CN102388988B - Separated extraction method of microorganism oil - Google Patents
Separated extraction method of microorganism oil Download PDFInfo
- Publication number
- CN102388988B CN102388988B CN 201110350200 CN201110350200A CN102388988B CN 102388988 B CN102388988 B CN 102388988B CN 201110350200 CN201110350200 CN 201110350200 CN 201110350200 A CN201110350200 A CN 201110350200A CN 102388988 B CN102388988 B CN 102388988B
- Authority
- CN
- China
- Prior art keywords
- oil
- solid
- surfactant solution
- microbial oil
- aqueous surfactant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 244000005700 microbiome Species 0.000 title abstract description 12
- 238000000605 extraction Methods 0.000 title abstract 3
- 239000004094 surface-active agent Substances 0.000 claims abstract description 89
- 239000007787 solid Substances 0.000 claims abstract description 75
- 239000013078 crystal Substances 0.000 claims abstract description 46
- 238000000034 method Methods 0.000 claims abstract description 43
- 239000007788 liquid Substances 0.000 claims abstract description 42
- 239000004519 grease Substances 0.000 claims abstract description 38
- 239000002002 slurry Substances 0.000 claims abstract description 33
- 238000003756 stirring Methods 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000000839 emulsion Substances 0.000 claims abstract description 18
- 238000002425 crystallisation Methods 0.000 claims abstract description 10
- 230000008025 crystallization Effects 0.000 claims abstract description 7
- 238000009413 insulation Methods 0.000 claims abstract description 7
- 239000003921 oil Substances 0.000 claims description 138
- 230000000813 microbial effect Effects 0.000 claims description 87
- 239000012530 fluid Substances 0.000 claims description 38
- 150000003839 salts Chemical class 0.000 claims description 24
- 230000008014 freezing Effects 0.000 claims description 16
- 238000007710 freezing Methods 0.000 claims description 16
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 14
- 239000007790 solid phase Substances 0.000 claims description 14
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 13
- 238000005119 centrifugation Methods 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 11
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 10
- 235000011152 sodium sulphate Nutrition 0.000 claims description 10
- 239000000470 constituent Substances 0.000 claims description 9
- 230000001804 emulsifying effect Effects 0.000 claims description 8
- 230000004927 fusion Effects 0.000 claims description 8
- 239000012071 phase Substances 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 8
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical group OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 7
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 7
- -1 sodium alkyl sulfate Chemical class 0.000 claims description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- 229940077388 benzenesulfonate Drugs 0.000 claims description 4
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 150000004996 alkyl benzenes Chemical class 0.000 claims 1
- 239000006228 supernatant Substances 0.000 claims 1
- 238000001816 cooling Methods 0.000 abstract description 14
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 48
- 239000003925 fat Substances 0.000 description 31
- 235000019197 fats Nutrition 0.000 description 31
- 241000894006 Bacteria Species 0.000 description 11
- YZXBAPSDXZZRGB-DOFZRALJSA-N arachidonic acid Chemical compound CCCCC\C=C/C\C=C/C\C=C/C\C=C/CCCC(O)=O YZXBAPSDXZZRGB-DOFZRALJSA-N 0.000 description 10
- 238000005194 fractionation Methods 0.000 description 10
- 230000008569 process Effects 0.000 description 10
- 150000002632 lipids Chemical class 0.000 description 9
- 239000002904 solvent Substances 0.000 description 9
- 238000002844 melting Methods 0.000 description 8
- 230000008018 melting Effects 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 230000015556 catabolic process Effects 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 235000021342 arachidonic acid Nutrition 0.000 description 5
- 229940114079 arachidonic acid Drugs 0.000 description 5
- 238000009472 formulation Methods 0.000 description 5
- 235000020978 long-chain polyunsaturated fatty acids Nutrition 0.000 description 5
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 4
- JAZBEHYOTPTENJ-JLNKQSITSA-N all-cis-5,8,11,14,17-icosapentaenoic acid Chemical compound CC\C=C/C\C=C/C\C=C/C\C=C/C\C=C/CCCC(O)=O JAZBEHYOTPTENJ-JLNKQSITSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000008280 blood Substances 0.000 description 3
- 210000004369 blood Anatomy 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 235000020673 eicosapentaenoic acid Nutrition 0.000 description 3
- 229960005135 eicosapentaenoic acid Drugs 0.000 description 3
- JAZBEHYOTPTENJ-UHFFFAOYSA-N eicosapentaenoic acid Natural products CCC=CCC=CCC=CCC=CCC=CCCCC(O)=O JAZBEHYOTPTENJ-UHFFFAOYSA-N 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 230000035800 maturation Effects 0.000 description 2
- 230000000050 nutritive effect Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- 235000019737 Animal fat Nutrition 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- SBJKKFFYIZUCET-JLAZNSOCSA-N Dehydro-L-ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(=O)C1=O SBJKKFFYIZUCET-JLAZNSOCSA-N 0.000 description 1
- PVNIQBQSYATKKL-UHFFFAOYSA-N Glycerol trihexadecanoate Natural products CCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCC PVNIQBQSYATKKL-UHFFFAOYSA-N 0.000 description 1
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229940121363 anti-inflammatory agent Drugs 0.000 description 1
