CN115109647A - Oil extraction method and obtained oil - Google Patents
Oil extraction method and obtained oil Download PDFInfo
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- CN115109647A CN115109647A CN202210644600.6A CN202210644600A CN115109647A CN 115109647 A CN115109647 A CN 115109647A CN 202210644600 A CN202210644600 A CN 202210644600A CN 115109647 A CN115109647 A CN 115109647A
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- 238000000605 extraction Methods 0.000 title claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000006228 supernatant Substances 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 43
- 239000002904 solvent Substances 0.000 claims abstract description 33
- 239000012535 impurity Substances 0.000 claims abstract description 29
- 238000002156 mixing Methods 0.000 claims abstract description 23
- 239000000725 suspension Substances 0.000 claims abstract description 22
- 241001052560 Thallis Species 0.000 claims abstract description 18
- 150000003904 phospholipids Chemical class 0.000 claims abstract description 18
- 150000002978 peroxides Chemical class 0.000 claims abstract description 15
- BHAAPTBBJKJZER-UHFFFAOYSA-N p-anisidine Chemical compound COC1=CC=C(N)C=C1 BHAAPTBBJKJZER-UHFFFAOYSA-N 0.000 claims abstract description 13
- 241000894006 Bacteria Species 0.000 claims abstract description 12
- 239000003921 oil Substances 0.000 claims description 46
- 239000010779 crude oil Substances 0.000 claims description 34
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 33
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- 230000000813 microbial effect Effects 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 3
- 235000020777 polyunsaturated fatty acids Nutrition 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims 1
- 238000004062 sedimentation Methods 0.000 abstract description 21
- 239000004519 grease Substances 0.000 abstract description 10
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 26
- 230000000052 comparative effect Effects 0.000 description 13
- 241000199914 Dinophyceae Species 0.000 description 11
- 238000000926 separation method Methods 0.000 description 9
- 238000005119 centrifugation Methods 0.000 description 8
- 238000001556 precipitation Methods 0.000 description 8
- 239000003925 fat Substances 0.000 description 7
- 238000000227 grinding Methods 0.000 description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 239000000498 cooling water Substances 0.000 description 6
- 239000002028 Biomass Substances 0.000 description 5
- 241000233671 Schizochytrium Species 0.000 description 5
- 210000004027 cell Anatomy 0.000 description 5
- 241000233866 Fungi Species 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 230000001580 bacterial effect Effects 0.000 description 3
- 244000005700 microbiome Species 0.000 description 3
- 238000000638 solvent extraction Methods 0.000 description 3
- 241000195493 Cryptophyta Species 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004332 deodorization Methods 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 239000013557 residual solvent Substances 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- 241000003595 Aurantiochytrium limacinum Species 0.000 description 1
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 1
- 238000005273 aeration Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000013592 cell lysate Substances 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000006911 enzymatic reaction Methods 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000000703 high-speed centrifugation Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000010813 municipal solid waste Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Microbiology (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention provides a method for extracting grease and the grease obtained by the method. The oil extraction method comprises the following steps: after the dry thalli are physically broken, adding an extraction solvent to obtain a suspension, adding water for mixing, and settling to obtain a supernatant; the amount of the water is 0.5-2 times of the mass of the dry bacteria. The oil extraction method provided by the invention can obtain the oil with very low impurity content without a degumming step by adding a specific amount of water for sedimentation after the extraction step, and simultaneously, other indexes of the obtained oil, such as peroxide value, anisidine and phospholipid content, are all in a required range.
Description
Technical Field
The invention relates to the technical field of oil extraction, and particularly relates to an oil extraction method and obtained oil.
