CN108949337A - A kind of extracting method of microorganism crude oil - Google Patents
A kind of extracting method of microorganism crude oil Download PDFInfo
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- CN108949337A CN108949337A CN201810887142.2A CN201810887142A CN108949337A CN 108949337 A CN108949337 A CN 108949337A CN 201810887142 A CN201810887142 A CN 201810887142A CN 108949337 A CN108949337 A CN 108949337A
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- CN
- China
- Prior art keywords
- crude oil
- microorganism
- bacterium solution
- extracting method
- phase centrifuge
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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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
- C11B1/02—Pretreatment
- C11B1/025—Pretreatment by enzymes or microorganisms, living or dead
-
- 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
-
- 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
-
- 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
- C11B3/16—Refining fats or fatty oils by mechanical means
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- 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)
- Biochemistry (AREA)
- Mechanical Engineering (AREA)
- Fats And Perfumes (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention belongs to microbial oil processing technique fields, are related to the extractive technique of crude oil, specially a kind of extracting method of microorganism crude oil.The extracting method of microorganism crude oil of the present invention are as follows: fermentation liquid is first passed through into two-phase centrifuge, remove most of moisture, microbial cells are collected, cellulase is used later, cracks cell wall, enzyme-deactivating, again plus then alkali protease, broken cell film are centrifuged by three-phase centrifuge, microorganism crude oil rouge is collected, crude oil rouge obtains microorganism crude oil after hydration process.Crude oil can be put in storage storage according to production needs or be refined into essential oil.No solvent residue of the present invention is digested using two steps, grease extraction efficiency is made to be up to 95% or more.Extraction process conditional is mild, low for equipment requirements, high-efficient, is suitble to industrialized production.It is avoided that the destruction of grease during the extraction process.The quality for improving crude oil extends the Storage period of crude oil.
Description
Technical field
The invention belongs to microbial oil processing technique fields, are related to the extractive technique of crude oil, specially a kind of microorganism
The extracting method of crude oil.
Background technique
The extraction of grease mainly has physical squeezing method and solvent extraction at present.Physical squeezing method is the traditional side of comparison
Method is not thorough the disadvantage is that mentioning oil, will cause the waste of grease.Although solvent extraction grease extracts more thoroughly, can make
Risk in terms of having dissolvent residual at the grease extracted.Then supercritical extract is derived on the basis of solvent extraction
With subcritical abstraction method, the method very good solution dissolvent residual, the disadvantage is that very high to equipment requirement, need once to put into compared with
More funds.
Microbial oil is the third-largest edible oil and fat source after vegetable fat, animal fat.Due to oleaginous microorganism
Most of is unicellular organism, and extraction of the extraction of its grease compared with plant and animal grease is made to have more better choices, but
It is the method that existing microbial oil is extracted mostly is the deriving method of physical squeezing method or solvent extraction, principle is essentially identical.
It is after collecting thallus using physical squeezing method such as the method that a kind of dry method of ZL 201310235046.7 extracts microbial oil
Obtain crude oil.The method for extracting microbial oil as CN104479862A is a kind of, ZL 201410797861.7 is a kind of to extract micro- life
The method of object grease, a kind of extracting method of the microbial oil of ZL 201410761605.2, ZL 201310497556.1 are a kind of
The method for extracting microbial oil, a kind of method of the efficient extraction of microbial oil of ZL 201210287434.5,
CN103421595A it is a kind of extract microbial oil method, a kind of extraction of the microbial oil of ZL 201110228151.9 and
Method of refining, a kind of microbial oil extraction method of ZL 201010593183.4, a kind of microbial oil of ZL201010527702.7
The extracting method of rouge, 200810138499.7 separation and extraction method of microbial oil of ZL etc. are carried out using solvent extraction
The extraction of microorganism crude oil, only the means of microorganism broken wall are different.In addition it is mentioned there are also the method similar with solvent extraction
Microorganism crude oil is taken, only the technique comparatively safe using the solvent extracted, extracts micro- life as ZL 201110376750.5 is a kind of
The method of object grease, is extracted with grease, and 200910060589.3 microbial oil of ZL and its short-link alcohol fatty acid ester extract
Method is extracted with short-link alcohol fatty acid ester, and the supercritical carbon dioxide extracting of 03139630.5 microbial oil of ZL mentions for another example
Method is taken, extracts (the high requirements on the equipment) with liquid carbon dioxide.
