CN104293485A - Method for fractionating and crystallizing palm oil - Google Patents
Method for fractionating and crystallizing palm oil Download PDFInfo
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- CN104293485A CN104293485A CN201410609990.9A CN201410609990A CN104293485A CN 104293485 A CN104293485 A CN 104293485A CN 201410609990 A CN201410609990 A CN 201410609990A CN 104293485 A CN104293485 A CN 104293485A
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- grease
- point
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- cooling
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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
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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
Abstract
The invention discloses a method for fractionating and crystallizing palm oil. Through the adoption of the method, not only is the crystallizing efficiency of the palm oil with the lower content of stearic acids improved, but also the yield of liquid palm oil is improved. The method comprises five steps of oil feeding, heating and crystal destruction, cooling and crystallization, crystal maintenance and filtration, wherein the step of the oil feeding comprises the steps of adding palm oil fat of which the melting point is 26-30 DEG C to palm oil fat to be fractionated, and mixing the two kinds of palm oil fat.
Description
Technical field
The present invention relates to palmitic preparation method field, particularly relate to a kind of palmitic point and carry crystallization method.
Background technology
Plam oil is by the grease extracted in the palm fruit on oil palm tree, and plam oil has abundant nutritive substance and oxidation-resistance, is all widely used in foodstuffs industry and chemical industrial field.Plam oil can carry out point proposing processing, that is by following process, plam oil can be divided into the different several prods of fusing point.Some product main component is stearic acid, and fusing point is generally higher, at normal temperatures in semi-solid state or solid-state; Some product is mainly Palmiticacid (oleic acid), and fusing point is generally lower, is liquid under normal temperature.Stearic fusing point is generally 50 DEG C, and palmitin is generally about 24 DEG C.For the plam oil that stearic acid content is lower, when point to carry in the temperature-fall period of crystallization, due to ctystallizing point lower (ctystallizing point is numerically equal to fusing point), there will be not easily crystallization, crystallization time long, form the phenomenons such as sticky cake, liquid fat yield are low when filtering.
Palmitic point of extracting method mainly contains dry fractionation and solvent point formulation.Wherein dry fractionation refers to and does not add any solvent, is slowly cooled to a certain degree by the grease being in thawing, liquid state completely, then by crystal filtering separation, obtains the method for solid-state fat.Chinese patent CN102719311A discloses a kind of dry fractionation of palm oil method, comprises the steps: raw material plam oil to be heated with stirring to 50 DEG C-75 DEG C; Plam oil after heating is cooled to overcooling, supersaturation; Add crystal seed, the add-on of described crystal seed accounts for 0.3 ﹪-10 ﹪ of described raw material plam oil quality; Place growing the grain; When plam oil iodine number reaches predefine target, filter described plam oil.This dry fractionation method, cooling rate is very fast, and fat crystals cooling required time is shorter, Gu fat is separated comparatively effective with palmitin, quality product is higher.
A solvent point formulation refers to that in grease, add a certain solvent in proportion forms mixing oil system, then carries out crystallisation by cooling, point one carried divides extracting method.Chinese patent CN101939405A discloses a kind of method preparing palm oil products, and the method comprises: (i) when there is not solvent, by plam oil or its ends fraction ground crystallization; (ii) by through the plam oil of partial crystallization and solvent; (iii) by the crystalline mixture that obtains to higher degree; (iv) in the separator the solid obtained is separated from liquid, wherein, when (ii) is front solid is not separated from liquid, the plam oil through partial crystallization formed in (i) or its cut are directly mixed with the solvent in (ii).
The shortcoming of these two kinds of methods is that needs add crystal seed in plam oil or a certain amount of solvent could realize crystallized abstract, not only increases operation steps, and easily introduces impurity.
Therefore, when point carrying the lower grease of stearic acid content, the present invention proposes a kind of new method to solve the problem.
Summary of the invention
The object of this invention is to provide a kind of palmitic point and carried crystallization method, the method achieving does not need to introduce solvent and crystal seed and just can reach good dividing and put forward effect.
