ", " having " and similar word represent open, but also should be understood to specifically disclose enclosed situation simultaneously.Such as, " comprising " expression can also comprise other key elements do not listed, but also specifically discloses the situation only comprising listed key element simultaneously.
In this article, unless otherwise indicated, the concrete steps recorded in embodiment, concrete numerical value and concrete material can with other integrate features of specification sheets other parts.Such as, the temperature that specification sheets summary of the invention or embodiment part mention reaction is 10-100 DEG C, and the concrete temperature of reaction that embodiment is recorded is 20 DEG C, so can think the scope having specifically disclosed 10-20 DEG C herein, or the scope of 20-100 DEG C, and this scope can get up formed new technical scheme with other integrate features of specification sheets other parts.
As mentioned above, the present invention provides oil fractionation method in first aspect, and it passes into the step of microbubble wherein under being included in and raw oil material being in be situated between the condition of steady state, described microbubble has about 200 μm or following diameter.
In this article, term " grease " has the implication that this area accepts usually, particularly represent the mixture being main component with higher fatty acid ester of plant or animal-origin, include but not limited to, Oleum Gossypii semen, plam oil, rapeseed oil, haco oil, tallow, cream, soybean oil, safflower oil, sunflower seed oil, sesame oil, Fructus Maydis oil, sweet oil, peanut oil, Oleum Cocois, palm-kernel oil, lard, fish oil etc.The grease being applicable to the inventive method is preferably plam oil, fish oil, tallow, anhydrous milkfat, poultry wet goods, is more preferably plam oil, is particularly preferably 24 degree of plam oils.
In this article, term " be situated between steady state " can claim again " metastable state " or " metastable state ", represent grease be between stable with instability between a kind of state, now grease has the tendency of spontaneous formation crystal owing to crossing cold and/or supersaturation.Usually, can by heat and/or cool make raw oil material reach specific temperature make its be in be situated between steady state.For different raw oil materials, make it reach the temperature of Jie needed for steady state different, can be determined by ordinary method these those skilled in the art.Such as, for 24 degree of plam oils, usually when its temperature reach about 19 DEG C to about 25 DEG C, particularly about 20 DEG C to about 21 DEG C time can be in this " be situated between steady state ".Preferably, in the methods of the invention, raw oil material entered be situated between steady state but not yet formed can the nucleus of detection limit time, in this raw oil material, pass into microbubble.
Be not limited to concrete theory, it is believed that when grease has reached the steady state of Jie but not yet formed or only form a small amount of nucleus, slowly pass into a small amount of diameter at about 200 μm or following microbubble, can make microbubble with longer time stable existence in grease, the change of the interfacial tension of microbubble and grease can promote the generation of nucleus.Further, when the temperature of grease during the temperature of microbubble is slightly lower than crystallizer, the heat of crystallization of release when nucleus produces can be taken away quickly, thus accelerate the formation of nucleus further.Preferably, to pass into the temperature of bubble lower than the temperature of raw oil material about 1 DEG C to about 3 DEG C, more preferably from about 1 DEG C to about 2 DEG C.In a preferred embodiment, by adopting same heat-eliminating medium for the grease in crystallizer and providing cooling to obtain for the formation of the gas of microbubble and keep this temperature difference.
In the methods of the invention, gas produces microbubble preferably by bubble generator and is distributed to equably in crystallizer.For ensureing the quality of grease in crystallizer, even if preferably with under residing condition, under also raw oil material is in the condition of the steady state that is situated between, not with the gas of lubricant component generation chemical reaction (namely in inertia) as the gaseous media forming bubble, object lesson includes but not limited to nitrogen, helium and carbonic acid gas etc.In addition, preferably crystallizer is closed, and make gas circulation by crystallizer, to reduce gas usage; Simultaneously cycle period also preferably constantly carries out temperature adjustment refrigeration to this gas, to guarantee the controlled and constant of microbubble temperature.
In this article, term " microbubble " or " having the bubble of micron order or following diameter " are used interchangeably, and represent that diameter is about 200 μm or following bubble, preferably diameter is about 100 μm or following.The not special restriction of lower limit for the diameter of described microbubble can be such as the minimum bubble diameter that existing bubble generator or air bubbles dispersion device can obtain.But, for the consideration simplified the operation and to reduce costs etc., preferably the diameter of " microbubble " be about 10nm or more usually, is more preferably about 100nm or more, further preferably about 1 μm or more.In particularly preferred embodiments, the diameter of described microbubble is about 50 μm to about 100 μm.
Produce the method for microbubble for those skilled in the art known by, such as can by aperture about 200 μm or following, the bubble generator of preferred about 100 μm or following, more preferably from about 50 μm to about 100 μm or gas dispersion apparatus produce.The example of described bubble generator or gas dispersion apparatus includes but not limited to gas cake, Bubbled stone, organic membrane and kapillary etc.
In this article, unless otherwise indicated, when mentioning the diameter range of bubble be represent more than 50%, the bubble of preferably more than 80%, more preferably more than 90%, particularly preferably more than 95% has the diameter within the scope of this.Such as, when mentioning bubble " diameter is about 200 μm or following " or " there is about 200 μm or following diameter ", represent in the bubble that produces have more than 50%, the diameter of preferably more than 80%, more preferably more than 90%, particularly preferably more than 95% is at 200 μm or following.Again such as, when mentioning bubble " diameter is about 50 μm to about 100 μm " or " there is the diameter of about 50 μm to about 100 μm ", represent in the bubble that produces have more than 50%, the diameter of preferably more than 80%, more preferably more than 90%, particularly preferably more than 95% is about 50 μm to about 100 μm.
