CN102965182A - Method for extracting grease from schizochytrium - Google Patents
Method for extracting grease from schizochytrium Download PDFInfo
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- CN102965182A CN102965182A CN2012104916107A CN201210491610A CN102965182A CN 102965182 A CN102965182 A CN 102965182A CN 2012104916107 A CN2012104916107 A CN 2012104916107A CN 201210491610 A CN201210491610 A CN 201210491610A CN 102965182 A CN102965182 A CN 102965182A
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Abstract
The invention discloses a method for extracting grease from schizochytrium. The method comprises the following steps: (1) adjusting the pH (Potential of Hydrogen) of the fermentation broth of the schizochytrium until reaching an acid stage, and then adding an organic solvent to stir, so as to realize the wall breaking of schizochytrium cells and extraction of microalgae oil; (2) adding a flocculant to the fermentation broth obtained in step (1) to flocculate, and extracting by the organic solvent to obtain crude algae oil; and (3) treating the crude algae oil by degumming, discoloring, and deacidifying/deodorizing, so as to obtain the microalgae oil rich in DHA (Docosahexaenoic Acid). According to the method disclosed by the invention, autolysis wall-breaking technology is adopted, so that the technological process in wall breaking and extraction of the schizochytrium can be simplified, the operation time in wall breaking can be shortened, the investment on equipment is decreased, and the cost is lowered; and the biological flocculant flocculation technology is carried out, therefore, the demulsification technological process is simplified, the time for layering is shortened, the layering effect is improved, the load due to wastewater discharge and water treatment caused by the demulsification process can be avoided, and the cost of water treatment can be lowered.
Description
Technical field
The invention belongs to biological technical field, relate to a kind of method of from fragmentation kettle algae, extracting and making with extra care rich grease-contained microalgae grease.
Background technology
Docosahexenoic acid (Docosahexaenoic acid is called for short DHA) is the long-chain highly unsaturated fatty acid that carbochain is the longest, degree of unsaturation is the highest of finding at present.DHA is the biomembranous important structure component of body, has vital role at aspects such as infant's neurodevelopment, retina formation, intellectual developments, and be prostaglandin(PG), change the precursor that Prostaglandins and Leukotrienes element etc. has the self-regulation material of strong physiologically active, to preventing cardiovascular disease, anti-lipid, hypotensive, suppress tumour formation etc. and have remarkable effect.Owing to have above-mentioned multiple important physiological function, DHA has become widely fatty acid product of value height, market.
Schizochytrium limacinum claims again to split the kettle algae, belongs to a class thalassiomycetes of Mycophyta (Eumycota), Oomycete (Oomycetes), Saprolegniales (Saprolegniales), thraustochytriale section (Thraustochytriaceae), and is unicellular, spherical.The a large amount of active substances useful to human body of fragmentation kettle frustule accumulation, as: grease, pigment, squalene etc., wherein grease accounts for more than 70% of dry cell weight, docosahexenoic acid (DHA) content is very high in total fat, reach 35% ~ 40%, the fatty acid content of similar is low, easily separation and purification, and do not have fishy smell, so schizochytrium limacinum is one of a kind of microorganism that has realization suitability for industrialized production DHA potentiality.
CN 101638361A discloses a kind of from schizochytrium limacinum extraction and the refining method that is rich in docosahexenoic acid, the fermented liquid flocculation treatment is carried out solid-liquid separation again, by behind the alkali broken wall with the cell Mechanical Crushing, then the thalline of fragmentation adopted organic solvent extraction, obtain slightly oil of DHA, the thick oil of DHA is through coming unstuck, obtaining the DHA essential oil behind the alkali refining, decolouring, deodorization.The method has solved fragmentation kettle algae grease and has extracted the technical problem of refining, but this technology technology for broken wall is loaded down with trivial details, and the time spent is longer, equipment investment is large, adopt standing demix technique in water, algae and organic solvent hierarchical process, this technique is bad at the practical application layered effect, and the time is longer.
CN102199485A discloses the method that kettle algae grease is split in a kind of extraction, and the method is that to split kettle algae mud be raw material, through homogeneous, alkali carry, enzymolysis, centrifugal, organic solvent extraction obtain splitting kettle algae oil.Raw material carries out pyroprocessing first after sodium citrate buffer solution dilution and average, carry and adopt successively neutral protease and Sumizyme MP to carry out enzymolysis through alkali again, and centrifugal rear separation edible vegetable oil also adopts organic solvent extraction missible oil.The method adopts aqueous enzymatic method to carry oil tech and has solved the technical problem that fragmentation kettle algae algae oil extracts, but this technical matters is complicated, the broken wall operation is various, is not suitable for suitability for industrialized production and uses.
The chemical refining technology is all adopted in the refining of the thick oil of fragmentation kettle algae in the prior art, and the thick oil of DHA is through coming unstuck, obtaining the DHA essential oil behind the alkali refining, decolouring, deodorization.There are some problems inevitably in this technique, and for example: part neutral oil is inevitably by saponification; The contaminated wastewater environment; When from the byproduct Chinese honey locust, reclaiming lipid acid, need through complicated processing link (hydrolysis, distillation); During especially for the refining of high acid value crude oil, grease refining consumption is large, and economical effectiveness is not good enough.And, the methods such as adding ethanol, sodium-chlor that adopt are carried out the breakdown of emulsion layering more in the present breakdown of emulsion layering, and this technique exists production cost height, complex operation in practical application, separation time is long, layered effect is unstable, ethanol reclaims difficulty and produce a large amount of problems such as effluent brine.
Summary of the invention
The object of the present invention is to provide a kind of method of from fragmentation kettle algae, extracting grease, described method broken wall operating time and hierarchical process time are short, layered effect is good, has avoided simultaneously the discharge of wastewater that causes because of demulsification technology and the burden of water treatment, has reduced the cost of water treatment.