The present invention also object solves the not high problem of the crystalline rate of the lower plam oil grease of stearic acid content, can shorten the time of fat crystals and improve palmitic point of liquid palmitic yield when proposing crystallization, making yield be increased to about 50%.
The invention provides a kind of palmitic point and carry crystallization method, comprise: oil-feed, heating broken crystalline substance, crystallisation by cooling, growing the grain and filtration five steps, described oil-feed step comprises: to treating that adding fusing point in point plam oil grease carried is the plam oil grease of 26-30 DEG C and mixes.
In one embodiment of the present invention, in described oil-feed step, fusing point is the addition of the plam oil grease of 26-30 DEG C is the 10-15% mixing rear grease total mass, is preferably 11%.The fusing point adding above-mentioned mass range is that the grease of 26-30 DEG C can the stearic acid content of the original grease of polishing effectively, the ctystallizing point of mixed grease is raised, thus accelerates crystallization velocity, shorten crystallization time, and there will not be sticky cake situation when filtering.When it will be understood by those skilled in the art that sticky cake refers to filtration, because amount of crystals is few, solid and liquid separation insufficient, make the phenomenon that the yield of liquid fat is on the low side.
In the present invention one preferred embodiment, described oil-feed step also comprises the grease mixed is delivered to the process stored in crystallizer.This process is that the crystallization of follow-up grease is prepared, crystallization apparatus used is in the present invention that conventional laboratory, this area is divided and carried device, preferably, shell and tube crystallizer is furnished with in described crystallization apparatus, there is separation cooling jacket inside, carry out preservation and controlling, the finned agitator of the built-in stainless steel of described crystallization apparatus.
Heating of the present invention is broken brilliant step and is referred to the heating of plam oil grease after mixing broken brilliant.Because plam oil grease is in put procedure, sometimes oil temperature is lower than meeting crystallize out during lipid acid ctystallizing point, this part crystal is separated out in non-at the uniform velocity temperature-fall period, crystal formation is different, grain size differs, be unfavorable for uniform growth and the maturation of subsequent crystallographic, so plam oil will first carry out heating brokenly crystalline substance, the small-crystalline of irregularity in this mixture all melted as liquid state.In the present invention one preferred embodiment, Heating temperature is 50-75 DEG C, and the time is 2-4h.In a preferred mode, Heating temperature is 60 DEG C, and the time is 3h.
The heating unit that this area is suitable can be used in described heating steps, be preferably water bath.Because water bath can make Heating temperature even, avoid the situation occurring local superheating.
It will be appreciated by those skilled in the art that, temperature range and the time of heating are not changeless, as long as original crystal in grease can be made all to melt and melt fully, but the setting of top temperature can not exceed makes lubricant component decomposition rotten, the scope that heat-up time can set with antipyretic temperature correspondingly changes, namely, when Heating temperature setting is higher, heat-up time can be shorter; When Heating temperature setting is lower, heat-up time is longer.But in the present invention one preferred embodiment, described heating is broken in brilliant step and is kept 5-60min in the temperature that heating is the highest, is preferably 15-60min, is more preferably 40-60min.Above-mentionedly keep for some time in top temperature, the original crystal in grease can be made to melt fully thoroughly.
The step of crystallisation by cooling described in the present invention is Tc point grease being cooled to grease.In the present invention one preferred embodiment, first with the temperature difference of per minute 3-5 DEG C cooling, lower the temperature with the temperature difference of per minute 0.5-1 DEG C again close to during Tc point.In the present invention one preferred embodiment, the temperature starting to lower the temperature is higher than Tc point 5 DEG C.The present invention another preferred embodiment in, described is 18-20 DEG C close to Tc point, is 19 DEG C in one more optimal way.In temperature-fall period, amount of grease reaches ctystallizing point, starts to form little nucleus particle, prolongation in time, and nucleus quantity gets more and more.It will be understood by those skilled in the art that nucleus is not yet formed when starting to lower the temperature, therefore cooling rate can be accelerated to shorten temperature fall time, and near the Tc point of liquid fat, time generally to 19 DEG C, with comparatively jogging speed cooling, crystallization is carried out under uniform speed.