In the methods of the invention, the passing into speed and can adjust according to the needs of practical application of described microbubble.In a preferred embodiment, described microbubble passes into about 0.05-0.1L/min every kilogram grease, the more preferably from about speed of 0.05-0.75L/min every kilogram grease.
In a preferred embodiment, during bubble passes into step, described raw oil material is cooled, to promote the formation of nucleus.Any stage that this cooling can pass into step at described bubble is carried out, such as, carry out during whole bubble passes into step, or passes into early stage of step, mid-term and/or later stage at bubble and carry out.Preferably, carry out during whole bubble passes into step or in the later stage that bubble passes into step.
In a preferred embodiment, when having produced the nucleus of aequum in described raw oil material, stop passing into described microbubble.Usually, can according to the change of the proterties of raw oil material as transparency (turbidity) or temperature, or determine whether by sampling analysis the nucleus producing aequum, such as, when being to carry out cooling during bubble passes into step, when the temperature of described raw oil material reduce further about 1-2 DEG C or be brought down below the temperature maintaining and be situated between needed for steady state time, usually in this raw oil material, created enough nucleus.Now, if do not stop and continuing to pass into microbubble, then because the reduction of grease viscosity along with temperature constantly raises, likely can cause serious foam on the contrary, produce and freeze tank phenomenon, and then next step filtration cannot be carried out.
In a preferred embodiment, described method, before bubble passes into step, can also comprise the step of the fat crystalline substance removing original existence in described raw oil material.Those skilled in the art knownly, grease is in refining, course of conveying, sometimes oil temperature is lower than also can crystallize out during solid-state fat zero pour, because this part crystal is separated out in non-at the uniform velocity temperature-fall period, crystal formation is different, grain size differs, and its existence may affect point uniform growth carrying fat crystalline substance in process and a maturation, is therefore preferably removed before enforcement point is carried.
One preferred embodiment in, the step of the fat crystalline substance of the original existence of described removal comprises the step that the described raw oil material of heating is remembered to eliminate crystallization, preferably includes and described raw oil material is heated to sufficiently high temperature and keeps one sufficiently long period.Preferably, the described sufficiently long time is about 10-60 minute, is more preferably about 20-40 minute, most preferably is about 30 minutes.
In this article, term " eliminates crystallization memory " also referred to as " broken brilliant ", refers to the fat crystalline substance being eliminated wherein original existence by heating raw grease, such as, makes it again be dissolved in raw oil material.For different raw oil materials, the temperature eliminated needed for crystallization memory is different, can be determined these those skilled in the art by ordinary method.Such as, for 24 degree of plam oils, usually crystallization memory can be eliminated by the temperature being heated about 50 DEG C to about 75 DEG C, preferred about 55 DEG C to about 70 DEG C.
Another preferred embodiment in, the step of the fat crystalline substance of the original existence of described removal comprise by solid-liquid separation as filter from as described in remove the fat of original existence raw oil material brilliant.
In a preferred embodiment, after bubble passes into step, described method can also comprise conventional growing the grain step and solid-liquid separation step, includes but not limited to centrifugation and filtering separation.
In particularly preferred embodiments, described method comprises the steps:
I) raw oil material be heated to sufficiently high temperature and keep one sufficiently long period to eliminate crystallization memory, then cooling makes this raw oil material reach the steady state that is situated between, such as will be heated to about 50 DEG C to about 75 DEG C, the preferred temperature of about 55 DEG C to about 70 DEG C as 24 degree of plam oils of raw oil material, and keeping about 10 minutes to about 60 minutes, preferably about 20 to about 40 minutes, then cooling makes this raw oil material reach the temperature of about 19 DEG C to about 25 DEG C, preferred about 20 DEG C to about 21 DEG C;
Ii) under the condition keeping cooling, pass in this raw oil material and there is about 200 μm or following, the bubble of the diameter of preferably about 100 μm or following, more preferably from about 50 μm to about 100 μm, the speed that passes into of wherein said bubble is preferably about 0.05-0.1L/min every kilogram grease, is more preferably about 0.05-0.075L/min every kilogram grease, and to pass into the temperature of bubble preferably low than the temperature of raw oil material about 1 DEG C to about 3 DEG C, more preferably low about 1 DEG C to about 2 DEG C;
Iii) when the temperature of described raw oil material reduce further about 1-2 DEG C or be brought down below the temperature maintaining and be situated between needed for steady state time, stop passing into bubble; And
Iv) continue cooling and growing the grain until obtain required product.
In a particularly preferred embodiment, described method comprises the steps:
A) add 24 degree of plam oil raw materials in a crystallizer, and in crystallizer, pass into rare gas element as nitrogen, helium and/or carbonic acid gas, to ensure to be full of this rare gas element in crystallizer He in gas piping;
B) open heating and stir, keeping agitator to be about the rotating speed of 30-50r/min, make the grease in crystallizer be warming up to about 55-70 DEG C, be incubated about 30min, to eliminate crystallization memory;
C) grease in cooling crystallizer also continues to stir, continue in crystallizer when grease temperature is down to about 20-21 DEG C to pass into the rare gas element microbubble that diameter is about 50 μm to about 100 μm, gas flow controls the scope at every kilogram of grease 0.05-0.1L/min;
D) keep cooling, and when grease temperature reduce further about 1-2 DEG C or be brought down below about 19 DEG C when grease temperature time stopping pass into microbubble; And
E) continue stir and cooling condition under growing the grain until obtain required product.
The present invention provides the crystallizer for oil fractionation in second aspect, it is characterized in that, comprise the container for holding grease, for stirring the whipping appts of grease and the bubble generator for generation of bubble, the bubble exit of this bubble generator is positioned at the bottom of described container, and this bubble generator can produce the bubble with about 200 μm or following diameter.