- 239000002260 anti-inflammatory agent Substances 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003225 biodiesel Substances 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000002490 cerebral effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 235000012000 cholesterol Nutrition 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- MBMBGCFOFBJSGT-KUBAVDMBSA-N docosahexaenoic acid Natural products CC\C=C/C\C=C/C\C=C/C\C=C/C\C=C/C\C=C/CCC(O)=O MBMBGCFOFBJSGT-KUBAVDMBSA-N 0.000 description 1
- 235000020669 docosahexaenoic acid Nutrition 0.000 description 1
- 239000008157 edible vegetable oil Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 235000021149 fatty food Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000002218 hypoglycaemic effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000035772 mutation Effects 0.000 description 1
- 210000001640 nerve ending Anatomy 0.000 description 1
- 210000004126 nerve fiber Anatomy 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 235000014593 oils and fats Nutrition 0.000 description 1
- 235000019629 palatability Nutrition 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000020777 polyunsaturated fatty acids Nutrition 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000004491 retinal development Effects 0.000 description 1
- 230000001932 seasonal effect Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000004614 tumor growth Effects 0.000 description 1
- 235000019871 vegetable fat Nutrition 0.000 description 1
Images
Landscapes
- Fats And Perfumes (AREA)
Abstract
The invention relates to a separated extraction method of microorganism oil, which is characterized by comprising the following steps: firstly, homogenizing, stirring microorganism oil to be in separated extraction uniformly; secondly, breaking crystals; thirdly, cooling and crystallizing, crystallizing the heat-insulation microorganism oil for 4-7h at the temperature being 4 DEG C, and then arranging the heat-insulation microorganism oil for 1-4h at the low temperature being 10 DEG C, thus obtaining thick slurry containing solid crystallization; fourthly, adding surface active agent water solution in the thick slurry containing solid crystallization, and stirring, thus obtaining elusion system; fifthly, conducting centrifugal separation to obtain liquid oil, standing the emulsion system for 1-5h at the low temperature being 5-10 DEG C, centrifuging the emulsion system in a cooling centrifuge, separating liquid components in a light phase mode, putting the liquid components in light phase in water for cleaning, and dehydrating and drying the liquid components in light phase, thus obtaining the liquid oil of the microorganism oil; and sixthly, breaking the emulsion to obtain solid grease. The liquid oil of the microorganism separated and extracted by the method is not easy to solidify at lower temperature, the method procedure is simple and the cost is low.
Description
Technical field
The invention belongs to the Food Science field, be specifically related to a kind of minute extracting method of microbial oil.
Background technology
Microbial grease is another the human edible oil and fat new resources that develops after vegetable fat, animal fat.Microbial grease claims again Unicell Oils and Fats, is that to utilize carbohydrate, hydrocarbon and common grease under certain condition be carbon source, nitrogenous source, be aided with grease and other lipids with commercial value of production of inorganic by microorganisms such as yeast, mould, bacterium and algae.The micro-organisms grease not only have fat content high, with short production cycle, be not subjected to seasonal effect, the advantage such as do not occupy cultivated land, and the method such as available Fusion of Cells, cell mutation, make the grease of microorganisms high-nutrition oil fat or some special fatty acid composition, as contain the functional grease of the long-chain polyunsaturated fatty acids (LC-PUFAs) such as arachidonic acid (ARA), eicosapentaenoic acid (EPA), DHA (DHA).LC-PUFAs has obvious effect at aspects such as angiocardiopathy preventing, reducing blood lipid, reduction cholesterol, fat-reducing, inhibition tumor growth, anti-inflammatories.Since the nineties in 20th century, the production that the development and use microorganism carries out functional grease has become a large focus, as utilizes microorganism to cultivate and produce the research that ARA, EPA, DHA etc. are of high nutritive value and have the biodiesel of special health care.ARA belongs to the serial long-chain polyunsaturated fatty acid of ω-6 (LC-PUFA), it is widely distributed in human body, content generally accounts for 40%～50% of polyunsaturated fatty acid total amount in brain and nerve fiber, at nerve endings more up to 70%, to cerebral function and the retinal development material that is absolutely necessary; In addition, ARA also has the function of enhancing development and the effect of hypoglycemic, reducing blood lipid and reduction Blood Cholesterol.
But microbial oil can occur solidifying when low tempertaure storage, just can become solid-state or semisolid when low such as temperature in the winter time, not only causes the oil product poor mobile performance, and inconvenience is used, and is difficult for storage; The transparency of oil product is reduced, the palatability variation, thus reduced the quality of nutritive value and the fatty foods of microbial oil.Oil fractionation is according to different fatty acid triglycercide fusing point differences in the grease, makes high melting point component produce crystallization by cooling, after filtration or centrifugation obtain the different component of fusing point.Oil fractionation can be classified into relatively single product with forming complicated natural oil, realize the fluid oil of different melting points and separating of solid fat, to improve grease to the conformability of different instructions for uses, enlarge the purposes of grease, improve use value and the economic worth of grease.