In the present invention one preferred embodiment, the cooling in described crystallisation step is undertaken by agitator, and stirring frequency is at 30-60Hz.It will be understood by those skilled in the art that agitator can monitor grease temperature in real time, be convenient to change stirring frequency.By regulating the stirring frequency of agitator to realize cooling rate, need fast cooling during beginning, stirring frequency is relatively higher, treats that temperature drops to 18-20 DEG C, preferably after 19 DEG C, relatively reduces stirring velocity.
In the present invention one preferred embodiment, crystallization time is 15-20h, is preferably 18h.The temperature starting slowly to separate out due to crystal than normal crystallization temperature height 2-3 DEG C, when crystallization velocity is faster than normal crystallization speed 10-15%, crystallization time is faster than normal crystallization time 2-3 are little.
It will be appreciated by those skilled in the art that, normal crystallization temperature mentioned here, normal crystallization speed, normal crystallization time are all that now grease does not add dystectic grease in advance for the crystallisation process of the lower plam oil grease of simple stearic acid content.
Growing the grain described in the method refers to and stops cooling, and allow between nucleus and combine the larger nucleus particle of formation, and extend increasing in time, general rearing crystal time is 5-10h, makes crystal growth complete.In the present invention one preferred embodiment, rearing crystal time is 6h.
Filtration step of the present invention refers to and solid-state crystalline particle and liquid oil is made a distinction, and oil temperature during preferred described filtration, at 13-15 DEG C, is more preferably 13.5 DEG C.It will be understood by those skilled in the art that because crystallisation process is exothermic process, if crystallization is too fast, heat release not in time, can cause phenomenon of rising again.Filtration temperature of the present invention can prevent from rising again, and avoids filtration insufficient.Filtering described in the method is filtered out by crystal grain with filtration unit, thus separates with the grease of liquid state, and filtration unit used is pressure filter.In the present invention one preferred embodiment, filtration unit used is membrane type press filter, and filtration capacity is 0.8/1.4 liter, squeeze pressure 0-30bar.Under the pressure of 15bar, the thickness of filter cake is at 40mm.
In the present invention's embodiment, carry crystallization method, comprising for described palmitic point:
(1) oil-feed: the fusing point to grease total mass 10-15% after adding in point plam oil grease carried and accounting for mixing is the plam oil grease of 26-30 DEG C, makes the two mix;
(2) heating is broken brilliant: be heated to 50-75 DEG C to the grease of mixing, and keeps 40-60min when being heated to top temperature, and overall heat-up time is 2-4h;
(3) crystallisation by cooling: grease is lowered the temperature, after being first cooled to 18-20 DEG C with the temperature difference of per minute 3-5 DEG C, be cooled to the Tc point of grease with the temperature difference of per minute 0.5-1 DEG C, total crystallization time is at 15-20h;
(4) growing the grain: stop grease cooling, carry out growing the grain, overall rearing crystal time is at 5-10h.
(5) filter: treat that temperature drops to after 13-15 DEG C, solid granulates is separated with the grease filtrating of liquid state.
The method that the present invention proposes has following outstanding technical superiority:
1. the present invention uses high-melting-point, namely the plam oil that stearic acid content is higher with treat point to carry plam oil, namely the plam oil that stearic acid content is lower carries out mixing and dividing carrying, improve and treat point to carry palmitic Tc point, make it reach normal point and put forward level of crystallization, in crystallization overall process, can shorten overall time 2-3 hour, crystalline rate significantly improves; Solve simultaneously the lower plam oil of stearic acid content point to carry filter in process time the problems such as not easily separated, sticky cake, yield be low.
2. do not need to add crystal seed and solvent promotion crystal structure in crystallisation process, thus decrease procedure of processing, and do not introduce other impurity.
Embodiment
Below in conjunction with embodiment, the present invention is further elaborated.