In a preferred embodiment, described bubble generator is arranged on the bottom of described container.Being applicable to bubble generator of the present invention can be that any can generation has about 200 μm or following, the bubble generator of the bubble of the diameter of preferably about 100 μm or following, more preferably from about 50 μm to about 100 μm or gas dispersion apparatus, include but not limited to micropore air bubble generator or gas distributor, such as aperture is at the gas cake, Bubbled stone, organic membrane, kapillary etc. of about 200 μm or following, preferably about 100 μm or following, more preferably from about 50 μm to about 100 μm.The upper surface of this bubble generator can have the geometric shape be applicable to arbitrarily, is preferably level and smooth plane, concave surface or convex surface, is preferably plane.Such as, described bubble generator can protrude for having smooth, center or the patty of flat top surface of central concave.
In a preferred embodiment, described whipping appts is arranged in described container, and is positioned at the top of described bubble generator.Being applicable to whipping appts of the present invention can be the whipping appts of any routine for oil fractionation, includes but not limited to rotary propeller type, turbine type, paddle, anchor formula, helical-ribbon type and grid agitator, is preferably grid agitator.
In a preferred embodiment, the upper surface of bubble generator is close in the lower end of described whipping appts, and there is the shape matched with bubble generator upper surface, can again reduce thus microbubble diameter and by produce microbubble short mix in the material in crystallizer.Coordinated with this of whipping appts by bubble generator, the microbubble diameter of generation can be made to reach 100 μm or following and even to reach nano level, simultaneously can make microbubble consistent output and evenly spread in the material in crystallizer, and stable existence for some time and not separating out in material.
See Fig. 1, which show the schematic diagram of oil fractionation equipment according to an embodiment of the present invention, and schematically show crystallizer according to an embodiment of the present invention.As shown in the figure, this crystallizer has treats point container carrying grease for holding, and is positioned at the agitator of container, and is positioned at the bubble generator of container bottom.Described container has gas inlet and the outlet of supplied gas expellant gas that supplied gas enters bubble generator, external container has for the logical chuck of cooling medium flow.Wherein, bubble generator is smooth patty, and agitator is grid agitator and lower end is the flat shape being close to bubble generator upper surface.
The present invention provides the oil fractionation equipment for oil fractionation in the third aspect, it is characterized in that, comprises crystallizer of the present invention and provides the refrigerating unit of cooling for described crystallizer.
In a preferred embodiment, described refrigerating unit is simultaneously also for the gas for producing bubble via bubble generator provides cooling, more preferably described refrigerating unit adopts same heat-eliminating medium to provide cooling for described crystallizer and described gas, thus make the temperature of described gas lower than the grease in described crystallizer about 1 DEG C to about 3 DEG C, more preferably low about 1 DEG C to about 2 DEG C.Specifically, when described gas and crystallizer adopt same heat-eliminating medium to cool, due to the difference of the aspects such as rate of heat transfer, the temperature of described gas reaches identical with heat-eliminating medium substantially, the temperature of grease is then than heat-eliminating medium height about 1-3 DEG C, make the temperature difference having about 1-3 DEG C between produced microbubble and grease thus, and the temperature difference of this scope contributes to forming the good nucleus of quality.
In a preferred embodiment, described oil fractionation equipment also comprises gas-recycling plant, thus makes gas circulation by crystallizer, reaches saving gas consumption and energy consumption, and reduces the object of possible grease contamination.
Refer again to Fig. 1, which show the schematic diagram of oil fractionation equipment according to an embodiment of the present invention.As shown in the figure, described oil fractionation equipment comprises crystallizer and for providing the water-bath of cooling, this water-bath simultaneously also by the gas cooling coil pipe that is placed in one for rare gas element such as the nitrogen for generation of microbubble provides cooling.Wherein, crystallizer is connected with under meter with gas flow dryer, gas recycle pump, gas cooling coil pipe, forms gas circulation loop, and the chuck of crystallizer is connected with water-bath and forms cooling water circulation loop.When crystallizer is started working, in crystallizer and connected pipeline, first use rare gas element as nitrogen replacement; Then start gas recycle pump, gas flow is controlled by under meter, and the gas of the spiral coil cooling tube cooling in water-bath forms microbubble via bubble generator and enters in crystallizer; By the gas after crystallizer by crystallizer upper collection and through moisture eliminator purification, then the import entering gas recycle pump recycles.
Especially, the invention provides the technical scheme of following aspect:
1. oil fractionation method, it passes into the step of bubble in this raw oil material under being included in and raw oil material being in be situated between the condition of steady state, wherein said bubble has about 200 μm or following, the diameter of preferably about 100 μm or following, more preferably from about 50 μm to about 100 μm, and for the formation of the gas of described bubble be under residing condition not with the gas of described raw oil material generation chemical reaction.
2. according to the method for aspect 1, wherein said raw oil material is plam oil, is more preferably 24 degree of plam oils.
3., according to the method for any preceding aspect, the gas wherein for the formation of described bubble is selected from nitrogen, helium, carbonic acid gas and their arbitrary combination.
4., according to the method for any preceding aspect, the temperature of wherein passed into bubble is lower than the temperature of described raw oil material about 1 DEG C to about 3 DEG C, preferably about 1 DEG C to about 2 DEG C.
5., according to the method for any preceding aspect, the speed that passes into of wherein said bubble is about 0.05-0.1L/min every kilogram grease, is more preferably about 0.05-0.075L/min every kilogram grease.
6., according to the method for any preceding aspect, wherein saidly raw oil material is in be situated between steady state to comprise described raw oil material to be in make it reach cold and/or the temperature of hypersaturated state.