Background
The dinoflagellate has single fatty acid component, the DHA content is up to 35-50%, and the schizochytrium has high DHA content, so that the two microorganisms are one of the most ideal sources for producing DHA by a fermentation method. In the prior art, many methods for extracting the DHA oil from dinoflagellate and schizochytrium through a solvent-free method are adopted, an enzymatic method or a physical method is adopted to break the wall to obtain cell lysate, and then the DHA oil is obtained through means of demulsification, separation and the like, but the method for breaking the wall of the algae with thicker cell walls in the solvent-free method is complex, and meanwhile, the steps of demulsification and separation need means of heating, repeated centrifugation and the like, so that the process for extracting the oil becomes complex. The advantages of the solvent method for extracting the oil in the aspects of convenient process, cost control, simple fungus residue treatment and the like cannot be ignored, so the solvent method extraction is still an important technical reserve.
Disclosure of Invention
The present invention can be used for various spherical oleaginous microorganisms, such as algae and yeast, which are different from filamentous fungi in the solvent extraction process in that the filamentous fungi are easy to settle and filter in the solvent extraction process, and the spherical microorganisms have low density and small cell particles and are difficult to remove by the same method due to oil content. Although the bacteria residue can be separated from the mixture with the solvent by a centrifuge in some small experimental embodiments, different bacteria bodies need to search for different centrifugation processes, and explosion-proof centrifugation equipment needs to be adopted after the treatment capacity is increased to an industrial level, and obviously, the explosion-proof centrifugation equipment of the industrial level needs high cost investment, and the first aim of the invention is to provide a method for extracting the oil and fat, which has simple process and is suitable for industrialization, and the method for extracting the oil and fat comprises the following steps: after the dry thalli are physically broken, adding an extraction solvent to obtain a suspension, adding water for mixing, and settling to obtain a supernatant; the amount of the water is 0.5-2 times of the mass of the dry bacteria.
The grease obtained by the grease extraction method can well give consideration to peroxide value, anisidine, impurity content and phospholipid content. In the extraction method, the core invention is that after the dry thalli are physically broken, an extraction solvent is added to form a suspension, and then water with the mass of 0.5-2 times that of the dry thalli is added for mixing.
In one embodiment of the invention, the amount of water is a core point of the invention, the added amount is small, sedimentation is difficult, separation is difficult, the added amount is excessive, sedimentation time is long, and dehydration of fungus dregs in later period is difficult. The amount of water added is preferably 0.5 to 1 time of the mass of the dry bacteria.
In the embodiment of the present invention, it is preferable that the dry microbial cells are physically broken until the cell disruption rate reaches 95% or more. The wall breaking can be carried out by physical methods known in the art, for example, by various methods in the applicant's previously filed application, cn202010421634.x, such as micronization, to increase the wall breaking rate to 99%.
In a specific embodiment of the present invention, the mixing time after adding water is preferably 30min to 2 h. In the "sedimentation" step of the present invention: the settling time after adding water and mixing is preferably not less than 0.5 h. The preferable settling temperature is 45-50 ℃. The settling pressure is preferably 0.1-0.2 MPa.
In one embodiment of the present invention, the step of adding water for sedimentation may be repeated, and the step of adding water for sedimentation may be repeated 1 to 3 times, preferably 1 time, for example, when the object to be treated is schizochytrium or dinoflagellate, the object of the present invention can be achieved by repeating sedimentation once, and a preferable index can be achieved. Namely, the oil extraction method comprises the following steps: after the dry thalli are subjected to physical wall breaking, adding an extraction solvent to obtain a suspension, adding water with the mass of 0.5-2 times that of the dry thalli, mixing, and settling to obtain a supernatant; and adding water with the mass of 0.5-2 times of that of the solid impurities (in the supernatant) into the supernatant, mixing, and settling again to obtain the supernatant. Wherein, the water is added into a certain amount and then fully and uniformly mixed, and the mixing time is preferably 30 min-2 h. In the invention, if the precipitation comprises multiple times of water addition and precipitation, the supernatant in other steps after the precipitation step refers to the supernatant obtained after the last precipitation if no special description is provided. When water is required to be added for sedimentation repeatedly, the sedimentation time after water is added and mixed in the sedimentation step is preferably not less than 0.5h, the sedimentation temperature is preferably 45-50 ℃, and the sedimentation pressure is preferably 0.1-0.2 Mpa. Wherein, in a complete extraction step, the temperature and pressure of each water adding sedimentation can be the same or different.