Embodiment 1
(1) oil-feed: the fusing point to grease total mass 10% after adding in the plam oil grease point to carry and accounting for mixing is the plam oil grease of 26 DEG C, makes the two fully mix, and be delivered in crystallizer and keep in.
(2) heat: be heated to 50 DEG C by the grease of water bath to mixing and carry out brokenly brilliant process, be warming up to 60 DEG C and keep 60min, make thawing fully thorough, overall heat-up time is 4h.
(3) crystallization: lowered the temperature to grease with the temperature difference of per minute 3-5 DEG C cooling with 40Hz stirring velocity by agitator, after dropping to 18 DEG C, is reduced frequency to 30Hz, is cooled to the Tc point of grease with the temperature difference of per minute 0.5-1 DEG C; Overall crystallization time is at about 15h.
(4) growing the grain: combine between nucleus and form larger particle, and extend increasing in time; Rearing crystal time is 5h.
(5) filter: treat that temperature drops to after 13 DEG C, with membrane type press filter, solid granulates is filtered out, thus make a distinction with the grease of liquid state.
Through aforesaid method divide carry after the liquid plam oil of yield be increased to about 50%.
Embodiment 2
(1) oil-feed: the fusing point to grease total mass 11% after adding in the plam oil grease point to carry and accounting for mixing is the plam oil grease of 28 DEG C, makes the two fully mix, and be delivered in crystallizer and keep in.
(2) heat: be heated to 60 DEG C by the grease of water bath to mixing and carry out brokenly brilliant process, be warming up to top temperature 70 DEG C and keep 55min, making thawing fully thorough; Overall heat-up time is 3h.
(3) crystallization: lowered the temperature to grease with the temperature difference of per minute 3-5 DEG C cooling with 50Hz stirring velocity by cooling agitator, after dropping to 19 DEG C, is reduced frequency to 30Hz, is cooled to the Tc point of grease with the temperature difference of per minute 0.5-1 DEG C; Overall crystallization time is at about 18h.
(4) growing the grain: combine between nucleus and form larger particle, and extend increasing in time, rearing crystal time is 6h.
(5) filter: treat that temperature drops to after 13.5 DEG C, with membrane type press filter, solid granulates is filtered out, thus make a distinction with the grease of liquid state.
Through aforesaid method divide carry after liquid plam oil yield be increased to about 50%.
Embodiment 3
(1) oil-feed: the fusing point to grease total mass 15% after adding in the plam oil grease point to carry and accounting for mixing is 30 DEG C of plam oil greases, makes the two fully mix, and be delivered in crystallizer and keep in.
(2) heat: be heated to 70 DEG C by the grease of water bath to mixing and carry out brokenly brilliant process, be warming up to top temperature point 75 DEG C and keep 40min, making thawing fully thorough; Overall heat-up time is 2h.
(3) crystallization: lowered the temperature to grease with the temperature difference of per minute 3-5 DEG C cooling with 60Hz stirring velocity by agitator, after dropping to 20 DEG C, is reduced frequency to 30Hz, is cooled to the Tc point of grease with the temperature difference of per minute 0.5-1 DEG C; Overall crystallization time is at about 20h.
(4) growing the grain: combine between nucleus and form larger particle, and extend increasing in time, rearing crystal time is 10h.
(5) filter: treat that temperature drops to after 15 DEG C, with membrane type press filter, solid granulates is filtered out, thus make a distinction with the grease of liquid state.
Through aforesaid method divide carry after liquid plam oil yield be increased to about 50%.
What it will be understood by those skilled in the art that the crystal after filtration is stearic acid, mainly for the manufacture of oleomargarine and shortening; Filtering the filtrate portion obtained is Palmiticacid, is fabulous frying oil, thus reaches by dividing the product carrying crystallization acquisition different melting points.
The present invention adds the dystectic palmitic method of certain proportion by treating point plam oil carried, the plam oil lower to stearic acid content carries out point proposing crystallization, do not introduce crystal seed and other solvents in whole process, not only increase Tc point, thus improve crystalline rate; And solve the lower grease of stearic acid content and point putting forward some the intrinsic problems existed in process, as sticky cake phenomenon etc., from and make liquid palmitic yield have also been obtained raising.Whole process equipment therefor is the known and devices that are that easily obtain of these those skilled in the art, makes the method be suitable for promoting.