7., according to the method for any preceding aspect, wherein saidly raw oil material is in be situated between steady state to comprise the temperature making 24 degree plam oils as raw oil material be in about 19 DEG C to about 25 DEG C, preferred about 20 DEG C to about 21 DEG C.
8. according to the method for any preceding aspect, wherein during bubble passes into step, described raw oil material is cooled, preferably cool during whole bubble passes into step or in the later stage that bubble passes into step.
9. according to the method for any preceding aspect, wherein before bubble passes into step, also comprise the step of the fat crystalline substance removing original existence in described raw oil material, preferably include the described raw oil material of heating to eliminate the step of crystallization memory.
10. according to the method for any preceding aspect, wherein before bubble passes into step, also comprise and will be heated to about 50 DEG C to about 75 DEG C, the preferred temperature of about 55 DEG C to about 70 DEG C as 24 degree of plam oils of raw oil material, and keep about 10 minutes to about 60 minutes, preferably about 20 to about 40 minutes, then cool the step this raw oil material being reached be situated between steady state.
11. according to the method for any preceding aspect, wherein stop passing into bubble in described raw oil material after the nucleus obtaining aequum, when being preferably to carry out cooling during bubble passes into step, when the temperature of described raw oil material reduce further about 1-2 DEG C or be brought down below the temperature maintaining and be situated between needed for steady state time, stop passing into bubble.
12. according to the method for any preceding aspect, wherein after bubble passes into step, also comprise the described grease of cooling and growing the grain until obtain the step of required product.
13. according to the method for any preceding aspect, and wherein said method comprises the steps:
I) heat described raw oil material to eliminate crystallization memory, then cooling makes this raw oil material reach the steady state that is situated between;
Ii) while maintenance cooling, pass in this raw oil material and there is about 200 μm or following, the bubble of the diameter of preferably about 100 μm or following, more preferably from about 50 μm to about 100 μm;
Iii) when the temperature of described raw oil material reduce further about 1-2 DEG C or be brought down below the temperature maintaining and be situated between needed for steady state time, stop passing into bubble; And
Iv) continue cooling and growing the grain until obtain required product.
14. according to the method for any preceding aspect, and wherein said method comprises the steps:
I) about 50 DEG C to about 75 DEG C, the preferred temperature of about 55 DEG C to about 70 DEG C will be heated to as 24 degree of plam oils of raw oil material, and keep about 10 minutes to about 60 minutes, preferably about 20 to about 40 minutes, be then cooled to the temperature of about 19 DEG C to about 25 DEG C, preferred about 20 DEG C to about 21 DEG C;
Ii) while maintenance cooling, pass in this raw oil material and there is about 200 μm or following, the bubble of the diameter of preferably about 100 μm or following, more preferably from about 50 μm to about 100 μm;
Iii) when the temperature of described raw oil material reduce further about 1-2 DEG C or be brought down below about 19 DEG C time, stop passing into bubble; And
Iv) continue cooling and growing the grain until obtain required product.
15. for the crystallizer of oil fractionation, it is characterized in that, comprise the container for holding grease, for stirring the whipping appts of grease and the bubble generator for generation of bubble, wherein the bubble exit of this bubble generator is positioned at the bottom of described container, and this bubble generator can produce and has about 200 μm or following, the bubble of the diameter of preferably about 100 μm or following, more preferably from about 50 μm to about 100 μm.
16. crystallizers according to aspect 15, wherein said bubble generator is selected from the gas dispersion apparatus such as gas cake, Bubbled stone, organic membrane and kapillary of aperture about 200 μm or following, preferably about 100 μm or following, more preferably from about 50 μm to about 100 μm.
17. crystallizers according to aspect 15 or 16, the upper surface of described bubble generator is pressed close in the lower end of wherein said whipping appts, and has the shape matched with described bubble generator upper surface.
18. crystallizers according to any one of aspect 15-17, wherein said whipping appts is grid agitator.
19., for the oil fractionation equipment of oil fractionation, is characterized in that, comprise crystallizer according to any one of aspect 15-18 and provide the refrigerating unit of cooling for described crystallizer.
20. oil fractionation equipment according to aspect 19, wherein said refrigerating unit is simultaneously also for the gas for producing bubble via described bubble generator provides cooling.
21. oil fractionation equipment according to aspect 20, wherein said refrigerating unit adopts same heat-eliminating medium to provide cooling for described crystallizer and described gas, thus make the temperature of described gas lower than the grease in described crystallizer about 1 DEG C to about 3 DEG C, more preferably low about 1 DEG C to about 2 DEG C.
22. oil fractionation equipment any one of aspect 19-21, wherein said oil fractionation equipment also comprises gas-recycling plant.
In order to make statement more succinct; various preferred implementation of the present invention separately describes separately in the description; but it will be appreciated by those skilled in the art that; in not conflicting situation; the technical characteristic of each preferred implementation can reconfigure formed other or further preferred embodiment, these embodiments should be considered as by clearly open herein and fall within the scope of protection of the present invention.
Embodiment
By the following examples exemplary description is done to the present invention, be to be understood that these embodiments are not only construed as limiting the invention for illustration of object.
1) reagent source
In following examples and reference examples, 24 degree of plam oils used are 24 degree of plam oils that the iodine value purchased from beneficial Hai Jiali group is 57.6, free fatty acids (FFA): 0.1%, peroxide value (PV): 0.8meq/kg, fusing point: 21.6 DEG C.
2) detection method
Related detecting method involved in following examples and reference examples is as follows:
Iodine value measuring method is see IodineValueofFatsandOils, AOACOfficialMethod993.20.Reappproved.1997;
Solid fats content detection method is see SolidFatContent (SFC) byLow-ResolutionNuclearMagneticResonance-TheDirectMethod, AOCSOfficialMethodCd16b-93.Reapproved.1997;
The detection method that triglyceride level (TAG) forms is see Wei Tingting, Yang Hong, Yang Tiankui. the research of series connection silver ions chromatogram column analysis structured triglyceride isomers, Chinese oil, 2012,37 (7): 79-81.