In order to achieve the above object, the present invention has adopted following technical scheme:
A kind of method of extracting grease from fragmentation kettle algae, described method comprises the steps:
(1) pH that regulates fragmentation kettle algae fermented liquid adds organic solvent to acid, stirs, and realizes the broken wall of fragmentation kettle frustule and the extraction of microalgae grease;
(2) after adding the flocculation agent flocculation treatment in the fermented liquid that obtains to step (1), adopt organic solvent extraction to obtain the algae crude oil;
(3) the algae crude oil is through coming unstuck, decolouring, and depickling/deodorization obtains being rich in the microalgae grease of DHA.
Fragmentation kettle algae of the present invention also claims schizochytrium limacinum.
The preparation method of the fragmentation kettle algae fermented liquid that the present invention is exemplary is:
After adopting fragmentation kettle algae ampere tank to be inoculated into the inclined-plane, carry out after liquid shaking bottle cultivates, switching enters 6m again
3Fermentor cultivation, the substratum under it consists of: glucose 100-130g, yeast extract paste 15-30g, peptone 10-20g, potassium primary phosphate 2-4g, sal epsom 1-3g, trace element complex liquid 8-11ml, VITAMIN complex liquid 4-8ml is settled to 1L with 0.5 * seawater; Described 0.5 * seawater is that the water with the seawater of 1 volume and 1 volume is mixed to get;
The preparation method of described micro-complex liquid is as follows: Na2EDTA 6.0g, FeCl
36H
2O 0.29g, H
3BO
36.84g, MnCl
24H
2O 0.86g, ZnCl
20.06g, CoCl
26H
2O 0.026g, NiSO
46H
2O0.052g, CuSO
45H
2O 0.002g, NaMoO
42H
2O 0.005g, water is settled to 1L;
The preparation method of described VITAMIN complex liquid is as follows: VITMAIN B1 100mg, and vitamin B7 0.5mg, vitamin B12 0.5mg, water is settled to 1L;
The parameter of described fermentation culture is: 25 ~ 30 ℃ of temperature, and pH value 5.5 ~ 7.5, incubation time 72 ~ 96h, the parameter of described fermentation culture is preferably 25 ℃ of temperature, pH value 6.0, incubation time 96h, dissolved oxygen 10%.
After the present invention regulates the pH of fermented liquid, under certain temperature and rotating speed, stir, make microalgae cell autolyze broken wall, the grease of cell interior is free out, extract by organic solvent, effectively extract the grease in the microalgae cell when having realized the self-dissolving broken wall of fragmentation kettle frustule, greatly shortened the extraction time of microalgae grease.Autolysis method is a kind of special enzymic hydrolysis mode, and its required cytase is produced by microorganism itself.In the microorganism growth metabolic process, mostly can both produce the enzyme of polymer architecture on certain hydrolysis self cell walls, in order to the growth and breeding process is gone on.The control certain condition can bring out the cytase of microorganisms surplus or excite the vigor of self cytase, to reach the purpose of aqtocytolysis.By regulating the pH value of algae liquid, control the self-dissolving temperature and time in this patent, realized the self-dissolving broken wall of microalgae cell.
Described method has been simplified the technique that grease extracts greatly, and it is high to put forward oily efficient, and technique is simple, is conducive to realize suitability for industrialized production.
Preferably, described flocculation agent is biological flocculant, preferred chitosan.
In water, algae, organic solvent hierarchical process, the present invention adopts the biological flocculant chitosan to carry out biofloculation technique.Chitosan is the very abundant natural alkaline polysaccharides of a kind of reserves, the product that is generated behind the strong lye deacetylation by chitin.The flocculate with chitosan microalgae cell, thus breakdown of emulsion finished.Chitosan and microalgae cell mainly catch bridging action by neutralizing effect, adsorption and net and microalgae cell is had an effect, and microalgae cell is flocculated, and reaches the breakdown of emulsion layered effect.Adopt the biological flocculant chitosan to carry out the breakdown of emulsion layering, the time of breakdown of emulsion layering has been shortened in the adding of chitosan greatly, has improved simultaneously the effect of breakdown of emulsion layering, has avoided simultaneously the discharge of wastewater that causes because of demulsification technology and the burden of water treatment.
Preferably, vacuum depickling/deodorizing technology is adopted in the described depickling of step (3)/deodorization.Vacuum depickling/deodorizing technology is to utilize steam to carry under vacuum condition to remove FFA and volatile matter etc., it has avoided neutral oil saponification loss, reduced the grease loss, and simple to operate, the consumption of steam, water and energy is all less, therefore invest lessly, and pigment and stink substance are also along with steam is removed.
Preferably, step (2) comprises the steps:
Add biological flocculant in the fermented liquid that (2a) obtains to step (1), after fully stirring evenly, standing demix extracts upper strata mixing oil phase;
(2b) in step (2a) extract to be mixed fermented liquid behind the oil phase, again add organic solvent, 40 ~ 60 ℃ of lower stirrings, behind the standing demix, extract upper strata mixing oil phase;
Solvent evaporation in the mixing oil phase that (2c) step (2a) and step (2b) is obtained obtains the algae crude oil.
The present invention adopts three-phase layering technique to extract the mixing oil phase.Add biological flocculant in the fermented liquid that step (1) is obtained, after fully stirring evenly, standing demix, orlop are water, and the middle level is algae-residue, and the upper strata is for mixing oil phase, and described mixing oil phase is the mixture of organic solvent and algae crude oil.Behind the fermented liquid extraction upper strata mixing oil phase with step (2a), again add organic solvent, carry out reextraction.Solvent evaporation in the mixing oil phase that twice extraction obtained obtains the algae crude oil.The algae-residue in middle level can pass through solid-liquid separation, obtains after the drying, can be used for animal-feed and uses.