At present the oil fractionation technology mainly contains dry fractionation, solvent and divides to carry dividing with surfactant and carry.Dry fractionation refers to not add any solvent, and the grease that will be in dissolved state slowly is cooled to a certain degree, and the method for solid ester is separated out in then isolated by filtration crystallization.Dry fractionation is divided into three steps: heat treated; Form crystal atoms nuclear and allow crystal growing and maturation with cooling method; With filtering palmitin is separated from solid.Although dry fractionation has its advantage, dry fractionation efficient is low, and liquid oil contents is higher in the solid-state fat, makes the brilliant level of solid-state fat and fluid oil low.A solvent minute formulation refers to add in proportion a certain solvent and forms the miscella system in grease, then carry out crystallisation by cooling, divide a kind of minute extracting method of carrying.Solvent divides formulation can form the stable crystalline that easily filters, and improves separating effect, increases isolated yield, shortens disengaging time, improves the purity of products of separated.A solvent minute formulation divides that to put forward efficient high, and solid-state fat constituent mass is good.Yet because crystallization temperature is low and minute carry and to relate to solvent loss in the process, its investment is larger, and producing cost is high, is used as the hexane of solvent, acetone, and isopropyl alcohols etc. have inflammability.A surfactant minute formulation refers to behind the grease crystallisation by cooling, adds surfactant, improves the interfacial tension of oil and fat, borrows the affinity between fat and surfactant, forms the suspension of fat in aqueous surfactant solution, promotes the method for the brilliant segregation of fat.The operations such as its technique comprises that crystallisation by cooling, surfactant are moistening, centrifugation and surfactant recovery.Surfactant method divides that to put forward separative efficiency high, superior product quality, and purposes is wide, is applicable to large-scale production.
Summary of the invention
In order to solve the microbial oil problem that (10-20 ℃) easily solidifies when temperature is low, minute extracting method that the purpose of this invention is to provide a kind of microbial oil, the method divides the fluid oil (10-20 ℃) when temperature is low of the microbial oil of proposition to be difficult for solidifying, and the method operation is simple, cost is low.
To achieve these goals, technical scheme of the present invention is: a kind of minute extracting method of microbial oil is characterized in that it comprises the steps:
1) homogenizing: will treat that the microbial oil (or claiming microbial grease) of minute carrying stirs;
2) break crystalline substance: after the microbial oil that stirs is warming up to 25-30 ℃, insulation 5-10min;
Microbial grease destroys at freezing front inhomogeneous nucleus with self-assembling formation, and microbial grease is in refining, transportation, storage process, because the microbial grease temperature is lower than solid-state fat freezing point and crystallize out; This part crystal is owing to separating out in non-at the uniform velocity temperature-fall period, crystal formation is different, grain size differs, when forwarding freezing and crystallizing to after the stage, even growth and the maturation that can be unfavorable for the fat crystalline substance make crystalline solid itself produce defective, affect oil fractionation, broken crystalline substance is warming up to the grease melting more than the solid-state fat fusing point usually, keeps 5-10min;
3) freezing and crystallizing (the gradually process of cooling): with step 2) microbial oil after the insulation is in 4 ℃ of crystallization 4-7h (abundant under the cryogenic conditions), place again 1-4h under 10 ℃ of cryogenic conditions, obtain containing the viscous slurry (having formed the viscous slurry that contains solid crystal after lipid material process cooling this moment is freezing) of solid crystal;
4) adding of surfactant solution: by the viscous slurry that contains solid crystal: the volume ratio of aqueous surfactant solution=1: 0.5-1: 2, choose the viscous slurry and the aqueous surfactant solution that contain solid crystal; Wherein, aqueous surfactant solution is comprised of surfactant, inorganic salts and water, and the concentration of surfactant is 0.08-0.4wt%, and the concentration of inorganic salts is 0.5-3wt%;
In the viscous slurry that contains solid crystal, add aqueous surfactant solution, stir 0.5-1.0h, obtain the emulsion system;
Fully stirring is uniformly dispersed mixed system and forms the emulsion system, liquid component in the grease maintenance liquid phase that carries on as before, can not be wetting and under stirring action, become fine droplets and be scattered in the aqueous solution by surfactant, and the crystalline particle that is wrapped up by surfactant molecule is fully wetting because obtaining, got rid of the liquid component that invests crystal plane, so be transferred to aqueous phase;
5) centrifugation gets liquid oils: with step 4) emulsifying liquid lie in 5-10 ℃ of cryogenic conditions and leave standstill 0.5-5h, centrifugal in refrigerated centrifuge, liquid component is just gently to tell mutually, add entry and clean by dehydrating (20-25 ℃ of dry 2-6h), namely get the fluid oil (product) of microbial oil;
The aqueous surfactant solution of solid crystal of suspending is then told with heavy phase, obtains solid phase grease mixed liquor.