3) testing installation
Relevant device involved in following examples and reference examples is as follows:
Bubble generator: AngelaquaDY104 series Bubbled stone.
Water-bath: JulaboME (V.2) type temperature controller.
Embodiment 1
By in the crystallizer of equipment shown in 1.6kg24 degree plam oil load map 1, and pass into nitrogen, to ensure to be full of nitrogen in crystallizer He in gas piping.Open heating in water bath and stirring, maintenance agitator speed is 50r/min, makes the grease in crystallizer be warming up to 55 DEG C, insulation 30min, to eliminate crystallization memory.
Subsequently, the program of according to the form below 1 by the grease slow cooling in crystallizer and continue stir.Open gas recycle pump when oil temperature 20 DEG C, now the temperature of water coolant is 19 DEG C.The valve of adjusting gas flow meter, with the flow velocity of 0.1L/min, to bubble generator, (aperture is 200 μm, Air permenbility is the Bubbled stone of 0.6L/min) in pass into the nitrogen after spiral coil cooling tube temperature adjustment with produce mean diameter lower than 200 μm microbubble (by microscope sampling observation determine), this microbubble Absorbable organic halogens is present in for some time in grease.
Table 1 cooling process
| Step is poly- | Design temperature (DEG C) | Temperature fall time (min) * |
| 1 | 40 | 30 |
| 2 | 20 | 60 |
| 3 | 16.5 | 100 |
| 4 | 16.2 | 100 |
| 5 | 16.0 | 200 |
| 6 | 15.5 | 200 |
*represent and be at the uniform velocity cooled to from last temperature the time that Current Temperatures spends.
When oil temperature is down to 19 DEG C, be observed visually in crystallizer and produced more nucleus of uniform size, now stop gas recycle pump.Continue by the programmed cooling of table 1 and growing the grain to terminal of lowering the temperature, amount to 11.5h consuming time, now sampling filtering records palmitin iodine value is 60.9.In temperature-fall period, sampling records the solid fats content of grease as shown in Figure 2 at set intervals.Sample respectively when starting to lower the temperature 6h and 8h at 40 times of polarized light microscopy Microscopic observation crystal habits, result is respectively as shown in Fig. 3 b and 3d.
Reference examples 1
By in the crystallizer of equipment shown in 1.6kg24 degree plam oil load map 1, open heating in water bath and stirring, keep the rotating speed of 50r/min, make the grease in crystallizer be warming up to 55 DEG C, insulation 30min, to eliminate crystallization memory.
Continued to stir by grease slow cooling in crystallizer by the program of upper table 1, but in crystallizer, do not pass into gas, until cooling terminal, now sampling filtering records palmitin iodine value is 59.7.In temperature-fall period, sampling records the solid fats content of grease as shown in Figure 2 at set intervals.Sample respectively when starting to lower the temperature 6h and 8h at 40 times of polarized light microscopy Microscopic observation crystal habits, result is respectively as shown in Fig. 3 a and 3c.
The Comparative result analysis of embodiment 1 and reference examples 1:
1, as shown in Figure 2, after crystallization starts, when identical temperature fall time, embodiment 1 samples the solid fats content recorded and is obviously greater than reference examples 1, shows that the microbubble passed in embodiment 1 serves the effect accelerating fat crystals;
2, as illustrated in figs. 3 a-3d, after crystallization starts, when identical temperature fall time, embodiment 1 samples the crystal observed will obviously be greater than reference examples 1, and the microbubble showing through temperature adjustment obviously can promote the growth of crystal;
3, when lowering the temperature terminal 11.5h, it is 60.9 that embodiment 1 samples the palmitin iodine value recorded, higher than 59.7 of reference examples 1.When showing identical temperature fall time, embodiment 1 can remove the stearic component of more how low iodine value, obtains the palmitin component of higher iodine value, thus significantly improves the quality of palmitin.
Embodiment 2
By in the crystallizer of equipment shown in 1.6kg24 degree plam oil load map 1, and pass into nitrogen, to ensure to be full of nitrogen in crystallizer He in gas piping.Open heating in water bath and stirring, keep the rotating speed of 40r/min, make the grease in crystallizer be warming up to 60 DEG C, insulation 30min, to eliminate crystallization memory.
The program of according to the form below 2 by the grease slow cooling in crystallizer and continue stir.Open gas recycle pump when oil temperature 21 DEG C, now the temperature of water coolant is 20 DEG C.The valve of adjusting gas flow meter, with the flow velocity of 0.1L/min, to bubble generator, (aperture is 100 μm, Air permenbility is the Bubbled stone of 0.6L/min) in pass into the nitrogen after spiral coil cooling tube temperature adjustment with produce mean diameter lower than 100 μm microbubble (by microscope sampling observation determine), this microbubble Absorbable organic halogens is present in for some time in grease.
Table 2 cooling process
| Step is poly- | Design temperature (DEG C) | Temperature fall time *(min) |
| 1 | 40 | 30 |
| 2 | 21 | 60 |
| 3 | 16.5 | 100 |
| 4 | 16.2 | 100 |
| 5 | 16.0 | 200 |
| 6 | 15.5 | 200 |
| 7 | 15 | 350 |
| 8 | 14.5 | 220 |
| 9 | 13.5 | 180 |
| 10 | 12.5 | 180 |
| 11 | 12.5 | 360 ** |
*represent and be at the uniform velocity cooled to from last temperature the time that Current Temperatures spends;
*represent the soaking time at 12.5 DEG C.