Step (1) is regulated pH to 3.5 ~ 4.5, for example regulates pH to 3.6,3.7,3.8,3.9,4.0,4., 1,4.2,4.3,4.4, preferred 3.7 ~ 4.2.The self-dissolving broken wall of fragmentation kettle algae can be realized in the pH to 3.5 of adjusting fermented liquid ~ 4.5, has simplified the technical process of fragmentation kettle algae extraction, has significantly reduced the broken wall operating time, has reduced equipment investment.
Preferably, step (1) adopts acid for adjusting pH value, described acid to be selected from the mixture of any one or at least two kinds in hydrochloric acid, phosphoric acid, acetic acid or the citric acid.Described mixture is the mixture of hydrochloric acid and phosphoric acid for example, the mixture of phosphoric acid and acetic acid, the mixture in acetic acid and the citric acid, the mixture in hydrochloric acid, acetic acid and the citric acid, the mixture in phosphoric acid, acetic acid and the citric acid.
Preferably, in step (1) and the step (2b), the volume of organic solvent is 0.8 ~ 2 times of step (1) fermentating liquid volume, for example 0.9 times, 1.1 times, 1.3 times, 1.4 times, 1.6 times, 1.8 times, 1.9 times, and preferred 1 ~ 1.5 times.
Preferably, step (1) is 40 ~ 60 ℃ of lower stirrings, for example 42 ℃, 46 ℃, 48 ℃, 50 ℃, 52 ℃, 54 ℃, 56 ℃, 58 ℃, 59 ℃ lower stirrings, preferably 45 ~ 55 ℃ of lower stirrings.
Described organic solvent is selected from the mixture of any one or at least two kinds in No. six solvents, normal hexane, isohexane or the iso-pentane.Described mixture is the mixture of No. six solvents and normal hexane for example, the mixture of normal hexane and isohexane, the mixture of isohexane and iso-pentane, the mixture of No. six solvents, normal hexane and isohexanes.Above-mentioned solvent is commercially available obtaining all.
The addition of biological flocculant is the fermented liquid that 100 ~ 500mg/L step (1) obtains, and namely " adds the biological flocculant of 100 ~ 500mg in the fermented liquid that every L step (1) obtains ", and preferred addition is the fermented liquid that 300 ~ 500mg/L step (1) obtains.
The stir speed (S.S.) of described stirring is 80 ~ 150rpm, for example 85rpm, 95rpm, 105rpm, 110rpm, 115rpm, 125rpm, 135rpm, preferred 90 ~ 140rpm, further preferred 100 ~ 130rpm.
The described churning time of step (1) is 2 ~ 6 hours, for example 2.5 hours, 3 hours, 3.5 hours, 4 hours, 4.5 hours, 5 hours, 5.5 hours, and preferred 2.5 ~ 5.5 hours.
The described churning time of step (2b) is 0.5 ~ 1 hour, for example 0.55 hour, 0.6 hour, 0.65 hour, 0.7 hour, 0.75 hour, 0.85 hour, 0.95 hour, and preferred 0.6 hour ~ 0.9 hour.
Described coming unstuck adopted phosphoric acid acidifying degumming technology; Preferably, described phosphoric acid acidifying degumming technology is: the algae crude oil that step (2) or step (2c) are obtained is preheating to 80 ~ 85 ℃, 0.3 ~ 0.5% the phosphoric acid that adds algae crude oil weight that step (2) or step (2c) obtain, after acidifying is come unstuck, 90 ~ 95 ℃ washing 2 ~ 5 times, the algae crude oil that comes unstuck after obtaining coming unstuck; The weight of described each washing water is 5 ~ 10% of the algae crude oil weight that obtains of step (2) or step (2c).The preheating temperature of described algae crude oil can be 81 ℃, 82 ℃, 83 ℃, 84 ℃.The add-on of described phosphoric acid is 0.3 ~ 0.5% of algae crude oil weight, for example 0.33%, 0.36%, 0.38%, 0.41%, 0.44%, 0.47%, 0.49%.The weight of described hot water is 5 ~ 10% of algae crude oil weight, for example 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, 9%, 9.5%.
Preferably, gac or activated decoloration are adopted in described decolouring.
Preferably, described decoloration process is under vacuum condition, and temperature is 100 ~ 105 ℃, and gac or atlapulgite that the algae crude oil after come unstuck adds the rear algae crude oil weight 3 ~ 5% of coming unstuck decolour, vacuum tightness is-and below the 0.094mPa.Described temperature for example can be 101 ℃, 102 ℃, 103 ℃, 104 ℃.Described vacuum tightness for example is-0.1mPa ,-0.2mPa ,-0.3mPa ,-0.4mPa ,-0.5mPa.Described vacuum tightness is gauge pressure.
Vacuum depickling/deodorizing technology is adopted in described depickling/deodorization, and described technique is: the algae crude oil after will decolouring is that 120 ~ 280 ℃, vacuum tightness be-below the 0.094mPa, decoloured 1 ~ 2 hour in temperature.Described temperature for example can be 130 ℃, 150 ℃, 180 ℃, 210 ℃, 230 ℃, 250 ℃, 270 ℃.Described bleaching time for example is 1.2 hours, 1.4 hours, 1.6 hours, 1.1 hours, 1.8 hours, 1.9 hours.Described vacuum tightness for example is-0.1mPa ,-0.2mPa ,-0.3mPa ,-0.4mPa ,-0.5mPa.Described vacuum tightness is gauge pressure.
