CN115109647B - Grease extraction method and obtained grease - Google Patents
Grease extraction method and obtained grease Download PDFInfo
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- CN115109647B CN115109647B CN202210644600.6A CN202210644600A CN115109647B CN 115109647 B CN115109647 B CN 115109647B CN 202210644600 A CN202210644600 A CN 202210644600A CN 115109647 B CN115109647 B CN 115109647B
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- 238000000605 extraction Methods 0.000 title claims abstract description 65
- 239000004519 grease Substances 0.000 title abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000006228 supernatant Substances 0.000 claims abstract description 41
- 238000004062 sedimentation Methods 0.000 claims abstract description 38
- 239000002904 solvent Substances 0.000 claims abstract description 35
- 239000000725 suspension Substances 0.000 claims abstract description 23
- 241001052560 Thallis Species 0.000 claims abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 34
- 239000010779 crude oil Substances 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 32
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 31
- 239000003921 oil Substances 0.000 claims description 31
- 238000002156 mixing Methods 0.000 claims description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims description 17
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000012535 impurity Substances 0.000 abstract description 26
- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical compound COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 abstract description 22
- 150000003904 phospholipids Chemical class 0.000 abstract description 17
- 150000002978 peroxides Chemical class 0.000 abstract description 14
- 230000001580 bacterial effect Effects 0.000 abstract description 11
- UZKWTJUDCOPSNM-UHFFFAOYSA-N methoxybenzene Substances CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 abstract description 11
- 210000004027 cell Anatomy 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 13
- 241000199914 Dinophyceae Species 0.000 description 12
- 238000000926 separation method Methods 0.000 description 12
- 239000002253 acid Substances 0.000 description 11
- 239000007787 solid Substances 0.000 description 10
- 238000005119 centrifugation Methods 0.000 description 7
- 238000000227 grinding Methods 0.000 description 7
- 238000001816 cooling Methods 0.000 description 6
- 239000000498 cooling water Substances 0.000 description 6
- 241000233671 Schizochytrium Species 0.000 description 4
- 244000005700 microbiome Species 0.000 description 4
- 241000233866 Fungi Species 0.000 description 3
- 238000005273 aeration Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000000638 solvent extraction Methods 0.000 description 3
- 241000003595 Aurantiochytrium limacinum Species 0.000 description 2
- 241000195493 Cryptophyta Species 0.000 description 2
- 238000004332 deodorization Methods 0.000 description 2
- 238000011534 incubation Methods 0.000 description 2
- 230000000813 microbial effect Effects 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 240000004808 Saccharomyces cerevisiae Species 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
- 235000014113 dietary fatty acids Nutrition 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
- 125000005313 fatty acid group Chemical group 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
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction 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
- BHAAPTBBJKJZER-UHFFFAOYSA-N p-anisidine Chemical compound COC1=CC=C(N)C=C1 BHAAPTBBJKJZER-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000020777 polyunsaturated fatty acids Nutrition 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000003807 solvent-free extraction 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 grease extraction method and grease obtained by the grease extraction method. The grease extraction method comprises the following steps: after physically breaking the wall of the dry thalli, adding an extraction solvent to obtain a suspension, adding water to mix, and settling to obtain a supernatant; the water amount is 0.5-2 times of the dry bacterial mass. According to the oil extraction method provided by the invention, the specific amount of water is added for sedimentation after the extraction step, so that the oil with very low impurity content can be obtained without a degumming step, and other indexes of the obtained oil, such as peroxide value, anisole and phospholipid content, are all in the required range.
Description
Technical Field
The invention relates to the technical field of oil extraction, in particular to an oil extraction method and oil obtained by the oil extraction method.
Background
As the composition of fatty acid is single, the DHA content of dinoflagellate is up to 35-50%, and schizochytrium limacinum also has higher DHA content, both microorganisms are one of the most ideal sources for producing DHA by fermentation. In the prior art, DHA grease in dinoflagellate and schizochytrium is obtained by a solvent-free extraction method, wherein an enzymatic method or a physical method is adopted to break the wall to obtain cell lysate, and then the DHA grease is obtained by means of demulsification, separation and the like, but the adopted wall breaking means are more complex for algae with thicker cell walls in the solvent-free method, and meanwhile, the demulsification and separation steps need to be carried out by means of heating, repeated centrifugation and the like, so that the process for extracting the grease becomes complex. The advantages of the solvent method for extracting the grease in the aspects of convenient process, cost control, simple fungus dreg treatment and the like still cannot be ignored, so the solvent method for extracting is still an important technical reserve.