When oil temperature is down to 20 DEG C, be observed visually in crystallizer and produced more nucleus of uniform size, now stop gas recycle pump.Continue the programmed cooling pressing table 2, until cooling terminal.In temperature-fall period, sampling filtering measures the iodine value of palmitin at set intervals, and result as shown in Figure 4.Sample about 100ml magma when lowering the temperature 30h, suction filtration obtains palmitin with stearic, measures gained palmitin and stearic iodine value, and calculates palmitin yield, the results are shown in following table 3.
Reference examples 2
By in the crystallizer of equipment shown in 1.6kg24 degree plam oil load map 1, open heating in water bath and stirring, keep the rotating speed of 40r/min, make the grease in crystallizer be warming up to 60 DEG C, insulation 30min, to eliminate crystallization memory.
By the program of upper table 2, the grease slow cooling in crystallizer is continued to stir, but do not pass into gas to crystallizer, until cooling terminal.In temperature-fall period, sampling filtering measures the iodine value of palmitin at set intervals, and result as shown in Figure 4.Sample about 100ml magma at terminal of lowering the temperature (namely during cooling 33h), suction filtration obtains palmitin with stearic, measures the iodine value of gained palmitin and tristearin, and calculates palmitin yield, the results are shown in following table 3.
The Comparative result of table 3 embodiment 2 and reference examples 2
| Project | Embodiment 2 | Reference examples 2 |
| Palmitin iodine value | 64.9 | 65.1 |
| Stearic iodine value | 49 | 52.6 |
| The suction filtration time | 4min | 4min |
| Palmitin yield | 52% | 37% |
The Comparative result analysis of embodiment 2 and reference examples 2:
1, as shown in Figure 4, after cooling 24h when identical temperature fall time, embodiment 2 samples the palmitin iodine value that records apparently higher than reference examples 2, correspondingly when with same palmitin iodine value for target time, the time needed for embodiment 2 is obviously less than reference examples 2.Such as, if with 10 of iodine value 65 degree of plam oils for target product, then embodiment 2 needs the time of 30h, and reference examples 2 needs the time of at least 33h.Therefore, compare as a rule 2, embodiment 2 in advance at least 3h just can obtain target product, thus improve production efficiency.
2, from upper table 3, embodiment 2 compares 2 not only can shorten the time needed for palmitin product obtaining identical iodine value as a rule, can also significantly improve the yield of this palmitin product.
Embodiment 3:
By in the crystallizer of equipment shown in 1.6kg24 degree plam oil load map 1, and pass into carbon dioxide, to ensure to be full of carbon dioxide in crystallizer He in gas piping.Open heating in water bath and stirring, keep the rotating speed of 50r/min, make the grease in crystallizer be warming up to 55 DEG C, insulation 30min, to eliminate crystallization memory.
By the program of upper table 2, the grease slow cooling in crystallizer is continued to stir.Open gas recycle pump when oil temperature 20 DEG C, now the temperature of water coolant is 19 DEG C.The valve of adjusting gas flow meter, with the flow velocity of 0.1L/min, to bubble generator, (aperture is 50 μm, Air permenbility is the Bubbled stone of 0.6L/min) in pass into the carbonic acid gas after spiral coil cooling tube temperature adjustment with produce mean diameter lower than 50 μm microbubble (by microscope sampling observation determine), this microbubble Absorbable organic halogens is present in for some time in grease.
When oil temperature is down to 19 DEG C, be observed visually in crystallizer and produced more nucleus of uniform size, now stop gas recycle pump.Continue press table 2 programmed cooling, and the iodine value of sampling monitoring palmitin at set intervals, stop stirring when palmitin iodine value reaches 65, get stearic part and carry out triglyceride level (TAG) and form and analyze, the results are shown in following table 4.
Reference examples 3:
By in the crystallizer of equipment shown in 1.6kg24 degree plam oil load map 1, open heating in water bath and stirring, keep the rotating speed of 50r/min, make the grease in crystallizer be warming up to 55 DEG C, insulation 30min, to eliminate crystallization memory.
By the program of upper table 2, the grease slow cooling in crystallizer is continued to stir.When grease temperature is down to 20 DEG C in a crystallizer, the palm stearin slurry adding 3% accelerates crystallization as crystal seed.Continue to stir cooling according to the program of table 2, and the iodine value of sampling monitoring palmitin, stop stirring when palmitin iodine value reaches 65, get stearic part and carry out triglyceride level (TAG) compositional analysis, the results are shown in following table 4.
Table 4 embodiment 3 forms with the stearic main TAG of reference examples 3 and contrasts
| TAG/% | Embodiment 3 | Reference examples 3 |
| MPP | 0.53 | 0.95 |
| PPP | 2.47 | 4.18 |
| MOP | 1.88 | 1.75 |
| PPS | 0.46 | 0.12 |
| POP | 50.0 | 50.77 |
| PLP | 9.92 | 9.85 |
| POS | 8.19 | 8.42 |
| POO | 13.0 | 10.74 |
| PLS | 1.75 | 1.68 |
| PLO | 4.80 | 4.31 |
| PLL | 0.91 | 0.89 |
| SOS | 0.81 | 0.82 |
| SOO | 1.20 | 1.11 |
| OOO | 1.45 | 1.32 |
In table 4, the implication of each english abbreviation is as follows:
MPP.1-myristic acid-2,3-glycerol-1,3-dipalmitate; PPP. tripalmitin; MOP.1-myristic acid-2-oleic acid-3-palmitin; PPS.1,2-bis-palmitinic acid-3-stearin; POP.1,3-bis-palmitinic acid-2-olein; PLP.1,3-bis-palmitinic acid-2-glyceryl linoleate; POS.1-palmitinic acid-2-oleic acid-3-stearin; POO.1-palmitinic acid-2,3-glyceryl dioleate; PLS.1-palmitinic acid-2-linolic acid-3-stearin; PLO.1-palmitinic acid-2-linolic acid-3-olein; PLL.1-palmitinic acid-2,3-dilinoleic acid glyceryl ester; SOS.1,3-distearyl acid-2-olein .SOO.1-stearic acid-2,3-glyceryl dioleate; OOO. triolein.