Preferably, a kind of method of from fragmentation kettle algae, extracting grease, described method comprises the steps:
(1) pH to 3.5 of adjusting fragmentation kettle algae fermented liquid ~ 4.5 add organic solvent, 40 ~ 60 ℃ of lower stirrings, realize the broken wall of fragmentation kettle frustule and the extraction of microalgae grease;
Add biological flocculant in the fermented liquid that (2a) obtains to step (1), after fully stirring evenly, standing demix extracts upper strata mixing oil phase;
(2b) in step (2a) extract to be mixed fermented liquid behind the oil phase, again add organic solvent, 40 ~ 60 ℃ of lower stirrings, behind the standing demix, extract upper strata mixing oil phase;
Solvent evaporation in the mixing oil phase that (2c) step (2a) and step (2b) is obtained obtains the algae crude oil;
(3) the algae crude oil is through coming unstuck, decolouring, and depickling/deodorization obtains being rich in the microalgae grease of DHA.
Preferably, a kind of method of from fragmentation kettle algae, extracting grease, described method comprises the steps:
(1) pH to 3.5 of adjusting fragmentation kettle algae fermented liquid ~ 4.5 add organic solvent, 40 ~ 60 ℃ of lower stirrings, realize the broken wall of fragmentation kettle frustule and the extraction of microalgae grease;
Add biological flocculant in the fermented liquid that (2a) obtains to step (1), after fully stirring evenly, standing demix extracts upper strata mixing oil phase;
(2b) in step (2a) extract to be mixed fermented liquid behind the oil phase, again add organic solvent, 40 ~ 60 ℃ of lower stirrings, behind the standing demix, extract upper strata mixing oil phase;
Solvent evaporation in the mixing oil phase that (2c) step (2a) and step (2b) is obtained obtains the algae crude oil;
(3) the algae crude oil that step (2) or step (2c) is obtained is preheating to 80 ~ 85 ℃, 0.3 ~ 0.5% the phosphoric acid that adds algae crude oil weight that step (2) or step (2c) obtain, after acidifying is come unstuck, 90 ~ 95 ℃ washing 2 ~ 5 times, the algae crude oil that comes unstuck after obtaining coming unstuck; The weight of the water of described each washing usefulness is 5 ~ 10% of the algae crude oil weight that obtains of step (2) or step (2c); Under vacuum condition, temperature is 100 ~ 105 ℃, and gac or atlapulgite that the algae crude oil after come unstuck adds the rear algae crude oil weight 3 ~ 5% of coming unstuck decolour, vacuum tightness is-below the 0.094mPa; Be that 120 ~ 280 ℃, vacuum tightness be-below the 0.094mPa, decoloured 1 ~ 2 hour with the algae crude oil after the decolouring in temperature, obtain being rich in the microalgae grease of DHA, obtain simultaneously the part free fatty acids.
Compared with prior art, the present invention has following beneficial effect:
(1) the present invention adopts the self-dissolving wall breaking technology, has simplified the technical process of fragmentation kettle algae extraction, has reduced the broken wall operating time, has reduced equipment investment, has reduced cost; In water, algae, organic solvent hierarchical process, adopt the biological flocculant flocculation process, simplify the demulsification technology flow process, reduced the hierarchical process time, improved layered effect, avoid simultaneously the discharge of wastewater that causes because of demulsification technology and the burden of water treatment, reduced the cost of water treatment;
(3) the present invention adopts microalgae wall breaking and grease to extract the technique of carrying out simultaneously, has realized that microalgae cell broken wall and grease extract to carry out simultaneously, has greatly shortened the extraction time of microalgae grease;
(2) the present invention adopts the physical refining technology to obtain being rich in the microalgae grease of DHA, and the refining that has reduced chemical refining consumes, and technical process is simple, product stability is good, and raw and auxiliary material is economized, and output is high, good in economic efficiency, avoided neutral oil saponification loss, refining efficiency is high, and product stability is good, can directly obtain high-quality byproduct-lipid acid, and do not have the plurality of advantages such as contaminated wastewater, particularly for the depickling of some high acid value fragmentation kettle algae greases, its superiority is more outstanding.
Description of drawings
Further specify technical scheme of the present invention below in conjunction with accompanying drawing and by embodiment.
Fig. 1: the present invention extracts the process flow sheet of grease from fragmentation kettle algae.
Embodiment
For the present invention is described better, be convenient to understand technical scheme of the present invention, typical but non-limiting embodiment of the present invention is as follows:
Embodiment 1
After adopting fragmentation kettle algae ampere tank to be inoculated into the inclined-plane, carry out after liquid shaking bottle cultivates, switching enters 6m again
3Fermentor cultivation, the substratum under it consists of: glucose 100-130g, yeast extract paste 15-30g, peptone 10-20g, potassium primary phosphate 2-4g, sal epsom 1-3g, trace element complex liquid 8-11ml, VITAMIN complex liquid 4-8ml is settled to 1L with 0.5 * seawater; Described 0.5 * seawater is that the water with the seawater of 1 volume and 1 volume is mixed to get.
The preparation method of described micro-complex liquid is as follows: Na2EDTA 6.0g, FeCl
36H
2O 0.29g, H
3BO
36.84g, MnCl
24H
2O 0.86g, ZnCl
20.06g, CoCl
26H
2O 0.026g, NiSO
46H
2O0.052g, CuSO
45H
2O 0.002g, NaMoO
42H
2O 0.005g, water is settled to 1L.
The preparation method of described VITAMIN complex liquid is as follows: VITMAIN B1 100mg, and vitamin B7 0.5mg, vitamin B12 0.5mg, water is settled to 1L.
The parameter of described fermentation culture is: 25 ~ 30 ℃ of temperature, and pH value 5.5 ~ 7.5, incubation time 72 ~ 96h, the parameter of described fermentation culture is preferably 25 ℃ of temperature, pH value 6.0, incubation time 96h, dissolved oxygen 10%.