This specification sheets above in conjunction with embodiment to invention has been explaination, but should be understood that these describe and explaination just in order to understand the present invention better, and not form any restriction of the present invention.Those skilled in the art can carry out necessary change to the specific embodiment of the present invention and not depart from the spirit and scope of the present invention after having read present specification.Protection scope of the present invention is limited by the accompanying claims, and covers the equivalents of claim.
Claims (10)
1. carry crystallization method for one kind palmitic point, comprise: oil-feed, heating broken crystalline substance, crystallisation by cooling, growing the grain and filtration five steps, it is characterized in that, described oil-feed step comprises: to treating that adding fusing point in point plam oil grease carried is the plam oil grease of 26-30 DEG C and mixes.
2. method according to claim 1, is characterized in that, in described oil-feed step, the addition of plam oil grease of fusing point 26-30 DEG C is the 10-15% of grease total mass after mixing.
3. method according to claim 1, is characterized in that, the Heating temperature that brilliant step is broken in described heating is 50-75 DEG C, and the time is 2-4h.
4. method according to claim 3, is characterized in that, described heating is broken brilliant step and is included in the highest temperature maintenance 5-60min of heating.
5. method according to claim 1, it is characterized in that, the step of described crystallisation by cooling comprises first with the temperature difference of per minute 3-5 DEG C cooling, during close to Tc point, again with the temperature difference of per minute 0.5-1 DEG C cooling, described is 18-20 DEG C close to Tc point.
6. method according to claim 5, is characterized in that, described crystallisation by cooling step is lowered the temperature by agitator, and stirring frequency is 30-60Hz.
7. the method according to claim 5-6 any one, is characterized in that, the crystallization time in described crystallisation step is 15-20h.
8. method according to claim 1, is characterized in that, the oil temperature of carrying out in described filtration step filtering is at 13-15 DEG C.
9. method according to claim 1, described oil-feed step specifically comprises:
(1) oil-feed: the fusing point to grease total mass 10-15% after adding in point plam oil grease carried and accounting for mixing is the plam oil grease of 26-30 DEG C, makes the two mix;
(2) heating is broken brilliant: be heated to 50-75 DEG C to the grease of mixing, and keeps 40-60min when being heated to top temperature, and overall heat-up time is 2-4h;
(3) crystallisation by cooling: grease is lowered the temperature, after being first cooled to 18-20 DEG C with the temperature difference of per minute 3-5 DEG C, be cooled to the Tc point of grease with the temperature difference of per minute 0.5-1 DEG C, total crystallization time is at 15-20h;
(4) growing the grain: stop grease cooling, carry out growing the grain, overall rearing crystal time is at 5-10h.
(5) filter: treat that temperature drops to after 13-15 DEG C, solid granulates is separated with the grease filtrating of liquid state.
10. method according to claim 9, described heating is broken in brilliant step and is adopted water bath to heat.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410609990.9A CN104293485A (en) | 2014-11-03 | 2014-11-03 | Method for fractionating and crystallizing palm oil |
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| CN201410609990.9A CN104293485A (en) | 2014-11-03 | 2014-11-03 | Method for fractionating and crystallizing palm oil |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105394205A (en) * | 2015-10-20 | 2016-03-16 | 广州市至润油脂食品工业有限公司 | Shortening composition |
| CN110915943A (en) * | 2019-12-18 | 2020-03-27 | 天津农学院 | Method for extracting beef oil |
-
2014
- 2014-11-03 CN CN201410609990.9A patent/CN104293485A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105394205A (en) * | 2015-10-20 | 2016-03-16 | 广州市至润油脂食品工业有限公司 | Shortening composition |
| CN110915943A (en) * | 2019-12-18 | 2020-03-27 | 天津农学院 | Method for extracting beef oil |
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Application publication date: 20150121 |