The Comparative result analysis of embodiment 3 and reference examples 3:
As shown in table 4, adopt the PPP component concentration in the stearic product of embodiment 3 gained of the inventive method to be starkly lower than the reference examples 3 adopting seed technology.When the byproduct tristearin point carrying gained is used as the raw material of substitute of cocoa fat, have certain requirement to PPP component concentration, PPP component concentration is more low more not easily produces wax-like mouthfeel.Therefore, in this respect, the present invention is better than the technology of conventional interpolation palm stearin slurry as crystal seed.
Reference examples 4:
By in the crystallizer of equipment shown in 1.6kg24 degree plam oil load map 1, and pass into nitrogen, to ensure to be full of nitrogen in crystallizer He in gas piping.Open heating in water bath and stirring, maintenance agitator speed is 50r/min, makes the grease in crystallizer be warming up to 55 DEG C, insulation 30min, to eliminate crystallization memory.
The program of according to the form below 5, by the grease slow cooling in crystallizer, is opened gas recycle pump, is closed agitator simultaneously.The valve of adjusting gas flow meter, with the flow velocity of 0.1L/min, to bubble generator, (aperture is 100 μm, Air permenbility is the Bubbled stone of 0.6L/min) in pass into the nitrogen after spiral coil cooling tube temperature adjustment with produce mean diameter lower than 100 μm microbubble (by microscope sampling observation determine), only with produced microbubble, the material in crystallizer is uniformly mixed.
Table 5 cooling process
| Step is poly- | Design temperature (DEG C) | Temperature fall time *(min) |
| 1 | 40 | 30 |
| 2 | 20 | 60 |
| 3 | 16.5 | 100 |
| 4 | 16.2 | 100 |
| 5 | 16.0 | 200 |
| 6 | 15.5 | 200 |
| 7 | 15 | 350 |
| 8 | 14.5 | 220 |
| 9 | 13.5 | 180 |
| 10 | 12.5 | 180 |
*represent and be at the uniform velocity cooled to from last temperature the time that Current Temperatures spends.
Continue to pass into bubble and last till cooling terminal in the mode of gas stirring, because grease viscosity constantly rose in the later stage, cause grease foam that the is inner and accumulation of crystallizer top to get more and more, make the material fluidity in cooling later stage very poor, occur freezing tank phenomenon, be difficult to filter.
Reference examples 5
By in the crystallizer of equipment shown in 1.6kg24 degree plam oil load map 1, and pass into nitrogen, to ensure to be full of nitrogen in crystallizer He in gas piping.Open heating in water bath and stirring, keep the rotating speed of 50r/min, make the grease in crystallizer be warming up to 55 DEG C, insulation 30min, to eliminate crystallization memory.
By the program of upper table 5, the grease slow cooling in crystallizer is continued to stir.When oil temperature 20 DEG C open gas recycle pump, gas in addition via the thermostat water bath temperature adjustment of 15 DEG C, to make the temperature of gas close to 15 DEG C.The valve of adjusting gas flow meter, with the flow velocity of 0.1L/min, to bubble generator, (aperture is 100 μm, Air permenbility is the Bubbled stone of 0.6L/min) in pass into through temperature adjustment nitrogen with produce mean diameter lower than 100 μm microbubble (by microscope sampling observation determine), this microbubble Absorbable organic halogens is present in for some time in grease.
When oil temperature is down to 19 DEG C, be observed visually in crystallizer and produced the uneven nucleus of more size, now stop gas recycle pump.Continue the programmed cooling pressing table 5, cooling secondary crystallization slurry viscosity rises very fast, occurs freezing tank phenomenon, causes to carry out effective solid-liquid separation by filtration.
Reference examples 6
By in the crystallizer of equipment shown in 1.6kg24 degree plam oil load map 1, and pass into nitrogen, to ensure to be full of nitrogen in crystallizer He in gas piping.Open heating in water bath and stirring, keep the rotating speed of 50r/min, make the grease in crystallizer be warming up to 55 DEG C, insulation 30min, to eliminate crystallization memory.
By the program of upper table 5, the grease slow cooling in crystallizer is continued to stir.Gas recycle pump is opened when oil temperature 20 DEG C, the valve of adjusting gas flow meter, with the flow velocity of 0.1L/min pass in bubble generator (aperture is 500 μm, and Air permenbility is the Bubbled stone of 0.6L/min) nitrogen after spiral coil cooling tube temperature adjustment with produce mean diameter lower than 500 μm microbubble (by microscope sampling observation determine).Now stir comparatively violent in crystallizer, produce a large amount of foams.
When oil temperature is down to 19 DEG C, do not observe obvious nucleus, when continuing to be cooled to 18 DEG C, be observed visually in crystallizer and produce the uneven nucleus of more size, now stop gas recycle pump.Continue cooling by the program of table 5, secondary crystallization slurry viscosity rises very fast, occurs freezing tank phenomenon, causes to carry out effective solid-liquid separation by filtration.
With reference to embodiment, specific descriptions have been done to the preferred embodiment of the present invention above, but these descriptions are only illustrative and nonrestrictive.Those skilled in the art, under the prerequisite not departing from marrow of the present invention and scope, can make various apparent change and amendment to these preferred implementations, and these change or amended embodiment still drops in protection scope of the present invention.