The fermented liquid 4m of fragmentation kettle algae
3, regulate pH to 4.5 with glacial acetic acid.Add 4m
3Normal hexane at 55 ~ 60 ℃, stirs 4h under the 100rpm rotating speed, realizes the broken wall of fragmentation kettle frustule, and extracts simultaneously microalgae grease, then adds the biological flocculant chitosan, makes chitosan concentration remain on 400mg/L.After fully stirring evenly, standing demix extracts upper strata mixing oil phase, and then adds 4m
3Normal hexane at 55 ~ 60 ℃, stirs 1h under the 100rpm rotating speed, behind the standing demix, extracts upper strata mixing oil phase.The algae-residue of lower floor obtains algae-residue by solid-liquid separation after the drying, can be used for animal-feed and use.The mixing oil phase that obtains by evaporating solvent, obtains the algae crude oil.
The algae raw oil refining technique adopts the physical refining process of advanced technology, and design parameter is as follows:
Degumming technology: adopt phosphoric acid acidifying degumming technology, algae crude oil temperature is 80 ~ 85 ℃, and the phosphoric acid add-on is 0.5% of algae crude oil weight, and the hot water add-on is 5% of algae crude oil weight during washing, washes three times.
Decoloration process: temperature is 100 ~ 105 ℃, and the atlapulgite addition is 5% of the algae crude oil weight of coming unstuck, vacuum tightness (gauge pressure) is-and below the 0.094mpa.
Depickling/deodorizing technology: temperature is 200 ℃, and vacuum tightness (gauge pressure) is-and below the 0.094mpa, the time is 2h.
Obtain being rich in the microalgae grease of DHA by above-mentioned technique.
Measuring the fermented liquid biomass is 50g/L, and the total fatty acid content of extraction is that 30%, DHA content (being the ratio that DHA accounts for total fatty acids) is 43.36%.
Embodiment 2
After adopting fragmentation kettle algae ampere tank to be inoculated into the inclined-plane, carry out after liquid shaking bottle cultivates, switching enters 6m again
3Fermentor cultivation, the substratum under it consists of: glucose 100-130g, yeast extract paste 15-30g, peptone 10-20g, potassium primary phosphate 2-4g, sal epsom 1-3g, trace element complex liquid 8-11ml, VITAMIN complex liquid 4-8ml is settled to 1L with 0.5 * seawater; Described 0.5 * seawater is that the water with the seawater of 1 volume and 1 volume is mixed to get.
The preparation method of described micro-complex liquid is as follows: Na2EDTA 6.0g, FeCl
36H
2O0.29g, H
3BO
36.84g, MnCl
24H
2O 0.86g, ZnCl
20.06g, CoCl
26H
2O 0.026g, NiSO
46H
2O 0.052g, CuSO
45H
2O 0.002g, NaMoO
42H
2O 0.005g, water is settled to 1L.
The preparation method of described VITAMIN complex liquid is as follows: VITMAIN B1 100mg, and vitamin B7 0.5mg, vitamin B12 0.5mg, water is settled to 1L.
The parameter of described fermentation culture is: 25 ~ 30 ℃ of temperature, and pH value 5.5 ~ 7.5, incubation time 72 ~ 96h, the parameter of described fermentation culture is preferably 25 ℃ of temperature, pH value 6.0, incubation time 96h, dissolved oxygen 10%.
The fermented liquid 4m of fragmentation kettle algae
3, regulate pH to 3.5 with glacial acetic acid.Add 6m
3Normal hexane at 55 ~ 60 ℃, stirs 4h under the 100rpm rotating speed, realizes the broken wall of fragmentation kettle frustule, and extracts simultaneously microalgae grease, then adds the biological flocculant chitosan, makes chitosan concentration remain on 500mg/L.After fully stirring evenly, standing demix extracts upper strata mixing oil phase, and then adds 6m
3Normal hexane at 55 ~ 60 ℃, stirs 1h under the 100rpm rotating speed, behind the standing demix, extracts upper strata mixing oil phase.The algae-residue of lower floor obtains algae-residue by solid-liquid separation after the drying, can be used for animal-feed and use.The mixing oil phase that obtains by evaporating solvent, obtains the algae crude oil.
The algae raw oil refining technique adopts the physical refining process of advanced technology, and design parameter is as follows:
Degumming technology: adopt phosphoric acid acidifying degumming technology, algae crude oil temperature is 80 ~ 85 ℃, and the phosphoric acid add-on is 0.3% of algae crude oil weight, and the hot water add-on is 5% of algae crude oil weight during washing, washes three times.
Decoloration process: temperature is 100 ~ 105 ℃, and the atlapulgite addition is 3% of the algae crude oil weight of coming unstuck, vacuum tightness (gauge pressure) is-and below the 0.094mpa.
Depickling/deodorizing technology: temperature is 280 ℃, and vacuum tightness (gauge pressure) is-and below the 0.094mpa, the time is 2h.
Obtain being rich in the microalgae grease of DHA by above-mentioned technique.
Measuring the fermented liquid biomass is 47g/L, and the total fatty acid content of extraction is that 32%, DHA content (being the ratio that DHA accounts for total fatty acids) is 36.81%.
Embodiment 3
After adopting fragmentation kettle algae ampere tank to be inoculated into the inclined-plane, carry out after liquid shaking bottle cultivates, switching enters 6m again
3Fermentor cultivation, the substratum under it consists of: glucose 100-130g, yeast extract paste 15-30g, peptone 10-20g, potassium primary phosphate 2-4g, sal epsom 1-3g, trace element complex liquid 8-11ml, VITAMIN complex liquid 4-8ml is settled to 1L with 0.5 * seawater; Described 0.5 * seawater is that the water with the seawater of 1 volume and 1 volume is mixed to get.