Surfactant is lauryl sodium sulfate (SDS), sodium alkyl benzene sulfonate or sodium alkyl sulfate etc.
Inorganic salts are magnesium sulfate (MgSO
4), sodium sulphate, aluminum sulfate or sodium chloride etc.
Step 5) condition of described centrifugation is: 3000-6000rpm, centrifugal 5-10min.
6) get solid fat behind the breakdown of emulsion: after taking out the fluid oil (being liquid component) of microbial oil, the solid phase grease mixed liquor of gained is processed 2-10min through 80-95 ℃ of heating demulsification type, watery fusion, solid constituent is namely separated with water, the water that removes sub-cloud namely obtains the solid fat component, add entry and wash the aqueous surfactant solution of removing remnants, after dehydrating, the solid that namely gets microbial oil is stearic.
The present invention divides the fluid oil of carrying rear microbial bacteria oil (being the product that will obtain required for the present invention), and clearing time is 120h above (its physical and chemical index sees Table 1) under 10 ℃ of conditions.This invention has solved the microbial oil problem that (＜20 ℃) easily solidify when temperature is low, thereby has improved use value and the economic worth of microbial grease.
The comparison of table 1 physical and chemical index (embodiment 1-5)
The invention has the beneficial effects as follows:
1) the method divides the fluid oil (10-20 ℃) when temperature is low of the microbial oil of proposition to be difficult for solidifying.The present invention divides the fluid oil of carrying rear microbial bacteria oil (being the product that will obtain required for the present invention), and clearing time is more than the 120h under 10 ℃ of conditions.
The fluid oil fusing point of the microbial oil that obtains after minute carrying is low, and frost resistance is strong, and still keep liquid winter in south, can be used as the situation that the ready-mixed oil component also can change the inconvenience of microbial oil use in winter, enriches grease market.
2) the method operation is simple, does not need complex device.
The present invention compares with dry fractionation to have with short production cyclely, and separative efficiency is high, the advantage that production process is easy to control; Comparing with a solvent minute formulation does not need with an organic solvent, thereby safety, and equipment investment is few, and cost is lower.
3) fluid oil of microbial oil (product) better quality, the yield of liquid oil is higher, without any the pollution of organic solvent;
4) used surfactant is reused after can reclaiming in the technique;
5) owing to not needing complex device and need not use organic solvent, save great deal of investment, operating cost, thereby reduced production cost, be applicable to suitability for industrialized production.
Description of drawings
Fig. 1 is process chart of the present invention.
The specific embodiment
In order to understand better the present invention, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
Embodiment 1:
As shown in Figure 1, a kind of minute extracting method of microbial oil, it comprises the steps:
1) homogenizing: will treat that the microbial oil of minute carrying stirs;
2) broken brilliant: as the microbial oil melting that stirs to be warming up to (25 ℃) more than the solid-state fat fusing point, to keep 5min;
3) freezing and crystallizing: with step 2) the microbial oil sufficient crystallising 5h under 4 ℃ of cryogenic conditions after the insulation, place again 10 ℃ of cryogenic thermostat water-bath 2h, obtain containing the viscous slurry (having formed the viscous slurry that contains solid crystal after lipid material process cooling this moment is freezing) of solid crystal;
4) adding of surfactant solution: by the viscous slurry that contains solid crystal: the volume ratio of aqueous surfactant solution=1: 1, choose the viscous slurry and the aqueous surfactant solution that contain solid crystal; Wherein, aqueous surfactant solution is comprised of surfactant, inorganic salts and water, and the concentration of surfactant is 0.4wt%, and the concentration of inorganic salts is 1wt%;
Surfactant is lauryl sodium sulfate (SDS); Inorganic salts are magnesium sulfate (MgSO
4);
In the viscous slurry that contains solid crystal, add aqueous surfactant solution, stir 0.5h, obtain the emulsion system;
5) centrifugation gets liquid oils: with step 4) emulsifying liquid lie in 10 ℃ of cryogenic conditions and leave standstill 0.5h, centrifugal in refrigerated centrifuge, liquid component is just gently to tell mutually (oily referred to as liquid among Fig. 1), adding entry cleans by dehydrating (20 ℃ of dry 6h), namely get the fluid oil (product, yield are 59.9%) of microbial oil;
The aqueous surfactant solution of solid crystal of suspending is then told (as solid phase grease mixed liquor) take heavy phase;
6) get solid fat behind the breakdown of emulsion: after taking out the fluid oil (being liquid component) of microbial oil, the solid phase grease mixed liquor of gained is processed 2-10min through 90 ℃ of heating demulsification types, watery fusion, solid constituent is namely separated with water, the water that removes sub-cloud namely obtains the solid fat component, add entry and wash and remove remaining aqueous surfactant solution, after dehydrating, the solid that namely gets microbial oil stearic (among Fig. 1 referred to as solid fat).Surplus solution is surfactant solution, recycling after reclaiming.