Claims (10)
1. oil fractionation method, it passes into the step of bubble in this raw oil material under being included in and raw oil material being in be situated between the condition of steady state, wherein said bubble has about 200 μm or following, the diameter of preferably about 100 μm or following, more preferably from about 50 μm to about 100 μm, gas for the formation of described bubble be under residing condition not with the gas of described raw oil material generation chemical reaction, be preferably selected from nitrogen, helium, carbonic acid gas and their arbitrary combination, described raw oil material is preferably plam oil, is more preferably 24 degree of plam oils.
2. method according to claim 1, wherein the temperature of passed into bubble is lower than the temperature of raw oil material about 1 DEG C to about 3 DEG C, more preferably from about 1 DEG C to about 2 DEG C, preferably the speed that passes into of described bubble is about 0.05-0.1L/min every kilogram grease, is more preferably about 0.05-0.075L/min every kilogram grease.
3. the method according to any one of claim 1-2, wherein saidly raw oil material is in be situated between steady state to comprise described raw oil material to be in make it reach cold and/or the temperature of hypersaturated state, preferably to make 24 degree plam oils as raw oil material be in the temperature of about 19 DEG C to about 25 DEG C, preferred about 20 DEG C to about 21 DEG C.
4. the method according to any one of claim 1-3, wherein cools described raw oil material during bubble passes into step, preferably cools during whole bubble passes into step or in the later stage that bubble passes into step.
5. the method according to any one of claim 1-4, wherein before bubble passes into step, also comprise the step of the fat crystalline substance removing original existence in described raw oil material, preferably include the described raw oil material of heating to eliminate the step of crystallization memory, more preferably comprise and will be heated to about 50 DEG C to about 75 DEG C, the preferred temperature of about 55 DEG C to about 70 DEG C as 24 degree of plam oils of raw oil material, and keep the step of about 10 minutes to about 60 minutes, preferred about 20 to about 40 minutes.
6. the method according to any one of claim 1-5, wherein stop passing into bubble in described raw oil material after the nucleus obtaining aequum, when being preferably to carry out cooling during bubble passes into step, when the temperature of described raw oil material reduce further about 1-2 DEG C or be brought down below the temperature maintaining and be situated between needed for steady state time, stop passing into bubble.
7. the method according to any one of claim 1-6, wherein after bubble passes into step, also comprise cooling described grease and growing the grain to obtain the step of required product.
8. the method according to any one of claim 1-7, comprises the steps:
I) described raw oil material is heated to eliminate crystallization memory, then cooling makes this raw oil material reach the steady state that is situated between, preferably will be heated to about 50 DEG C to about 75 DEG C, the preferred temperature of about 55 DEG C to about 70 DEG C as 24 degree of plam oils of raw oil material, and keep about 10 minutes to about 60 minutes, preferably about 20 minutes to about 40 minutes, be then cooled to the temperature of about 19 DEG C to about 25 DEG C, preferred about 20 DEG C to about 21 DEG C;
Ii) while maintenance cooling, pass in this raw oil material and there is about 200 μm or following, the bubble of the diameter of preferably about 100 μm or following, more preferably from about 50 μm to about 100 μm;
Iii) when the temperature of described raw oil material reduce further about 1-2 DEG C or be brought down below the temperature maintaining and be situated between needed for steady state time, stop passing into bubble; And
Iv) cooling also growing the grain is continued, to obtain required product.
9. for the crystallizer of oil fractionation, it is characterized in that, comprise the container for holding grease, for stirring the whipping appts of grease and the bubble generator for generation of bubble, the bubble exit of this bubble generator is positioned at the bottom of described container, and this bubble generator can produce and has about 200 μm or following, preferably about 100 μm or following, the more preferably from about bubble of diameter of 50 μm to about 100 μm, preferred bubble generator is selected from aperture at about 200 μm or following, preferably about 100 μm or following, the more preferably from about gas cake of 50 μm to about 100 μm, Bubbled stone, the gas dispersion apparatus such as organic membrane and kapillary, preferably the upper surface of described bubble generator is pressed close in the lower end of described whipping appts, and there is the shape matched with described bubble generator upper surface, preferred whipping appts is grid agitator.
10. oil fractionation equipment, it is characterized in that, comprise crystallizer according to claim 9 and provide the refrigerating unit of cooling for described crystallizer, preferably described refrigerating unit is simultaneously also for the gas for producing bubble through bubble generator provides cooling, more preferably described refrigerating unit adopts same heat-eliminating medium to provide cooling for described crystallizer and described gas, thus make the temperature of described gas lower than the grease in described crystallizer about 1 DEG C to about 3 DEG C, more preferably low about 1 DEG C to about 2 DEG C.
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| CN108085133A (en) * | 2017-12-30 | 2018-05-29 | 湘南学院 | A kind of efficient fractionation method of solid-state goose oil and liquid goose oil |
| CN113481248A (en) * | 2021-07-30 | 2021-10-08 | 江南大学 | Method for preparing 1, 3-dioleoyl-2-palmitic acid triglyceride |
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| JP2001200288A (en) * | 2000-01-14 | 2001-07-24 | Tone Corporation:Kk | Method and apparatus for preventing deterioration of oil |
| JP2013053187A (en) * | 2011-09-01 | 2013-03-21 | Kao Corp | Method for producing oil-and-fat composition |
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| CN108085133A (en) * | 2017-12-30 | 2018-05-29 | 湘南学院 | A kind of efficient fractionation method of solid-state goose oil and liquid goose oil |
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| CN113481248A (en) * | 2021-07-30 | 2021-10-08 | 江南大学 | Method for preparing 1, 3-dioleoyl-2-palmitic acid triglyceride |
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Application publication date: 20160406 |