The preparation method of described micro-complex liquid is as follows: Na2EDTA 6.0g, FeCl
36H
2O 0.29g, H
3BO
36.84g, MnCl
24H
2O 0.86g, ZnCl
20.06g, CoCl
26H
2O 0.026g, NiSO
46H
2O0.052g, CuSO
45H
2O 0.002g, NaMoO
42H
2O 0.005g, water is settled to 1L;
The preparation method of described VITAMIN complex liquid is as follows: VITMAIN B1 100mg, and vitamin B7 0.5mg, vitamin B12 0.5mg, water is settled to 1L.
The parameter of described fermentation culture is: 25 ~ 30 ℃ of temperature, and pH value 5.5 ~ 7.5, incubation time 72 ~ 96h, the parameter of described fermentation culture is preferably 25 ℃ of temperature, pH value 6.0, incubation time 96h, dissolved oxygen 10%.
The fermented liquid 4m of fragmentation kettle algae
3, regulate pH to 3.5 with glacial acetic acid.Add 3.2m
3Normal hexane at 55 ~ 60 ℃, stirs 4h under the 100rpm rotating speed, realizes the broken wall of fragmentation kettle frustule, and extracts simultaneously microalgae grease, then adds the biological flocculant chitosan, makes chitosan concentration remain on 500mg/L.After fully stirring evenly, standing demix extracts upper strata mixing oil phase, and then adds 3.2m
3Normal hexane at 55 ~ 60 ℃, stirs 1h under the 100rpm rotating speed, behind the standing demix, extracts upper strata mixing oil phase.The algae-residue of lower floor obtains algae-residue by solid-liquid separation after the drying, can be used for animal-feed and use.The mixing oil phase that obtains by evaporating solvent, obtains the algae crude oil.
The algae raw oil refining technique adopts the physical refining process of advanced technology, and design parameter is as follows:
Degumming technology: adopt phosphoric acid acidifying degumming technology, algae crude oil temperature is 80 ~ 85 ℃, and the phosphoric acid add-on is 0.5% of algae crude oil weight, and the hot water add-on is 5% of algae crude oil weight during washing, washes three times.
Decoloration process: temperature is 100 ~ 105 ℃, and the atlapulgite addition is 5% of the algae crude oil weight of coming unstuck, vacuum tightness (gauge pressure) is-and below the 0.094mpa.
Depickling/deodorizing technology: temperature is 260 ℃, and vacuum tightness (gauge pressure) is-and below the 0.094mpa, the time is 2h.
Obtain being rich in the microalgae grease of DHA by above-mentioned technique.
Measuring the fermented liquid biomass is 43g/L, and the total fatty acid content of extraction is that 28%, DHA content (being the ratio that DHA accounts for total fatty acids) is 35.73%.
Embodiment 4
After adopting fragmentation kettle algae ampere tank to be inoculated into the inclined-plane, carry out after liquid shaking bottle cultivates, switching enters 6m again
3Fermentor cultivation, the substratum under it consists of: glucose 100-130g, yeast extract paste 15-30g, peptone 10-20g, potassium primary phosphate 2-4g, sal epsom 1-3g, trace element complex liquid 8-11ml, VITAMIN complex liquid 4-8ml is settled to 1L with 0.5 * seawater; Described 0.5 * seawater is that the water with the seawater of 1 volume and 1 volume is mixed to get.
The preparation method of described micro-complex liquid is as follows: Na2EDTA 6.0g, FeCl
36H
2O 0.29g, H
3BO
36.84g, MnCl
24H
2O 0.86g, ZnCl
20.06g, CoCl
26H
2O 0.026g, NiSO
46H
2O0.052g, CuSO
45H
2O 0.002g, NaMoO
42H
2O 0.005g, water is settled to 1L.
The preparation method of described VITAMIN complex liquid is as follows: VITMAIN B1 100mg, and vitamin B7 0.5mg, vitamin B12 0.5mg, water is settled to 1L.
The parameter of described fermentation culture is: 25 ~ 30 ℃ of temperature, and pH value 5.5 ~ 7.5, incubation time 72 ~ 96h, the parameter of described fermentation culture is preferably 25 ℃ of temperature, pH value 6.0, incubation time 96h, dissolved oxygen 10%.
The fermented liquid 4m of fragmentation kettle algae
3, with lemon acid for adjusting pH to 4.0.Add 8m
3Isohexane at 40 ~ 50 ℃, stirs 6h under the 80rpm rotating speed, realizes the broken wall of fragmentation kettle frustule, and extracts simultaneously microalgae grease, then adds the biological flocculant chitosan, makes chitosan concentration remain on 100mg/L.After fully stirring evenly, standing demix extracts upper strata mixing oil phase, and then 8m
3Isohexane at 40 ~ 50 ℃, stirs 0.8h under the 80rpm rotating speed, behind the standing demix, extracts upper strata mixing oil phase.The algae-residue of lower floor obtains algae-residue by solid-liquid separation after the drying, can be used for animal-feed and use.The mixing oil phase that obtains by evaporating solvent, obtains the algae crude oil.
Degumming technology: adopt phosphoric acid acidifying degumming technology, algae crude oil temperature is 80 ~ 85 ℃, and the phosphoric acid add-on is 0.4% of algae crude oil weight, and the hot water add-on is 10% of algae crude oil weight during washing, washes twice.
Decoloration process: temperature is 100 ~ 105 ℃, and the atlapulgite addition is 4% of the algae crude oil weight of coming unstuck, vacuum tightness (gauge pressure) is-and below the 0.094mpa.
Depickling/deodorizing technology: temperature is 120 ℃, and vacuum tightness (gauge pressure) is-and below the 0.094mpa, the time is 1.5h.