In a preferred embodiment of the present invention, in order to further reduce the peroxide number and the phospholipid content on the basis of considering the acid value, the impurity content and the solvent residue, the oil extraction method provided by the present invention further comprises a concentration step of concentrating the obtained supernatant to obtain a concentrated solution, such that the crude oil content in the concentrated solution is 20% to 30%. In the present invention, the concentration step may be placed after all the sedimentation steps, or may be placed between the multiple sedimentation steps. In a preferred embodiment of the present invention, the method for extracting fats and oils comprises two steps of adding water for sedimentation, and the concentration step is carried out between the two steps of sedimentation.
The oil extraction method provided by the invention preferably comprises the following steps:
(1) after the dry thalli are physically broken, adding an extraction solvent to obtain a suspension, adding water for mixing, and settling to obtain a supernatant; the amount of the water is 0.5-2 times of the mass of the dry thalli;
(2) concentrating the supernatant obtained in the step (1) to obtain a concentrated solution, so that the crude oil content in the concentrated solution is 20-30%;
(3) and (3) adding water with the mass of 0.5-2 times of that of solid impurities in the concentrated solution into the concentrated solution obtained in the step (2), mixing, settling and taking supernatant.
In embodiments of the present invention, the extraction solvent includes, but is not limited to, hexane, ethyl acetate, isopropanol, n-hexane, and the like. The amount of the extraction solvent is preferably 8 to 10 times the mass of the dry cells. In the invention, the extractant can be added at one time or added in batches. If the extraction agent is added in batches, water is only added for sedimentation when the extraction agent is added for the first time, and water is not added for extraction in the later batches.
In one embodiment of the present invention, the method for extracting oil and fat of the present invention further comprises a desolventizing step. Wherein, the desolventizing step can be a desolventizing step commonly used in the field, and preferably comprises the following steps: desolventizing at 40-50 ℃ until the content of the solvent is less than or equal to 10%, keeping the pressure at less than or equal to-0.08 Mpa, a) controlling the temperature at 100-110 ℃, introducing steam, preserving heat for 1-3 h, introducing nitrogen, and preserving heat for 1-3 h; repeating the step a) for 0-2 times.
In the embodiment of the present invention, the aeration amount of the steam and the nitrogen gas can be set according to actual needs. In some specific embodimentsThe preferred ventilation rate of the steam is 0.02-0.1 m 3 H, the ventilation amount of nitrogen is 0.02-0.1 m 3 /h。
In the embodiment of the present invention, the number of repetitions is 0 or 1 or 2, and for example, the repetitions may be 0 (i.e., 1 operation), 1 (i.e., 2 operations) or 2 (i.e., 3 operations). The holding time of each time can be shortened as required, for example, the holding time is 1h, and the number of times of alternation is three (namely, the repetition is 2 times).
In a preferred embodiment of the invention, the temperature is reduced to below 30 ℃ after the end of the desolventizing.
The extraction method provided by the invention is more suitable for extracting the grease in dinoflagellate or schizochytrium. The dry thallus of the invention is preferably dinoflagellate or schizochytrium.
The extraction method provided by the invention can obtain the oil with very low impurity content without additional degumming and deodorization steps. In a preferred embodiment of the present invention, the method for extracting oil and fat of the present invention comprises the steps of extraction, precipitation with water, concentration, precipitation with water (or multiple precipitation with water if there are multiple precipitations with water), and desolventizing. The oil extraction method does not need additional degumming step and deodorization step.
In the present invention, "%" represents mass%, and the unit of acid value is mg/g in KOH, and the unit of peroxide value is meq/kg, unless otherwise specified.