The present embodiment divides the fluid oil of carrying rear microbial bacteria oil, and clearing time is 120h above (its physical and chemical index sees Table 1) under 10 ℃ of conditions.Illustrate that the method divides the fluid oil (10-20 ℃) when temperature is low of the microbial oil of proposition to be difficult for solidifying.
Embodiment 2:
A kind of minute extracting method of microbial oil, it comprises the steps:
1) homogenizing: will treat that the microbial oil of minute carrying stirs;
2) broken brilliant: as the microbial oil melting that stirs to be warming up to (30 ℃) more than the solid-state fat fusing point, to keep 5min;
3) freezing and crystallizing: with microbial oil sufficient crystallising 5h under 4 ℃ of cryogenic conditions, place again 10 ℃ of cryogenic thermostat water-bath 2h, obtain containing the viscous slurry (having formed the viscous slurry that contains solid crystal after lipid material process cooling this moment is freezing) of solid crystal;
4) adding of surfactant solution: by the viscous slurry that contains solid crystal: the volume ratio of aqueous surfactant solution=1: 1, choose the viscous slurry and the aqueous surfactant solution that contain solid crystal; Wherein, aqueous surfactant solution is comprised of surfactant, inorganic salts and water, and the concentration of surfactant is 0.4wt%, and the concentration of inorganic salts is 2wt%;
Surfactant is lauryl sodium sulfate (SDS); Inorganic salts are magnesium sulfate (MgSO
4);
In the viscous slurry that contains solid crystal, add aqueous surfactant solution, stir 1.0h, obtain the emulsion system;
5) centrifugation gets liquid oils: with step 4) emulsifying liquid lie in 10 ℃ of cryogenic conditions and leave standstill 1h, centrifugal in refrigerated centrifuge, liquid component is just gently to tell mutually, adding entry cleans by dehydrating (25 ℃ of dry 6h), namely get the fluid oil (product, yield are 57.1%) of microbial oil;
The aqueous surfactant solution of solid crystal of suspending is then told (as solid phase grease mixed liquor) take heavy phase;
6) get solid fat behind the breakdown of emulsion: after taking out the fluid oil (being liquid component) of microbial oil, the solid phase grease mixed liquor of gained is processed 2-10min through 90 ℃ of heating demulsification types, watery fusion, solid constituent is namely separated with water, the water that removes sub-cloud namely obtains the solid fat component, add entry and wash the aqueous surfactant solution of removing remnants, after dehydrating, the solid that namely gets microbial oil is stearic.
The present embodiment divides the fluid oil of carrying rear microbial bacteria oil, and clearing time is 120h above (its physical and chemical index sees Table 1) under 10 ℃ of conditions.Illustrate that the method divides the fluid oil (10-20 ℃) when temperature is low of the microbial oil of proposition to be difficult for solidifying.
Embodiment 3:
A kind of minute extracting method of microbial oil, it comprises the steps:
1) homogenizing: will treat that the microbial oil of minute carrying stirs;
2) broken brilliant: as the microbial oil melting that stirs to be warming up to (28 ℃) more than the solid-state fat fusing point, to keep 5min;
3) freezing and crystallizing: with microbial oil sufficient crystallising 5h under 4 ℃ of cryogenic conditions, place again 10 ℃ of cryogenic thermostat water-bath 2h, formed the viscous slurry that contains solid crystal after lipid material process cooling this moment is freezing;
4) adding of surfactant solution: by the viscous slurry that contains solid crystal: the volume ratio of aqueous surfactant solution=1: 1.5, choose the viscous slurry and the aqueous surfactant solution that contain solid crystal; Wherein, aqueous surfactant solution is comprised of surfactant, inorganic salts and water, and the concentration of surfactant is 0.4wt%, and the concentration of inorganic salts is 1wt%;
Surfactant is lauryl sodium sulfate (SDS); Inorganic salts are magnesium sulfate (MgSO
4);
In the viscous slurry that contains solid crystal, add aqueous surfactant solution, stir 0.8h, obtain the emulsion system;
5) centrifugation gets liquid oils: with step 4) emulsifying liquid lie in 10 ℃ of cryogenic conditions and leave standstill 2h, centrifugal in refrigerated centrifuge, liquid component is just gently to tell mutually, adding entry cleans by dehydrating (22 ℃ of dry 4h), namely get the fluid oil (product, 56.8%) of microbial oil;
The aqueous surfactant solution of solid crystal of suspending is then told (as solid phase grease mixed liquor) take heavy phase;
6) get solid fat behind the breakdown of emulsion: after taking out the fluid oil (being liquid component) of microbial oil, the solid phase grease mixed liquor of gained is processed 2-10min through 80 ℃ of heating demulsification types, watery fusion, solid constituent is namely separated with water, the water that removes sub-cloud namely obtains the solid fat component, add entry and wash the aqueous surfactant solution of removing remnants, after dehydrating, the solid that namely gets microbial oil is stearic.
The present embodiment divides the fluid oil of carrying rear microbial bacteria oil, and clearing time is 120h above (its physical and chemical index sees Table 1) under 10 ℃ of conditions.Illustrate that the method divides the fluid oil (10-20 ℃) when temperature is low of the microbial oil of proposition to be difficult for solidifying.