Obtain being rich in the microalgae grease of DHA by above-mentioned technique.
Measuring the fermented liquid biomass is 48g/L, and the total fatty acid content of extraction is that 26%, DHA content (being the ratio that DHA accounts for total fatty acids) is 37.25%.
Embodiment 5
After adopting fragmentation kettle algae ampere tank to be inoculated into the inclined-plane, carry out after liquid shaking bottle cultivates, switching enters 6m again
3Fermentor cultivation, the substratum under it consists of: glucose 100-130g, yeast extract paste 15-30g, peptone 10-20g, potassium primary phosphate 2-4g, sal epsom 1-3g, trace element complex liquid 8-11ml, VITAMIN complex liquid 4-8ml is settled to 1L with 0.5 * seawater; Described 0.5 * seawater is that the water with the seawater of 1 volume and 1 volume is mixed to get.
The preparation method of described micro-complex liquid is as follows: Na2EDTA 6.0g, FeCl
36H
2O 0.29g, H
3BO
36.84g, MnCl
24H
2O 0.86g, ZnCl
20.06g, CoCl
26H
2O 0.026g, NiSO
46H
2O0.052g, CuSO
45H
2O 0.002g, NaMoO
42H
2O 0.005g, water is settled to 1L.
The preparation method of described VITAMIN complex liquid is as follows: VITMAIN B1 100mg, and vitamin B7 0.5mg, vitamin B12 0.5mg, water is settled to 1L.
The parameter of described fermentation culture is: 25 ~ 30 ℃ of temperature, and pH value 5.5 ~ 7.5, incubation time 72 ~ 96h, the parameter of described fermentation culture is preferably 25 ℃ of temperature, pH value 6.0, incubation time 96h, dissolved oxygen 10%.
The fermented liquid 4m of fragmentation kettle algae
3, with lemon acid for adjusting pH to 4.0.Add 5m
3No. six solvents at 50 ~ 60 ℃, stir 2h under the 150rpm rotating speed, realize the broken wall of fragmentation kettle frustule, and extract simultaneously microalgae grease, then add the biological flocculant chitosan, make chitosan concentration remain on 300mg/L.After fully stirring evenly, standing demix extracts upper strata mixing oil phase, and then adds 5m
3No. six solvents at 50 ~ 60 ℃, stir 0.5h under the 150rpm rotating speed, behind the standing demix, extract upper strata mixing oil phase.The algae-residue of lower floor obtains algae-residue by solid-liquid separation after the drying, can be used for animal-feed and use.The mixing oil phase that obtains by evaporating solvent, obtains the algae crude oil.
Degumming technology: adopt phosphoric acid acidifying degumming technology, algae crude oil temperature is 80 ~ 85 ℃, and the phosphoric acid add-on is 0.4% of algae crude oil weight, and the hot water add-on is 8% of algae crude oil weight during washing, washes five times.
Decoloration process: temperature is 100 ~ 105 ℃, and the atlapulgite addition is 4% of the algae crude oil weight of coming unstuck, vacuum tightness (gauge pressure) is-and below the 0.094mpa.
Depickling/deodorizing technology: temperature is 280 ℃, and vacuum tightness (gauge pressure) is-and below the 0.094mpa, the time is 1h.
Obtain being rich in the microalgae grease of DHA by above-mentioned technique.
Measuring the fermented liquid biomass is 39g/L, and the total fatty acid content of extraction is that 24%, DHA content (being the ratio that DHA accounts for total fatty acids) is 38.14%.
Applicant's statement, the present invention illustrates method detailed of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned method detailed, does not mean that namely the present invention must rely on above-mentioned method detailed and could implement.The person of ordinary skill in the field should understand, any improvement in the present invention to the interpolation of the equivalence replacement of each raw material of product of the present invention and ancillary component, the selection of concrete mode etc., all drops within protection scope of the present invention and the open scope.
Claims (10)
1. a method of extracting grease from fragmentation kettle algae is characterized in that described method comprises the steps:
(1) pH that regulates fragmentation kettle algae fermented liquid adds organic solvent to acid, stirs, and realizes the broken wall of fragmentation kettle frustule and the extraction of microalgae grease;
(2) after adding the flocculation agent flocculation treatment in the fermented liquid that obtains to step (1), adopt organic solvent extraction to obtain the algae crude oil;
(3) the algae crude oil is through coming unstuck, decolouring, and depickling/deodorization obtains being rich in the microalgae grease of DHA.
2. the method for claim 1 is characterized in that, described flocculation agent is biological flocculant, preferred chitosan.
3. method as claimed in claim 1 or 2 is characterized in that, vacuum depickling/deodorizing technology is adopted in the described depickling of step (3)/deodorization.
4. method as claimed in claim 2 or claim 3 is characterized in that step (2) comprises the steps:
Add biological flocculant in the fermented liquid that (2a) obtains to step (1), after fully stirring evenly, standing demix extracts upper strata mixing oil phase;
(2b) in step (2a) extract to be mixed fermented liquid behind the oil phase, again add organic solvent, 40 ~ 60 ℃ of lower stirrings, behind the standing demix, extract upper strata mixing oil phase;
Solvent evaporation in the mixing oil phase that (2c) step (2a) and step (2b) is obtained obtains the algae crude oil.
5. method as claimed in claim 4 is characterized in that, step (1) is regulated pH to 3.5 ~ 4.5, preferred 3.7 ~ 4.2;
Preferably, step (1) adopts acid for adjusting pH value, described acid to be selected from the mixture of any one or at least two kinds in hydrochloric acid, phosphoric acid, acetic acid or the citric acid;
Preferably, step (1) is 40 ~ 60 ℃ of lower stirrings, preferably 45 ~ 55 ℃ of lower stirrings;
Preferably, in step (1) and the step (2b), the volume of organic solvent is 0.8 ~ 2 times of step (1) fermentating liquid volume, preferred 1 ~ 1.5 times;
Preferably, described organic solvent is selected from the mixture of any one or at least two kinds in No. six solvents, normal hexane, isohexane or the iso-pentane.