In addition to this, there are also the methods different from mentioned microorganism grease extraction process, mainly lean on film by crude fat
It is separated from microorganism shell-broken liquid.As CN107523417A extracts the method and CN107723319A mono- of microbial oil
The extracting method of kind microbial oil.Membrane filter method extracts microorganism crude fat, extremely stringent to the pore size requirement of film, and
And certain pressure is needed, promote passing through for fat, it is relatively low that this has resulted in extraction efficiency, higher cost.
In order to change the extraction process defect of existing microorganism crude oil, meet the market demand, spy invents this microorganism hair
The extracting method of oil.
Summary of the invention
The purpose of the present invention is to provide a kind of completely new microorganism crude oil extracting methods, to make up the prior art not
Foot.
To achieve the goals above, technical scheme is as follows:
A kind of extracting method of microorganism crude oil, characterized in that the following steps are included:
A, after the completion of microbial fermentation, open two-phase centrifuge, when revolving speed reaches >=7000rpm when, by fermentation liquid with 6
~10m3The flow of/h is by two-phase centrifuge, and clear liquid above directly exhausts after centrifugation, collects the magma where following thallus
Body；
B, after the bacterium solution after the concentration of a) step being warming up to 30~60 DEG C, the pH value of bacterium solution is adjusted to 4.0 with pH adjusting agent
~5.5, the cellulase of 1000~50000U is then added according to per kilogram dry mycelium weight, stirring digests 0.5~3h, later
The temperature of bacterium solution is risen to 70~90 DEG C, stirs and keep the temperature 0.4~1h, go out cellulase；
C, its pH value is adjusted to 5~7 with pH adjusting agent again by above-mentioned enzymatic hydrolysis bacterium solution, temperature is adjusted to 30~55 DEG C, according to every
The protease of 1000~50000U is added in kilogram dry mycelium weight, stirs and digests 2~8h, bacterium solution is warming up to 80~95 later
DEG C, 0.4~1h is kept, go out protease；
D, open three-phase centrifuge, when revolving speed reaches >=8000rpm when, by the bacterium solution in step c after enzymatic hydrolysis with 1~
3m3The flow of/h collects the microorganism crude oil rouge on upper layer by three-phase centrifuge；
E, the aqueous citric acid solution of its weight 1% is added in the microorganism crude oil rouge that d) step obtains, later by micro- life
The temperature of object crude oil rouge rises to 80~90 DEG C, stirs 0.5~1h, is centrifuged later, obtains microorganism crude oil.
Preferably, step b) and c) in pH adjusting agent be hydrochloric acid, sulfuric acid, acetic acid, any one in citric acid.
Preferably, the protease in step c) is any one in neutral proteinase, papain or bromelain
Kind.
Preferably, the aqueous citric acid solution in step e) is the aqueous citric acid solution that concentration is 40%.
Compared with prior art, the present invention having the advantage that
1, no solvent residue of the present invention is digested using two steps, grease extraction efficiency is made to be up to 95% or more.
2, the present invention is mild in entire crude oil extraction process conditional, low for equipment requirements, high-efficient, is suitble to industry metaplasia
It produces.
3, present invention pH value during entire crude oil extracts and stores maintains always 7 hereinafter, being avoided that grease is mentioning
Destruction during taking.
4, crude fat of the invention uses centrifugal separation, can make the polyphenoils quality guarantee of more microorganisms endogenous
It stays in crude oil, improves the quality of crude oil, extend the Storage period of crude oil.
Specific embodiment
Many details are elaborated in following description to facilitate a thorough understanding of the present invention, still the present invention is not by following
The limitation of disclosed specific embodiment.
Embodiment 1
A kind of extracting method of microorganism crude oil, comprising the following steps:
A, after the completion of microbial fermentation, open two-phase centrifuge, when revolving speed reaches 7000rpm, by fermentation liquid with
6m3The flow of/h is by two-phase centrifuge, and clear liquid above directly exhausts after centrifugation, collects the thick liquid where following thallus
2.4 tons (dry biomass 50%, total ester amount account for the 50% of dry biomass)；
B, after the bacterium solution after the concentration of a) step being warming up to 30 DEG C, the pH value of bacterium solution is adjusted to 4.0 with hydrochloric acid, is then added
The cellulase of 1200000 U, stirring enzymatic hydrolysis 3h, rises to 70 DEG C for the temperature of bacterium solution later, stirs and keep the temperature 1h, go out cellulase；
C, its pH value is adjusted to 5 with hydrochloric acid again by above-mentioned enzymatic hydrolysis bacterium solution, temperature is adjusted to 30 DEG C, and the pineapple egg of 1,200,000 U is added
White enzyme stirs and digests 8h, and bacterium solution is warming up to 80 DEG C later, keeps 1h, go out protease；
D, three-phase centrifuge is opened, when revolving speed reaches 8000rpm, by the bacterium solution in step c after enzymatic hydrolysis with 2m3/h
Flow by three-phase centrifuge, collect the microorganism crude oil rouge 710kg on upper layer；
E, it is added 7.1kg in the microorganism crude oil rouge that d) step obtains, the aqueous citric acid solution that concentration is 40%, later
The temperature of microorganism crude oil rouge is risen to 80 DEG C, 1h is stirred, is centrifuged later, obtains microorganism crude oil 680kg (total ester amount
83.8%), total ester yield 95%.
Embodiment 2
A kind of extracting method of microorganism crude oil, comprising the following steps:
A, after the completion of microbial fermentation, open two-phase centrifuge, when revolving speed reaches 8000rpm, by fermentation liquid with
9m3The flow of/h is by two-phase centrifuge, and clear liquid above directly exhausts after centrifugation, collects the thick liquid where following thallus
2.4 tons (dry biomass 50%, total ester amount account for the 50% of dry biomass)；
B, after the bacterium solution after the concentration of a) step being warming up to 50 DEG C, the pH value of bacterium solution is adjusted to 4.8 with sulfuric acid, is then added
The cellulase of 60000000 U, stirring enzymatic hydrolysis 0.5h, rises to 90 DEG C for the temperature of bacterium solution later, stirs and keep the temperature 1h, go out cellulose
Enzyme；
C, its pH value is adjusted to 6.5 with sulfuric acid again by above-mentioned enzymatic hydrolysis bacterium solution, temperature is adjusted to 50 DEG C, is added in 60,000,000 U
Property protease, stir and digest 2h, bacterium solution is warming up to 95 DEG C later, keep 0.4h, go out neutral proteinase；
D, three-phase centrifuge is opened, when revolving speed reaches 8000rpm, by the bacterium solution in step c after enzymatic hydrolysis with 4m3/h
Flow by three-phase centrifuge, collect the microorganism crude oil rouge 750kg on upper layer；
E, 7.5kg is added in the microorganism crude oil rouge that d) step obtains, the aqueous citric acid solution that concentration is 40%, later
The temperature of microorganism crude oil rouge is risen to 90 DEG C, 1h is stirred, is centrifuged later, obtains microorganism crude oil 690kg (total ester amount
85.2%), total ester yield 98%.
Embodiment 3
A kind of extracting method of microorganism crude oil, comprising the following steps:
A, after the completion of microbial fermentation, open two-phase centrifuge, when revolving speed reaches 75000rpm, by fermentation liquid with
12m3The flow of/h is by two-phase centrifuge, and clear liquid above directly exhausts after centrifugation, collects the thick liquid where following thallus
2.4 tons (dry biomass 50%, total ester amount account for the 50% of dry biomass)；
B, after the bacterium solution after the concentration of a) step being warming up to 60 DEG C, the pH value of bacterium solution is adjusted to 5.5 with acetic acid, is then added
The cellulase of 36000000 U, stirring enzymatic hydrolysis 2h, rises to 80 DEG C for the temperature of bacterium solution later, stirs and keep the temperature 0.7h, go out cellulose
Enzyme；
C, its pH value is adjusted to 7 with citric acid again by above-mentioned enzymatic hydrolysis bacterium solution, temperature is adjusted to 55 DEG C, and the wood of 36,000,000 U is added
Melon protease stirs and digests 2h, and bacterium solution is warming up to 95 DEG C later, keeps 0.4h, go out neutral proteinase；
D, three-phase centrifuge is opened, when revolving speed reaches 7500rpm, by the bacterium solution in step c after enzymatic hydrolysis with 6m3/h
Flow by three-phase centrifuge, collect the microorganism crude oil rouge 730kg on upper layer；
E, 7.3kg is added in the microorganism crude oil rouge that d) step obtains, the aqueous citric acid solution that concentration is 40%, later
The temperature of microorganism crude oil rouge is risen to 85 DEG C, 0.7h is stirred, is centrifuged later, obtains microorganism crude oil 670kg (total ester amount
86%), total ester yield 98%.
Claims (4)
1. a kind of extracting method of microorganism crude oil, characterized in that the following steps are included:
A, after the completion of microbial fermentation, open two-phase centrifuge, when revolving speed reaches >=7000rpm when, by fermentation liquid with 6~
10m3The flow of/h is by two-phase centrifuge, and clear liquid above directly exhausts after centrifugation, collects the thick liquid where following thallus；
B, after the bacterium solution after the concentration of a) step being warming up to 30~60 DEG C, the pH value of bacterium solution is adjusted to 4.0 with pH adjusting agent~
5.5, the cellulase of 1000~50000U is then added according to per kilogram dry mycelium weight, stirring 0.5~3h of enzymatic hydrolysis later will
The temperature of bacterium solution rises to 70~90 DEG C, stirs and keep the temperature 0.4~1h, and go out cellulase；
C, its pH value is adjusted to 5~7 with pH adjusting agent again by above-mentioned enzymatic hydrolysis bacterium solution, temperature is adjusted to 30~55 DEG C, according to per kilogram
The protease of 1000~50000U is added in dry mycelium weight, stirs and digests 2~8h, bacterium solution is warming up to 80~95 DEG C later,
0.4~1h is kept, go out protease；
D, open three-phase centrifuge, when revolving speed reaches >=8000rpm when, by the bacterium solution in step c after enzymatic hydrolysis with 1~3m3/h
Flow by three-phase centrifuge, collect the microorganism crude oil rouge on upper layer；
E, the aqueous citric acid solution of its weight 1% is added in the microorganism crude oil rouge that d) step obtains, it is later that microorganism is thick
The temperature of grease rises to 80~90 DEG C, stirs 0.5~1h, is centrifuged later, obtains microorganism crude oil.
2. a kind of extracting method of microorganism crude oil according to claim 1, it is characterized in that: step b) and c) in pH adjust
Agent is hydrochloric acid, sulfuric acid, acetic acid, any one in citric acid.
3. the extracting method of a kind of microorganism crude oil according to claim 1, it is characterized in that: the protease in step c) is
Any one in neutral proteinase, papain or bromelain.
4. the extracting method of a kind of microorganism crude oil according to claim 1, it is characterized in that: the citric acid water in step e)
Solution is the aqueous citric acid solution that concentration is 40%.
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| CN201810887142.2A CN108949337A (en) | 2018-08-06 | 2018-08-06 | A kind of extracting method of microorganism crude oil |
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| CN201810887142.2A CN108949337A (en) | 2018-08-06 | 2018-08-06 | A kind of extracting method of microorganism crude oil |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112500918A (en) * | 2020-10-29 | 2021-03-16 | 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 |
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| CN103173273A (en) * | 2011-12-21 | 2013-06-26 | 新奥科技发展有限公司 | Microalgae grease extraction method |
| US20150176042A1 (en) * | 2013-12-20 | 2015-06-25 | MARA Renewables Corporation | Methods of recovering oil from microorganisms |
| CN106811285A (en) * | 2017-02-23 | 2017-06-09 | 湖北福星生物科技有限公司 | A kind of method that physics extracts DHA grease in zymotic fluid from DHA |
| CN107099561A (en) * | 2017-07-04 | 2017-08-29 | 南京工业大学 | A kind of Solventless Extraction Process containing docosahexaenoic acid grease |
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2018
- 2018-08-06 CN CN201810887142.2A patent/CN108949337A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103173273A (en) * | 2011-12-21 | 2013-06-26 | 新奥科技发展有限公司 | Microalgae grease extraction method |
| US20150176042A1 (en) * | 2013-12-20 | 2015-06-25 | MARA Renewables Corporation | Methods of recovering oil from microorganisms |
| CN106811285A (en) * | 2017-02-23 | 2017-06-09 | 湖北福星生物科技有限公司 | A kind of method that physics extracts DHA grease in zymotic fluid from DHA |
| CN107099561A (en) * | 2017-07-04 | 2017-08-29 | 南京工业大学 | A kind of Solventless Extraction Process containing docosahexaenoic acid grease |
Non-Patent Citations (1)
| Title |
|---|
| 罗质: "《油脂精炼工艺学》", 30 June 2016, 中国轻工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112500918A (en) * | 2020-10-29 | 2021-03-16 | 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 |
| CN112500918B (en) * | 2020-10-29 | 2022-06-10 | 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 |
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