Embodiment 4:
A kind of minute extracting method of microbial oil, it comprises the steps:
1) homogenizing: will treat that the microbial oil of minute carrying stirs;
2) broken brilliant: as the microbial oil melting that stirs to be warming up to (26 ℃) more than the solid-state fat fusing point, to keep 5min;
3) freezing and crystallizing: with microbial oil sufficient crystallising 4h under 4 ℃ of cryogenic conditions, place again 10 ℃ of cryogenic thermostat water-bath 1h, formed the viscous slurry that contains solid crystal after lipid material process cooling this moment is freezing;
4) adding of surfactant solution: by the viscous slurry that contains solid crystal: the volume ratio of aqueous surfactant solution=1: 0.5, choose the viscous slurry and the aqueous surfactant solution that contain solid crystal; Wherein, aqueous surfactant solution is comprised of surfactant, inorganic salts and water, and the concentration of surfactant is 0.08wt%, and the concentration of inorganic salts is 0.5wt%;
Surfactant is lauryl sodium sulfate (SDS); Inorganic salts are magnesium sulfate (MgSO
4);
In the viscous slurry that contains solid crystal, add aqueous surfactant solution, stir 0.6h, obtain the emulsion system;
5) centrifugation gets liquid oils: with step 4) emulsifying liquid lie in 5 ℃ of cryogenic conditions and leave standstill 1h, centrifugal in refrigerated centrifuge, liquid component is just gently to tell mutually, adding entry cleans by dehydrating (20 ℃ of dry 2h), namely get the fluid oil (product, yield are 58.8%) of microbial oil;
The aqueous surfactant solution of solid crystal of suspending is then told (as solid phase grease mixed liquor) take heavy phase;
6) get solid fat behind the breakdown of emulsion: after taking out the fluid oil (being liquid component) of microbial oil, the solid phase grease mixed liquor of gained is processed 2-10min through 85 ℃ of heating demulsification types, watery fusion, solid constituent is namely separated with water, the water that removes sub-cloud namely obtains the solid fat component, add entry and wash the aqueous surfactant solution of removing remnants, after dehydrating, the solid that namely gets microbial oil is stearic.
The present embodiment divides the fluid oil of carrying rear microbial bacteria oil, and clearing time is 120h above (its physical and chemical index sees Table 1) under 10 ℃ of conditions.Illustrate that the method divides the fluid oil (10-20 ℃) when temperature is low of the microbial oil of proposition to be difficult for solidifying.
Embodiment 5:
A kind of minute extracting method of microbial oil, it comprises the steps:
1) homogenizing: will treat that the microbial oil of minute carrying stirs;
2) broken brilliant: as the microbial oil melting that stirs to be warming up to (30 ℃) more than the solid-state fat fusing point, to keep 10min;
3) freezing and crystallizing: with microbial oil sufficient crystallising 7h under 4 ℃ of cryogenic conditions, place again 10 ℃ of cryogenic thermostat water-bath 4h, obtain containing the viscous slurry (having formed the viscous slurry that contains solid crystal after lipid material process cooling this moment is freezing) of solid crystal;
4) adding of surfactant solution: in this slip, contain 0.3%SDS and 1%MgSO according to the adding of 1: 1 ratio of oil-water ratio
4Aqueous surfactant solution, fully stir and mixed system be uniformly dispersed form the emulsion system;
5) centrifugation gets liquid oils: this emulsifying liquid is lain in 10 ℃ of conditions leave standstill 0.5h, in refrigerated centrifuge with 5000rpm, centrifugal 5min, liquid component is just gently to tell mutually, add washed with de-ionized water by dehydrating the fluid oil (yield is 57.2%) that namely gets microbial oil, the aqueous surfactant solution of the solid crystal that suspending is then told with heavy phase;
4) adding of surfactant solution: by the viscous slurry that contains solid crystal: the volume ratio of aqueous surfactant solution=1: 2, choose the viscous slurry and the aqueous surfactant solution that contain solid crystal; Wherein, aqueous surfactant solution is comprised of surfactant, inorganic salts and water, and the concentration of surfactant is 0.2wt%, and the concentration of inorganic salts is 3wt%;
Surfactant is lauryl sodium sulfate (SDS); Inorganic salts are magnesium sulfate (MgSO
4);
In the viscous slurry that contains solid crystal, add aqueous surfactant solution, stir 1.0h, obtain the emulsion system;
5) centrifugation gets liquid oils: with step 4) emulsifying liquid lie in 8 ℃ of cryogenic conditions and leave standstill 5h, centrifugal in refrigerated centrifuge, liquid component is just gently to tell mutually, adding entry cleans by dehydrating (25 ℃ of dry 2h), namely get the fluid oil (product, yield are 57.2%) of microbial oil;
The aqueous surfactant solution of solid crystal of suspending is then told (as solid phase grease mixed liquor) take heavy phase;
6) get solid fat behind the breakdown of emulsion: after taking out the fluid oil (being liquid component) of microbial oil, the solid phase grease mixed liquor of gained is processed 2-10min through 95 ℃ of heating demulsification types, watery fusion, solid constituent is namely separated with water, the water that removes sub-cloud namely obtains the solid fat component, add entry and wash the aqueous surfactant solution of removing remnants, after dehydrating, the solid that namely gets microbial oil is stearic.