6. such as the described method of one of claim 2-5, it is characterized in that the addition of described biological flocculant is the fermented liquid that 100 ~ 500mg/L step (1) obtains, preferred addition is the fermented liquid that 300 ~ 500mg/L step (1) obtains.
7. such as the described method of one of claim 4-6, it is characterized in that the stir speed (S.S.) of described stirring is 80 ~ 150rpm, preferred 90 ~ 140rpm, further preferred 100 ~ 130rpm;
Preferably, the described churning time of step (1) is 2 ~ 6 hours, preferred 2.5 ~ 5.5 hours;
Preferably, the described churning time of step (2b) is 0.5 ~ 1 hour, preferred 0.6 hour ~ 0.9 hour.
8. such as the described method of one of claim 4-7, it is characterized in that described coming unstuck adopted phosphoric acid acidifying degumming technology; Preferably, described phosphoric acid acidifying degumming technology is: the algae crude oil that step (2) or step (2c) are obtained is preheating to 80 ~ 85 ℃, 0.3 ~ 0.5% the phosphoric acid that adds algae crude oil weight that step (2) or step (2c) obtain, after acidifying is come unstuck, 90 ~ 95 ℃ washing 2 ~ 5 times, the algae crude oil that comes unstuck after obtaining coming unstuck; The weight of described each washing water is 5 ~ 10% of the algae crude oil weight that obtains of step (2) or step (2c);
Preferably, gac or activated decoloration are adopted in described decolouring;
Preferably, described decoloration process is under vacuum condition, and temperature is 100 ~ 105 ℃, and gac or atlapulgite that the algae crude oil after come unstuck adds the rear algae crude oil weight 3 ~ 5% of coming unstuck decolour, vacuum tightness is-below the 0.094mPa;
Preferably, vacuum depickling/deodorizing technology is adopted in described depickling/deodorization, and described technique is: the algae crude oil after will decolouring is that 120 ~ 280 ℃, vacuum tightness be-below the 0.094mPa, decoloured 1 ~ 2 hour in temperature;
Preferably, after step (2b) extracts upper strata mixing oil phase, be positioned at the algae-residue in middle level by solid-liquid separation, obtain after the drying.
9. such as the described method of one of claim 4-8, it is characterized in that described method comprises the steps:
(1) pH to 3.5 of adjusting fragmentation kettle algae fermented liquid ~ 4.5 add organic solvent, 40 ~ 60 ℃ of lower stirrings, realize the broken wall of fragmentation kettle frustule and the extraction of microalgae grease;
Add biological flocculant in the fermented liquid that (2a) obtains to step (1), after fully stirring evenly, standing demix extracts upper strata mixing oil phase;
(2b) in step (2a) extract to be mixed fermented liquid behind the oil phase, again add organic solvent, 40 ~ 60 ℃ of lower stirrings, behind the standing demix, extract upper strata mixing oil phase;
Solvent evaporation in the mixing oil phase that (2c) step (2a) and step (2b) is obtained obtains the algae crude oil;
(3) the algae crude oil is through coming unstuck, decolouring, and depickling/deodorization obtains being rich in the microalgae grease of DHA.
10. method as claimed in claim 8 or 9 is characterized in that described method comprises the steps:
(1) pH to 3.5 of adjusting fragmentation kettle algae fermented liquid ~ 4.5 add organic solvent, 40 ~ 60 ℃ of lower stirrings, realize the broken wall of fragmentation kettle frustule and the extraction of microalgae grease;
Add biological flocculant in the fermented liquid that (2a) obtains to step (1), after fully stirring evenly, standing demix extracts upper strata mixing oil phase;
(2b) again add organic solvent in step (2a) extract to be mixed fermented liquid behind the oil phase, 40 ~ 60 ℃ of lower stirrings, behind the standing demix, extract upper strata mixings oil phase, the algae-residue in middle level passes through solid-liquid separation, obtains after the drying;
Solvent evaporation in the mixing oil phase that (2c) step (2a) and step (2b) is obtained obtains the algae crude oil;
(3) the algae crude oil that step (2) or step (2c) is obtained is preheating to 80 ~ 85 ℃, 0.3 ~ 0.5% the phosphoric acid that adds algae crude oil weight that step (2) or step (2c) obtain, after acidifying is come unstuck, 90 ~ 95 ℃ washing 2 ~ 5 times, the algae crude oil that comes unstuck after obtaining coming unstuck; The weight of described each washing water is 5 ~ 10% of the algae crude oil weight that obtains of step (2) or step (2c); Under vacuum condition, temperature is 100 ~ 105 ℃, and gac or atlapulgite that the algae crude oil after come unstuck adds the rear algae crude oil weight 3 ~ 5% of coming unstuck decolour, vacuum tightness is-below the 0.094mPa; Be that 120 ~ 280 ℃, vacuum tightness be-below the 0.094mPa, decoloured 1 ~ 2 hour with the algae crude oil after the decolouring in temperature, obtain being rich in the microalgae grease of DHA, obtain simultaneously the part free fatty acids.
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| CN109734264A (en) * | 2018-11-20 | 2019-05-10 | 江南大学 | A method of promoting the release of bloom blue algae content |
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| CN114343021B (en) * | 2021-12-22 | 2024-04-05 | 嘉必优生物技术（武汉）股份有限公司 | Application of DHA algae oil for improving fishy smell in edible oil |
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