Another object of the present invention is to provide the fat obtained by the above-mentioned fat extraction method.
The invention also aims to provide the microbial crude oil extracted by the solvent method, wherein the content of polyunsaturated fatty acid is higher than 40%, the content of phospholipid is not higher than 160ppm, the acid value is not higher than 2 (mg/g in KOH), the solvent residue is not higher than 100ppm, the peroxide value is not higher than 1meq/kg, the anisidine value is not higher than 5, and the impurity content in the oil is not higher than 5%. By optimizing the process of oil extraction, the impurity content can be less than 1%.
In the field, as crude oil can be refined to obtain finished oil, the index control of the crude oil is not high, and the crude oil obtained by solvent extraction has very high solvent residue which can reach 3000ppm, and the phospholipid content in the crude oil can also be as high as 800ppm, so that the requirement of direct application is difficult to meet. The index-controlled microbial crude oil, especially DHA crude oil, provided by the invention has the DHA content of more than or equal to 40%, and has the highest index control difficulty of DHA grease due to the high unsaturation degree of DHA.
The oil extraction method provided by the invention can be used for obtaining the oil with very low impurity content without adopting expensive explosion-proof centrifugal equipment by adding a specific amount of water for sedimentation after the extraction step without degumming, and simultaneously, other indexes of the obtained oil, such as peroxide value, anisidine, solvent residue and phospholipid content, are all in a required range. The crude oil obtained by the method provided by the invention has part index close to the refined oil level, but the required technological process is far less than that of refining the grease, and the expensive cost is not required.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
1. The dinoflagellate dry thalli is subjected to superfine grinding to break the wall, the wall breaking rate reaches 99%, and the single treatment capacity is 2 tons.
2. Hexane was added in an amount 8 times the amount of dried biomass and mixed to form an extract suspension.
3. Adding water with the amount of 0.5 times of that of the dry bacteria into the extracted suspension, mixing for 0.5h, settling at 50 ℃ under 0.1Mpa for 1h, and collecting the supernatant after the settling is finished.
4. The supernatant was concentrated to an oil content of 20%, at which point the solid impurities content was about 3%.
5. And (3) settling and separating again: adding water with solid impurity amount 0.8 times of the concentrated supernatant obtained in step 4, mixing at 50 deg.C and settling pressure 0.1Mpa for 1 hr, settling for 4 hr, and collecting supernatant.
6. Desolventizing: desolventizing the supernatant obtained in the step 5 at 50 ℃ and under-0.08 Mpa until the content of the solvent reaches 10%, maintaining the pressure at-0.08 Mpa, introducing steam at 105 +/-2 ℃, preserving heat for 1h, introducing nitrogen at 105 +/-2 ℃, preserving heat for 1h, wherein the flow of the introduced steam is 0.05m 3 Per, nitrogen flow of 0.05m 3 And/h, alternately operating for 2 times, and cooling by cooling water to obtain DHA crude oil with the extraction rate of 93.8%.
The indexes of the obtained DHA crude oil are as follows: acid value 1.2, peroxide value 0.04, anisidine 2.3, impurity content 0.2%, solvent residue 17ppm, phospholipid 68 ppm.
Example 2
1. The dinoflagellate dry thalli are subjected to superfine grinding to break the walls, the wall breaking rate reaches 99%, and the treatment capacity is 2 tons.
2. Hexane was added in an amount 8 times the amount of dried biomass and mixed to form an extract suspension.
3. Adding water with 2 times of dry bacteria amount into the extract suspension, mixing for 0.5 hr, settling at 50 deg.C under 0.1Mpa for 2 hr, and collecting supernatant.
4. Desolventizing: desolventizing the supernatant in the step 3 at 50 ℃ and 0.08Mpa until the content of the solvent reaches 10 percent, keeping the pressure at 0.08Mpa, introducing steam, controlling the temperature range at 105 +/-2 ℃, preserving heat for 1 hour, introducing nitrogen, controlling the temperature range at 105 +/-2 ℃, preserving heat for 1 hour, wherein the flow of the introduced steam is 0.05m 3 Per, nitrogen flow of 0.05m 3 And/h, alternately operating for 2 times, and cooling by cooling water to obtain DHA crude oil.
The indexes of the obtained DHA crude oil are as follows: acid value of 1.4, peroxide value of 0.2, anisidine content of 4.8, impurity content of 5%, residual solvent of 100ppm, and phospholipid content of 160 ppm.
Example 3
1. The dinoflagellate dry thalli are subjected to superfine grinding to break the walls, the wall breaking rate reaches 99%, and the treatment capacity is 2 tons.
2. Hexane was added in an amount 8 times the amount of dried biomass and mixed to form an extract suspension.
3. Adding water with the amount of 0.5 times of dry bacteria into the extract suspension, mixing for 0.5h, settling at 50 deg.C under 0.1Mpa for 1h, and collecting supernatant.
4. And (3) settling and separating again: adding water with 1 time of solid impurity amount (in the supernatant) into the supernatant of the step 3, settling at 50 ℃ under 0.1Mpa for 1h, mixing for 4h, and sucking the supernatant.
5. Desolventizing: desolventizing the supernatant obtained in the step 4 at 50 ℃ and under-0.08 Mpa until the content of the solvent reaches 10%, maintaining the pressure at-0.08 Mpa, introducing steam at 105 +/-2 ℃, preserving heat for 1h, introducing nitrogen at 105 +/-2 ℃, preserving heat for 1h, wherein the flow of the introduced steam is 0.05m 3 Per, nitrogen flow of 0.05m 3 And/h, alternately operating for 2 times, and cooling by cooling water to obtain DHA crude oil.
The indexes of the obtained DHA crude oil are as follows: acid value 1.6, peroxide value 0.4, anisidine 4.0, impurity content 0.4%, solvent residue 50ppm, phospholipid 100 ppm.
Example 4
1. The dinoflagellate dry thalli are subjected to superfine grinding to break the walls, the wall breaking rate reaches 99%, and the treatment capacity is 2 tons.
2. Hexane was added in an amount 10 times the amount of dried mycelia, and mixed to form an extraction suspension.
3. Adding water with the amount of 1 time of dry bacteria into the extract suspension, mixing for 1h, settling at 45 deg.C under 0.2Mpa for 0.5h, and collecting supernatant.
4. The supernatant was concentrated to an oil content of 20%, at which point the solid impurities content was about 3%.
5. And (3) settling and separating again: adding water with 1 time of solid impurities amount into the concentrated supernatant obtained in the step 4, settling at 45 ℃ under 0.2Mpa for 1h, settling for 4h, and sucking the supernatant.
6. Threshing deviceDissolving: desolventizing the supernatant obtained in the step 5 at 40 ℃ and under-0.08 Mpa until the content of the solvent reaches 10%, maintaining the pressure at-0.08 Mpa, introducing steam at 105 +/-2 ℃, preserving heat for 1h, introducing nitrogen at 105 +/-2 ℃, preserving heat for 1h, wherein the flow of the introduced steam is 0.05m 3 H, nitrogen flow is 0.05m 3 And/h, alternately operating for 3 times, and cooling by cooling water to obtain DHA crude oil with an extraction rate of 93.0%.
The indexes of the obtained DHA crude oil are as follows: acid value of 1.0, peroxide value of 0.05, anisidine of 2.0, impurity content of 0.3%, residual solvent of 15ppm, and phospholipid of 60 ppm.
Example 5
1. The dried schizochytrium limacinum thallus is subjected to superfine grinding to break the wall, the wall breaking rate reaches 99 percent, and the treatment amount is 2 tons.
2. Hexane was added in an amount 8 times the amount of dried biomass and mixed to form an extract suspension.
3. Adding water with the amount of 0.5 times of the dry bacteria into the extract suspension, mixing for 0.5h, settling at 50 deg.C under 0.1Mpa for 1h, and collecting supernatant.
4. The supernatant was concentrated to an oil content of 20%, at which point the solid impurities content was about 3.5%.
5. And (3) settling and separating again: adding water with solid impurity amount 0.8 times of the concentrated supernatant obtained in step 4, mixing at 50 deg.C and settling pressure 0.1Mpa for 1 hr, settling for 4 hr, and collecting supernatant.
6. Desolventizing: desolventizing the supernatant obtained in the step 5 at 45 ℃ and under-0.08 Mpa until the content of the solvent reaches 10%, maintaining the pressure at-0.08 Mpa, introducing steam at the temperature of 102 +/-2 ℃, preserving heat for 1h, introducing nitrogen at the temperature of 102 +/-2 ℃, preserving heat for 1h, wherein the flow of the introduced steam is 0.05m 3 Per, nitrogen flow of 0.05m 3 And/h, alternately operating for 3 times, and cooling by cooling water to obtain DHA crude oil with the extraction rate of 92.3%.
The indexes of the obtained DHA crude oil are as follows: acid value 1.1, peroxide value 0.02, anisidine 2.7, impurity content 0.2%, solvent residue 15ppm, phospholipid 34 ppm.
Comparative example 1
The extraction procedure of this comparative example is the same as example 1, except that: directly mixing the dinoflagellate dry thalli with hexane which is 8 times of the dry thalli amount to form an extraction suspension without adopting superfine grinding for wall breaking. No oil was detected in the suspension.
Comparative example 2
The extraction method of the comparative example is different from that of example 1 in that water is not added for sedimentation after the suspension is formed in the step 2, and the bacterial residues cannot be naturally settled, the grease is difficult to separate, and the subsequent steps cannot be carried out.
Comparative example 3
The extraction method of the comparative example is different from that of example 1 in that step 3 does not adopt hydration, part of the sample is directly taken for high-speed centrifugation, the thalli is separated by centrifugation for 10min under the condition of 10000r/min, and simultaneously, step 5 adopts the same method for re-centrifugation. And finally desolventizing by adopting a centrifugal separation method to obtain crude oil with the acid value of 1.5, the peroxide value of 0.1, the anisidine content of 3.2, the impurity content of 0.5 percent, the solvent residue of 44ppm and the phospholipid content of 500 ppm.
In the comparative example, a centrifuge is adopted for separation, so that the effect of obtaining crude oil, such as indexes such as impurity content, is not obviously superior to that of the example 1, and the phospholipid content cannot be effectively reduced by a centrifugal mode.
Comparative example 4
1. The dinoflagellate dry thalli are subjected to superfine grinding to break the walls, the wall breaking rate reaches 99%, and the treatment capacity is 2 tons.
2. Hexane was added in an amount 8 times the amount of dried biomass and mixed to form an extract suspension.
3. Adding water with the amount 0.1 time of the dry bacteria into the suspension, mixing for 0.5h, settling for 1h, and sucking the supernatant.
4. The supernatant was concentrated to an oil content of 30% and a solid impurity content of about 10%.
5. And (3) settling and separating again: adding water with the amount of 0.2 time of solid impurities into the concentrated supernatant obtained in the step 4, mixing for 1h at 50 ℃, settling for 4h, and sucking the supernatant.
6. Desolventizing: subjecting the product obtained in step 5Desolventizing the supernatant at 50 deg.C under-0.08 Mpa until the solvent content reaches 10%, maintaining the pressure at-0.08 Mpa, introducing steam at 105 + -2 deg.C for 1 hr, introducing nitrogen at 105 + -2 deg.C for 1 hr, wherein the flow rate of steam is 0.05m 3 Per, nitrogen flow of 0.05m 3 And/h, alternately operating for 3 times, and cooling by cooling water to obtain DHA crude oil.
The indexes of the obtained DHA crude oil are as follows: acid value 1.9, peroxide value 0.5, anisidine 9, impurity content 12%, solvent residue 300ppm, phospholipid 230 ppm.
Comparative example 5
The extraction method of the comparative example is different from that of example 5 in that hydration is not carried out after the bacterial suspension is formed in the step 2, and the bacterial residues cannot be naturally settled, so that grease is difficult to separate. After two separation steps by centrifugation as in comparative example 3, the crude oil obtained had an acid value of 1.5, a peroxide value of 0.2, anisidine of 3.8, a trash content of 0.4%, a solvent residue of 50ppm, and phospholipids of 350 ppm. Similarly, centrifugal separation has no obvious advantages compared with the method of the invention, but the method of the invention has lower requirements on equipment and is more suitable for matching with original industrial production equipment.
In the prior art, CN113684088A provides a method for extracting crude oil by water, which mainly comprises the steps of adopting water as a solvent in the extraction step to form emulsion, adjusting the pH value to 9, stirring at 55 ℃ for 6 hours, boiling at 95 ℃, and then carrying out centrifugal separation on the two to obtain the crude oil. Compared with the solvent-free direction, the crude oil obtained by the invention can obtain crude oil with equivalent quality, the oil extraction rate is higher, the working procedures of the sedimentation method are simpler and more convenient compared with the demulsification-separation direction in the method, and the requirement of refined oil on the phospholipid content can be met in the process of extracting the crude oil. In the prior art, CN113684088A also provides a method for extracting oil by using isopropanol, which mainly comprises the step of extracting oil from thalli subjected to dry wall breaking by using isopropanol. However, this method does not refer to a specific step of separating the hydrated cells, and mainly adopts a two-phase system centrifugation method. The result of this process is the same as that of comparative example 3, the crude oil contained more than 350ppm of phospholipids and the oil extraction rate was inferior to that of the process of the present invention. The content of DHA in the main polyunsaturated fatty acid in the grease obtained in the embodiment and the comparative examples 3-5 is more than or equal to 40%, and most application requirements can be met.
Finally, the method of the present invention is only a preferred embodiment and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for extracting oil is characterized by comprising the following steps: after the dry thalli are physically broken, adding an extraction solvent to obtain a suspension, adding water for mixing, and settling to obtain a supernatant; the amount of the water is 0.5-2 times of the mass of the dry bacteria.
2. The method for extracting oil or fat according to claim 1, wherein the amount of water is 0.5 to 1 time the mass of the dry microbial cells.
3. The oil and fat extraction method according to any one of claims 1 or 2, further comprising the steps of:
and adding water which is 0.5-2 times of the amount of solid impurities in the supernatant into the supernatant, mixing, settling, and taking the supernatant.
4. The fat extraction method according to any one of claims 1 to 3, further comprising the steps of:
and concentrating the supernatant to obtain a concentrated solution, so that the content of the crude oil in the concentrated solution is 20-40%.
5. The oil extraction method according to claim 4, wherein water is added to the concentrated solution, the mixture is mixed for 0.5 to 2 hours, the mixture is settled, and supernatant liquid is taken and desolventized.
6. The oil extraction method according to any one of claims 1 to 5, wherein the settling time is not less than 0.5h, the settling temperature is 45 to 50 ℃, and the settling pressure is 0.1 to 0.2 MPa.
7. The method for extracting oil according to claim 6, wherein the dissolving comprises the following steps: desolventizing at 40-50 ℃ until the content of the solvent is less than or equal to 10%, keeping the pressure at less than or equal to-0.08 Mpa, a) controlling the temperature at 100-110 ℃, introducing steam, preserving heat for 1-3 h, introducing nitrogen, and preserving heat for 1-3 h; and c), repeating the step a) for 0-2 times.
8. The oil extraction method according to claim 7, wherein the steam is introduced in the step a) in an amount of 0.02-0.1 m 3 The nitrogen is introduced in an amount of 0.02-0.1 m 3 /h。
9. An oil or fat obtained by the oil or fat extraction method according to any one of claims 1 to 8.
10. A microbial crude oil extracted by a solvent method is characterized in that the content of polyunsaturated fatty acid in the microbial crude oil is higher than 40%, the content of phospholipid is not higher than 160ppm, the acid value is not higher than 2 (calculated by KOH), the solvent residue is not higher than 100ppm, the peroxide value is not higher than 1meq/kg, the anisidine value is not higher than 5, and the impurity content is not higher than 5%;
preferably, the impurity content is not higher than 1%.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104388179A (en) * | 2014-10-27 | 2015-03-04 | 山东广博生物技术服务有限公司 | Method for extracting DHA algae oil and algae protein from algae |
| CN107488501A (en) * | 2017-09-21 | 2017-12-19 | 嘉必优生物技术（武汉）股份有限公司 | Microbe-derived polyunsaturated fatty acid grease and its preparation technology |
| WO2017219964A1 (en) * | 2016-06-21 | 2017-12-28 | 嘉必优生物技术（武汉）股份有限公司 | Method for extracting microbial grease |
| CN111690462A (en) * | 2020-06-09 | 2020-09-22 | 厦门汇盛生物有限公司 | Method for demulsifying and extracting oil from oil-containing algae or fungus cell wall-broken liquid |
| CN113684087A (en) * | 2020-05-18 | 2021-11-23 | 嘉必优生物技术（武汉）股份有限公司 | Solvent-free extraction method of microbial oil and microbial oil obtained by solvent-free extraction method |
| CN113684088A (en) * | 2020-05-18 | 2021-11-23 | 嘉必优生物技术（武汉）股份有限公司 | Microbial oil extraction method and microbial oil obtained by same |
| CN113698985A (en) * | 2021-08-27 | 2021-11-26 | 山东三星玉米产业科技有限公司 | Process for removing residual solvent in production process of crude corn oil |
| CN114574282A (en) * | 2021-06-29 | 2022-06-03 | 嘉必优生物技术（武汉）股份有限公司 | Refined microbial oil and refining method |
-
2022
- 2022-06-09 CN CN202210644600.6A patent/CN115109647B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104388179A (en) * | 2014-10-27 | 2015-03-04 | 山东广博生物技术服务有限公司 | Method for extracting DHA algae oil and algae protein from algae |
| WO2017219964A1 (en) * | 2016-06-21 | 2017-12-28 | 嘉必优生物技术（武汉）股份有限公司 | Method for extracting microbial grease |
| CN107488501A (en) * | 2017-09-21 | 2017-12-19 | 嘉必优生物技术（武汉）股份有限公司 | Microbe-derived polyunsaturated fatty acid grease and its preparation technology |
| CN113684087A (en) * | 2020-05-18 | 2021-11-23 | 嘉必优生物技术（武汉）股份有限公司 | Solvent-free extraction method of microbial oil and microbial oil obtained by solvent-free extraction method |
| CN113684088A (en) * | 2020-05-18 | 2021-11-23 | 嘉必优生物技术（武汉）股份有限公司 | Microbial oil extraction method and microbial oil obtained by same |
| CN111690462A (en) * | 2020-06-09 | 2020-09-22 | 厦门汇盛生物有限公司 | Method for demulsifying and extracting oil from oil-containing algae or fungus cell wall-broken liquid |
| CN114574282A (en) * | 2021-06-29 | 2022-06-03 | 嘉必优生物技术（武汉）股份有限公司 | Refined microbial oil and refining method |
| CN113698985A (en) * | 2021-08-27 | 2021-11-26 | 山东三星玉米产业科技有限公司 | Process for removing residual solvent in production process of crude corn oil |
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