The present embodiment divides the fluid oil of carrying rear microbial bacteria oil, and clearing time is 120h above (its physical and chemical index sees Table 1) under 10 ℃ of conditions.Illustrate that the method divides the fluid oil (10-20 ℃) when temperature is low of the microbial oil of proposition to be difficult for solidifying.
Embodiment 6
Substantially the same manner as Example 1, difference is: surfactant is sodium alkyl benzene sulfonate.Inorganic salts are sodium sulphate.
The present embodiment divides the fluid oil of carrying rear microbial bacteria oil, and clearing time is more than the 120h under 10 ℃ of conditions.Illustrate that the method divides the fluid oil (10-20 ℃) when temperature is low of the microbial oil of proposition to be difficult for solidifying.
Embodiment 7
Substantially the same manner as Example 1, difference is: surfactant is sodium alkyl sulfate.Inorganic salts are aluminum sulfate.
The present embodiment divides the fluid oil of carrying rear microbial bacteria oil, and clearing time is more than the 120h under 10 ℃ of conditions.Illustrate that the method divides the fluid oil (10-20 ℃) when temperature is low of the microbial oil of proposition to be difficult for solidifying.
Embodiment 7
Substantially the same manner as Example 1, difference is: surfactant is sodium alkyl benzene sulfonate.Inorganic salts are sodium chloride.
The present embodiment divides the fluid oil of carrying rear microbial bacteria oil, and clearing time is more than the 120h under 10 ℃ of conditions.Illustrate that the method divides the fluid oil (10-20 ℃) when temperature is low of the microbial oil of proposition to be difficult for solidifying.
The bound value of each technological parameter of the present invention (such as temperature, time etc.), with and interval value, can both realize the present invention, do not enumerate one by one embodiment at this.
Claims (2)
1. minute extracting method of a microbial oil is characterized in that it comprises the steps:
1) homogenizing: will treat that the microbial oil of minute carrying stirs;
2) break crystalline substance: after the microbial oil that stirs is warming up to 25-30 ℃, insulation 5-10 min;
3) freezing and crystallizing: with step 2) microbial oil after the insulation places 1-4 h under 10 ℃ of cryogenic conditions again in 4 ℃ of crystallization 4-7 h, obtains containing the viscous slurry of solid crystal;
4) adding of surfactant solution: the volume ratio=1:0.5-1:2 by the thickness Liao Jiang ﹕ aqueous surfactant solution that contains solid crystal, choose the viscous slurry and the aqueous surfactant solution that contain solid crystal; Wherein, aqueous surfactant solution is comprised of surfactant, inorganic salts and water, and the concentration of surfactant is 0.08-0.4 wt%, and the concentration of inorganic salts is 0.5-3 wt%;
Surfactant is lauryl sodium sulfate, sodium alkyl benzene sulfonate or sodium alkyl sulfate;
Inorganic salts are magnesium sulfate, sodium sulphate, aluminum sulfate or sodium chloride;
In the viscous slurry that contains solid crystal, add aqueous surfactant solution, stir 0.5-1.0 h, obtain the emulsion system;
5) centrifugation gets liquid oils: the emulsifying liquid of step 4) is lain in 5-10 ℃ of cryogenic conditions leave standstill 1-5h, centrifugal in refrigerated centrifuge, liquid component adds entry and cleans by dehydrating just gently to tell mutually, namely gets the fluid oil of microbial oil;
The aqueous surfactant solution of solid crystal of suspending is then told with heavy phase, obtains solid phase grease mixed liquor.