Disclosure of Invention
The invention can be aimed at various spherical oleaginous microorganisms, such as algae and yeast, which are the biggest difference from filamentous fungi in the process of solvent extraction in that the filamentous fungi are very easy to settle and filter in the solvent extraction process, and the spherical microorganisms have lower density and smaller cell particles due to the oil content, so that the spherical microorganisms are difficult to remove by the same method. In some small-scale embodiments, although bacterial residues can be separated from a mixture with a solvent through a centrifuge, different bacterial bodies need to be searched for different centrifugation processes, and explosion-proof centrifugal equipment is needed after the treatment capacity is increased to an industrial level, and obviously, the explosion-proof centrifugal equipment of the industrial level needs high cost investment, the first purpose of the invention is to provide a grease extraction method which is simple in process and suitable for industrialization, and the grease extraction method comprises the following steps: after physically breaking the wall of the dry thalli, adding an extraction solvent to obtain a suspension, adding water to mix, and settling to obtain a supernatant; the water amount is 0.5-2 times of the dry bacterial mass.
The oil obtained by the oil extraction method can well give consideration to peroxide value, anisole, impurity content and phospholipid content. In the extraction method, the core invention is that after dry thalli is physically broken, an extraction solvent is added into the wall to form suspension, and then water with the mass of 0.5 to 2 times of that of the dry thalli is added into the suspension for mixing.
In one embodiment of the invention, the amount of water is a core point of the invention, and the amount added is small, difficult to settle, difficult to separate, excessive, long in settling time and difficult to dehydrate in the later stages. The amount of water added is preferably 0.5 to 1 time the mass of the dry cell.
In the embodiment of the present application, it is preferable that the dry cell is physically broken until the cell disruption rate reaches 95% or more. The wall breaking may be performed using physical methods known in the art, for example, using various methods such as ultra-micro pulverizing methods in the application of CN202010421634.X previously filed by the present inventors, the wall breaking rate may be increased to 99%.
In a specific embodiment of the present invention, the mixing time after adding water is preferably 30min to 2h. In the "sedimentation" step of the present invention: the sedimentation time after mixing with water is preferably not less than 0.5h. The sedimentation temperature is preferably 45 to 50 ℃. The sedimentation pressure is preferably 0.1 to 0.2Mpa.
In one embodiment of the invention, the water adding and sedimentation steps can be repeated, and the water adding and sedimentation steps can be repeated for 1-3 times, preferably 1 time, for example, when the treated object is schizochytrium or dinoflagellate, the aim of the invention can be achieved by repeating sedimentation once, and better indexes are achieved. Namely, the oil extraction method comprises the following steps: after physically breaking the wall of dry thalli, adding an extraction solvent to obtain a suspension, adding water with the mass of 0.5-2 times of that of the dry thalli, mixing, and settling to obtain a supernatant; adding water with the mass of 0.5-2 times of solid impurities (in the supernatant) into the supernatant, mixing, and settling again to obtain the supernatant. Wherein, the mixture is fully and uniformly mixed after adding a specific amount of water, and the mixing time is preferably 30 min-2 h. In the present invention, if the method includes multiple times of water adding and sedimentation, the supernatant fluid in other steps after the sedimentation step refers to the supernatant fluid obtained after the last sedimentation unless otherwise specified. When water adding sedimentation is required to be repeatedly carried out, in the sedimentation step, the sedimentation time after water adding and mixing 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. In one complete extraction step, the temperature and pressure of each water addition sedimentation can be the same or different.
In a preferred embodiment of the present invention, in order to further reduce the peroxide value and the phospholipid content on the basis of combining the acid value, the impurity content and the solvent residue, the oil extraction method provided by the present invention further includes a concentration step of concentrating the obtained supernatant to obtain a concentrated solution, so that the crude oil content in the concentrated solution is 20% -30%. In the present invention, the concentration step may be placed after all the sedimentation steps or between the sedimentation steps. In a preferred embodiment of the invention, the fat extraction process comprises two water-added settling steps, with a concentration step between the two settling steps.
The grease extraction method provided by the invention preferably comprises the following steps:
(1) After physically breaking the wall of the dry thalli, adding an extraction solvent to obtain a suspension, adding water to mix, and settling to obtain a supernatant; the water amount is 0.5-2 times of the dry thallus mass;
(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) Adding water with the mass of 0.5-2 times of the mass of the solid impurities in the concentrated solution into the concentrated solution obtained in the step (2), mixing, settling and taking the supernatant.
In an embodiment of the present invention, the extraction solvent includes, but is not limited to, hexane, ethyl acetate, isopropyl alcohol, 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 present invention, the extractant may be added at one time or may be added in divided portions. If added in batches, water is only added for sedimentation when the extractant is added for the first time, and water is not added for the extraction of the subsequent batches.
In one embodiment of the present invention, the fat extraction method of the present invention further comprises a desolventizing step. The desolventizing step may be a desolventizing step commonly used in the art, and preferably includes the following steps: desolventizing at 40-50 ℃ until the solvent content is less than or equal to 10%, keeping the pressure at less than or equal to-0.08 mpa, a) controlling the temperature within 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 embodiments of the present invention, the aeration rates of steam and nitrogen may be set according to actual needs. In some embodiments, the aeration rate of steam is preferably 0.02 to 0.1m 3/h and the aeration rate of nitrogen is 0.02 to 0.1m 3/h.
In the embodiment of the present invention, the number of repetitions is 0 times, 1 time or 2 times, for example, 0 times (i.e. 1 time of operation), 1 time (i.e. 2 times of operation) or 2 times (i.e. 3 times of operation). The incubation time per time can be optionally shortened, for example, the incubation time is 1h, and the number of alternations is three (i.e., 2 repetitions).
In a preferred embodiment of the invention, the temperature is reduced to below 30 ℃ after the desolventizing is completed.
The extraction method provided by the invention is more suitable for extracting grease from dinoflagellate or schizochytrium. The dry bacterial cells of the present invention are preferably dinoflagellates or schizochytrium.
The extraction method provided by the invention can obtain the grease with very low impurity content without extra degumming and deodorization steps. In a preferred embodiment of the present invention, the fat extraction method of the present invention comprises the steps of extraction, water addition sedimentation, concentration, water addition sedimentation (if there are multiple water addition sedimentation, multiple water addition sedimentation is also included), and desolventizing. The oil extraction method does not require an additional degumming step and deodorization step.
In the present invention, "%" is mass percent, acid value is in mg/g in KOH and peroxide value is in meq/kg unless otherwise specified.
Another object of the present invention is to provide a fat and oil obtained by the above fat and oil extraction method.
Still another object of the present invention is to provide a microbial crude oil obtained by extraction with a solvent method, wherein the polyunsaturated fatty acid content is higher than 40%, the phospholipid content 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 extracting the grease, the impurity content can be less than 1%.
In the field, as the crude oil can be refined to obtain the finished oil, the index control attention on 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 reach 800ppm, so that the direct application requirement is difficult to meet. The index-controlled microbial crude oil, particularly DHA crude oil, provided by the invention, has the DHA content of 40% or more, and the index control difficulty of DHA grease is highest due to the high unsaturation degree of DHA.
According to the oil extraction method provided by the invention, high explosion-proof centrifugal equipment is not adopted, a specific amount of water is added for sedimentation after the extraction step, oil with very low impurity content can be obtained without a degumming step, and other indexes of the obtained oil such as peroxide value, anisole, solvent residue and phospholipid content are all in the required range. The crude oil part index obtained by the method provided by the invention is close to the level of refined oil, but the required technological process is far less than that of refined grease, and expensive cost is not required.
Detailed Description
The following describes the embodiments of the present invention in further detail with reference to examples. The following examples are illustrative of the invention and are not intended to limit the scope of the invention.
Example 1
1. The dry cells of dinoflagellate are subjected to superfine grinding and wall breaking, the wall breaking rate reaches 99%, and the single treatment capacity is 2 tons.
2. Hexane was added in an amount 8 times the dry cell mass, and mixed to form an extraction suspension.
3. Adding water with the quantity of 0.5 times of dry thalli into the extraction suspension, mixing for 0.5h, settling, wherein the settling temperature is 50 ℃, the settling pressure is 0.1Mpa, the settling time is 1h, and sucking the supernatant after the settling is finished.
4. The supernatant was concentrated until the oil content reached 20%, at which point the solid impurity content was about 3%.
5. Sedimentation and separation are carried out again: adding water with the solid impurity content of 0.8 times into the concentrated supernatant obtained in the step 4, mixing for 1h at 50 ℃ under the settling pressure of 0.1Mpa, settling for 4h, and sucking the supernatant.
6. Desolventizing: and (3) desolventizing the supernatant obtained in the step (5) to the solvent content of 10% at 50 ℃ under the pressure of-0.08 Mpa, maintaining the pressure of-0.08 Mpa, introducing steam, maintaining the temperature at 105+/-2 ℃, preserving heat for 1h, introducing nitrogen, maintaining the temperature at 105+/-2 ℃ for 1h, introducing steam with the flow rate of 0.05m 3/h and introducing nitrogen with the flow rate of 0.05m 3/h, alternately operating for 2 times, introducing cooling water, and cooling to obtain DHA crude oil with the extraction rate of 93.8%.
The obtained DHA crude oil index is as follows: acid value 1.2, peroxide value 0.04, anisole 2.3, impurity content 0.2%, solvent residue 17ppm, phospholipid 68ppm.
Example 2
1. The dry cells of dinoflagellate are subjected to superfine grinding and wall breaking, the wall breaking rate reaches 99%, and the treatment capacity is 2 tons.
2. Hexane was added in an amount 8 times the dry cell mass, and mixed to form an extraction suspension.
3. Adding water with the quantity of 2 times of that of dry thalli into the extraction suspension, mixing for 0.5h, settling, wherein the settling temperature is 50 ℃, the settling pressure is 0.1Mpa, the settling time is 2h, and sucking the supernatant.
4. Desolventizing: and (3) desolventizing the supernatant fluid in the step (3) to the solvent content of 10% at 50 ℃ under the pressure of-0.08 Mpa, maintaining the pressure of-0.08 Mpa, introducing steam, maintaining the temperature within the range of 105+/-2 ℃, preserving heat for 1h, introducing nitrogen, maintaining the temperature within the range of 105+/-2 ℃ for 1h, introducing steam with the flow rate of 0.05m 3/h and introducing nitrogen with the flow rate of 0.05m 3/h, alternately operating for 2 times, and introducing cooling water for cooling to obtain DHA crude oil.
The obtained DHA crude oil index is as follows: acid value 1.4, peroxide value 0.2, anisole 4.8, impurity content 5%, solvent residue 100ppm, phospholipid 160ppm.
Example 3
1. The dry cells of dinoflagellate are subjected to superfine grinding and wall breaking, the wall breaking rate reaches 99%, and the treatment capacity is 2 tons.
2. Hexane was added in an amount 8 times the dry cell mass, and mixed to form an extraction suspension.
3. Adding water with the quantity of 0.5 times of the dry bacterial cells into the extraction suspension, mixing for 0.5h, then settling, wherein the settling temperature is 50 ℃, the settling pressure is 0.1Mpa, the settling time is 1h, and sucking the supernatant.
4. Sedimentation and separation are carried out again: adding 1 times of water into the supernatant of the step 3, mixing for 1h at 50 ℃ under the sedimentation pressure of 0.1Mpa, and sucking the supernatant after the sedimentation time is 4 h.
5. Desolventizing: and (3) desolventizing the supernatant obtained in the step (4) to the solvent content of 10% at 50 ℃ under the pressure of-0.08 Mpa, maintaining the pressure of-0.08 Mpa, introducing steam, maintaining the temperature at 105+/-2 ℃, preserving heat for 1h, introducing nitrogen, maintaining the temperature at 105+/-2 ℃ for 1h, introducing steam with the flow rate of 0.05m 3/h and introducing nitrogen with the flow rate of 0.05m 3/h, alternately operating for 2 times, and introducing cooling water for cooling to obtain DHA crude oil.
The obtained DHA crude oil index is as follows: acid value 1.6, peroxide value 0.4, anisole 4.0, impurity content 0.4%, solvent residue 50ppm, phospholipid 100ppm.
Example 4
1. The dry cells of dinoflagellate are subjected to superfine grinding and wall breaking, the wall breaking rate reaches 99%, and the treatment capacity is 2 tons.
2. Hexane was added in an amount 10 times the dry cell mass, and mixed to form an extraction suspension.
3. Adding water with the quantity of 1 time of dry thalli into the extraction suspension, mixing for 1 hour, settling, wherein the settling temperature is 45 ℃, the settling pressure is 0.2Mpa, the settling time is 0.5 hour, and sucking the supernatant.
4. The supernatant was concentrated until the oil content reached 20%, at which point the solid impurity content was about 3%.
5. Sedimentation and separation are carried out again: adding water with the solid impurity content of 1 time into the concentrated supernatant obtained in the step 4, mixing for 1h at 45 ℃ under the sedimentation pressure of 0.2Mpa, settling for 4h, and sucking the supernatant.
6. Desolventizing: and (3) desolventizing the supernatant obtained in the step (5) to the solvent content of 10% at 40 ℃ under the pressure of-0.08 Mpa, maintaining the pressure of-0.08 Mpa, introducing steam, maintaining the temperature at 105+/-2 ℃, preserving heat for 1h, introducing nitrogen, maintaining the temperature at 105+/-2 ℃ for 1h, introducing steam with the flow rate of 0.05m 3/h and introducing nitrogen with the flow rate of 0.05m 3/h, alternately operating for 3 times, introducing cooling water, and cooling to obtain DHA crude oil with the extraction rate of 93.0%.
The obtained DHA crude oil index is as follows: acid value 1.0, peroxide value 0.05, anisole 2.0, impurity content 0.3%, solvent residue 15ppm, phospholipid 60ppm.
Example 5
1. The schizochytrium limacinum dry thalli adopts superfine grinding to break the wall, the wall breaking rate reaches 99%, and the treatment capacity is 2 tons.
2. Hexane was added in an amount 8 times the dry cell mass, and mixed to form an extraction suspension.
3. Adding water with the quantity of 0.5 times of the dry bacterial cells into the extraction suspension, mixing for 0.5h, then settling, wherein the settling temperature is 50 ℃, the settling pressure is 0.1Mpa, the settling time is 1h, and sucking the supernatant.
4. The supernatant was concentrated until the oil content reached 20%, at which point the solid impurity content was about 3.5%.
5. Sedimentation and separation are carried out again: adding water with the solid impurity content of 0.8 times into the concentrated supernatant obtained in the step 4, mixing for 1h at 50 ℃ under the settling pressure of 0.1Mpa, settling for 4h, and sucking the supernatant.
6. Desolventizing: and (3) desolventizing the supernatant obtained in the step (5) to the solvent content of 10% at 45 ℃ under the pressure of-0.08 Mpa, maintaining the pressure of-0.08 Mpa, introducing steam, maintaining the temperature at 102+/-2 ℃, preserving heat for 1h, introducing nitrogen, maintaining the temperature at 102+/-2 ℃ for 1h, introducing steam with the flow rate of 0.05m 3/h and introducing nitrogen with the flow rate of 0.05m 3/h, alternately operating for 3 times, introducing cooling water, and cooling to obtain DHA crude oil with the extraction rate of 92.3%.
The obtained DHA crude oil index is as follows: acid value 1.1, peroxide value 0.02, anisole 2.7, impurity content 0.2%, solvent residue 15ppm, phospholipid 34ppm.
Comparative example 1
The extraction method of this comparative example is the same as that of example 1, except that: the dried dinoflagellate thalli are directly mixed with hexane with the quantity of 8 times of the dried dinoflagellate thalli without superfine grinding wall breaking, so as to form an extraction suspension. No grease was detected in the suspension.
Comparative example 2
The extraction method of the comparative example is different from that of example 1 in that the suspension is formed in step 2, and then water addition sedimentation is not performed, and it is found that bacterial residues cannot be naturally settled, oil and fat are difficult to separate, and subsequent steps cannot be performed.
Comparative example 3
The extraction method of this comparative example is different from that of example 1 in that step 3 does not employ hydration, a part of the sample is directly taken and centrifuged at high speed, the cells are separated by centrifugation for 10min under 10000r/min, and step 5 is also centrifuged again by the same method. And finally, desolventizing by adopting a centrifugal separation method to obtain crude oil, wherein the acid value is 1.5, the peroxide value is 0.1, the anisole content is 3.2, the impurity content is 0.5%, the solvent residue is 44ppm, and the phospholipid is 500ppm.
In the comparative example, the crude oil is separated by a centrifuge, so that the indexes such as impurity content and the like of the crude oil are not obviously superior to those of the embodiment 1 of the invention, and the phospholipid content cannot be effectively reduced by the centrifugation mode.
Comparative example 4
1. The dry cells of dinoflagellate are subjected to superfine grinding and wall breaking, the wall breaking rate reaches 99%, and the treatment capacity is 2 tons.
2. Hexane was added in an amount 8 times the dry cell mass, and mixed to form an extraction suspension.
3. Adding water with the quantity of 0.1 times of the dry bacterial body 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. Sedimentation and separation are carried out again: adding water with the solid impurity amount of 0.2 times into the concentrated supernatant obtained in the step 4, mixing for 1h at 50 ℃, settling for 4h, and sucking the supernatant.
6. Desolventizing: and (3) desolventizing the supernatant obtained in the step (5) to the solvent content of 10% at 50 ℃ under the pressure of-0.08 Mpa, maintaining the pressure of-0.08 Mpa, introducing steam, maintaining the temperature at 105+/-2 ℃, preserving heat for 1h, introducing nitrogen, maintaining the temperature at 105+/-2 ℃ for 1h, introducing steam with the flow rate of 0.05m 3/h and introducing nitrogen with the flow rate of 0.05m 3/h, alternately operating for 3 times, and introducing cooling water for cooling to obtain DHA crude oil.
The obtained DHA crude oil index is as follows: acid value 1.9, peroxide value 0.5, anisole 9, impurity content 12%, solvent residue 300ppm, phospholipid 230ppm.
Comparative example 5
The extraction method of the comparative example is different from that of example 5 in that the bacterial suspension is not hydrated after the step 2 is formed, and the bacterial residues are found to be unable to naturally settle, so that the grease is difficult to separate. After two separations by centrifugation in the method of comparative example 3, crude oil was obtained, which had an acid value of 1.5, a peroxide value of 0.2, an anisole of 3.8, a content of impurities of 0.4%, a solvent residue of 50ppm and a phospholipid of 350ppm. Likewise, centrifugation is not significantly advantageous over the present method, but the present method is less demanding in terms of equipment and more compatible with existing industrial production equipment.
In the prior art CN113684088a, a method for extracting crude oil with water is provided, which mainly comprises the steps of forming emulsion by using water as solvent in the extraction step, adjusting the pH to 9, stirring for 6 hours at 55 ℃, boiling at 95 ℃, and performing centrifugal separation on the two to obtain crude oil. Compared with the solvent-free direction, the crude oil obtained by the method can obtain crude oil with equivalent quality, the oil extraction rate is higher, the sedimentation method is simpler and more convenient in procedure compared with the demulsification-separation direction in the method, and the requirements of refined oil on phospholipid content can be met in the crude oil extraction process. The prior art CN113684088A also provides a method for extracting grease by adopting isopropanol, which mainly comprises the step of extracting grease by adopting isopropanol to the thalli subjected to dry wall breaking. However, this method does not mention a detailed hydrated cell separation step, but mainly uses a two-system centrifugation method. As a result of this method, the crude oil contained more phospholipids than 350ppm as in comparative example 3, and the oil extraction rate was inferior to that of the method of the present invention. The content of DHA in the grease obtained in the examples and comparative examples 3-5 provided by the invention is more than or equal to 40%, and meets the most application requirements.
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, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The oil extraction method is characterized by comprising the following steps of: after physically breaking the wall of the dry thalli, adding an extraction solvent to obtain a suspension, adding water to mix, and settling to obtain a supernatant; the water amount is 0.5-2 times of the dry thallus mass; the extraction solvent is one of hexane, ethyl acetate, isopropanol and n-hexane;
Concentrating the supernatant to obtain a concentrated solution, so that the crude oil content in the concentrated solution is 20% -40%, adding water into the concentrated solution, mixing for 0.5-2 h, settling, taking the supernatant, and desolventizing; the sedimentation time is not less than 0.5h, the sedimentation temperature is 45-50 ℃, and the sedimentation pressure is 0.1-0.2 Mpa;
the desolventizing step comprises the following steps: desolventizing at 40-50 ℃ until the solvent content is less than or equal to 10%, keeping the pressure at less than or equal to-0.08 Mpa, a) controlling the temperature within 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;
The steam inlet amount in the step a) is 0.02-0.1 m 3/h, and the nitrogen inlet amount is 0.02-0.1 m 3/h.
2. The method for extracting oil or fat according to claim 1, wherein the amount of water is 0.5 to 1 times the mass of the dry cell.
3. The method for extracting oil or fat according to claim 1 or 2, wherein the amount of the extraction solvent is 8 to 10 times the mass of the dry cells.
4. A fat or oil obtained by the fat or oil extraction method according to any one of claims 1 to 3.
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