2. minute extracting method of a kind of microbial oil according to claim 1, it is characterized in that: the solid phase grease mixed liquor of gained is processed 2-10 min through 80-95 ℃ of heating demulsification type, watery fusion, solid constituent is namely separated with water, get supernatant, the solid constituent that obtains also adds entry and washes and remove remaining aqueous surfactant solution, and after dehydrating, the solid that namely gets microbial oil is stearic.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110350200 CN102388988B (en) | 2011-11-08 | 2011-11-08 | Separated extraction method of microorganism oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110350200 CN102388988B (en) | 2011-11-08 | 2011-11-08 | Separated extraction method of microorganism oil |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102388988A CN102388988A (en) | 2012-03-28 |
| CN102388988B true CN102388988B (en) | 2013-01-23 |
Family
ID=45856483
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110350200 Expired - Fee Related CN102388988B (en) | 2011-11-08 | 2011-11-08 | Separated extraction method of microorganism oil |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102388988B (en) |
Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DK1252324T3 (en) | 2000-01-19 | 2010-12-20 | Martek Biosciences Corp | Solvent-free extraction procedure |
| WO2011153246A2 (en) | 2010-06-01 | 2011-12-08 | Martek Biosciences Corporation | Extraction of lipid from cells and products therefrom |
| CN103421605B (en) * | 2012-05-25 | 2017-03-15 | 丰益(上海)生物技术研发中心有限公司 | Method and its application that oils and fatss are carried with erythritol fatty acid ester point |
| AR098895A1 (en) | 2013-12-20 | 2016-06-22 | Dsm Ip Assets Bv | PROCESS FOR OBTAINING MICROBIAL OIL FROM MICROBIAL CELLS |
| KR102435269B1 (en) | 2013-12-20 | 2022-08-22 | 디에스엠 아이피 어셋츠 비.브이. | Processes for obtaining microbial oil from microbial cells |
| EP3082793B1 (en) | 2013-12-20 | 2020-04-15 | DSM IP Assets B.V. | Processes for obtaining microbial oil from microbial cells |
| KR102435265B1 (en) | 2013-12-20 | 2022-08-22 | 디에스엠 아이피 어셋츠 비.브이. | Processes for obtaining microbial oil from microbial cells |
| CA2934491C (en) | 2013-12-20 | 2023-09-26 | Dsm Ip Assets B.V. | Processes for obtaining microbial oil from microbial cells |
| CN105176671B (en) * | 2014-06-18 | 2018-11-30 | 中国石油化工股份有限公司 | A kind of method of the broken wall and auxiliary agent assisted extraction grease of oil-containing micro-algae |
| CN105454466A (en) * | 2015-12-04 | 2016-04-06 | 润科生物工程（福建）有限公司 | Application of sucrose fatty acid ester serving as grease crystallization inhibitor in oil containing polyunsaturated fatty acid single-cell grease |
| CN108624403A (en) * | 2018-04-28 | 2018-10-09 | 武汉工程大学 | A kind of method of low temperature non-organic solvent extraction energy insect oils |
| CN117229848A (en) * | 2023-07-20 | 2023-12-15 | 青岛和合汇途工程技术有限公司 | Wet fractionation method for preparing 2-bit DHA algae oil |
-
2011
- 2011-11-08 CN CN 201110350200 patent/CN102388988B/en not_active Expired - Fee Related
Non-Patent Citations (4)
| Title |
|---|
| 何东平等.微生物油脂精炼的研究.《中国油脂》.2000,第25卷(第6期),第76-78页. |
| 周林.微生物油脂研究概况.《粮食与食品工业》.2011,第18卷(第1期),第20-23页. |
| 微生物油脂研究概况;周林;《粮食与食品工业》;20110215;第18卷(第1期);第20-23页 * |
| 微生物油脂精炼的研究;何东平等;《中国油脂》;20001225;第25卷(第6期);第76-78页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102388988A (en) | 2012-03-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102388988B (en) | Separated extraction method of microorganism oil | |
| Timms | Fractional crystallisation–the fat modification process for the 21st century | |
| EP2114851B1 (en) | Process for separating saturated and unsaturated fatty acids | |
| CN205501251U (en) | A simple and easy winterization device for fish oil | |
| JP2013100530A (en) | Extraction and winterization of lipid from oilseed and microbial source | |
| CN102229860A (en) | Supersonic wave method for promoting rapid crystallization and fractionation of palm oil | |
| Man et al. | Thermal analysis of failed-batch palm oil by differential scanning calorimetry | |
| CN102604739A (en) | Method for dry fractionation of palm oil | |
| WO2020024643A1 (en) | Method for winterizing microbial oil | |
| CN104629906B (en) | A kind of crystallization in motion agent and point method for mentioning grease | |
| CN107629873B (en) | Method for enriching fish oil EPA and DHA through low-temperature crystallization | |
| CN103614239A (en) | Method for preparing low-temperature-resistant palm oil with high iodine value | |
| CN103787864B (en) | Method for extracting DHA (Docosahexaenoic acid) from marine microalgae fermentation liquor | |
| CN106566656A (en) | Method of applying double-frequency ultrasonic waves to produce top-level palm olein | |
| CN105831370A (en) | Preparation method of cocoa butter equivalent | |
| CA1157043A (en) | Crude edible oil wax removal process | |
| CN108285826B (en) | Animal oil extraction method | |
| US3994943A (en) | Dewaxing of vegetable oils | |
| SU509215A3 (en) | The method of separation of fatty substances | |
| JPS58198423A (en) | Fractionation method of fat or oil | |
| Sulaiman et al. | Triacylglycerols responsible for the onset of nucleation during clouding of palm olein | |
| CN109528784B (en) | Method for extracting and preparing 4,4' -dimethyl sterol from shea butter | |
| JP5947064B2 (en) | Method for producing fatty acid composition | |
| CN113943605B (en) | Winterization and fractionation method for microbial oil | |
| CN106367202A (en) | Method for shortening cottonseed oil separation extraction time, cottonseed oil separation extraction method, and uses of extremely hydrogenated vegetable oil as crystallization promoting agent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130123 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |