CN104232300A - Method for refining mixed oil of microalgae DHA oil - Google Patents
Method for refining mixed oil of microalgae DHA oil Download PDFInfo
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Abstract
The invention relates to a technology for refining microbial oil, and particularly relates to a method for refining mixed oil of microalgae DHA oil. Leached microalgae DHA crude oil is taken as a raw material; before complete desolvation is carried out, firstly, degumming and deacidification are carried out; then desolvation is carried out; and finally decolorization and deodorization are carried out on oil according to the conventional method, thus obtaining refined microalgae DHA oil. The indexes of the microalgae DHA oil prepared by the method for refining the mixed oil of the microalgae DHA oil completely reach the index requirements of the national standard GB-26400. According to the method disclosed by the invention, the product quality and the refining yield (higher than 80%) of the microalgae DHA oil are improved, meanwhile, the oil content of nigre is reduced, the washing process is omitted, energy consumption is reduced, and industrial application of the mixed oil refining technology in the microbial oil is facilitated.
Description
Technical field
The present invention relates to the refining techniques of microbial oil, be specifically related to a kind of miscella refining method of micro-algae DHA grease.
Technical background
Currently mainly contain four class refinery practices, i.e. physical refining, continuous alkali-refining, interval type refining and miscella refining.Compared with other refining techniquess, miscella refining technique relies on processing ease, refining yield is high, energy consumption is low, product oil quality is good, environmental pollution is little and take off the advantages such as equipment damage is little to steaming, receive the concern (Zhou Renkai, 2012) of research institute and entrepreneur.
Since nineteen fifty-three, C.Cavangh proposed miscella refining first, this technology is in US and European country widespread use (Hui HY, 2001).The miscella refining technology of external representative at present mainly contains the conventional hybrid oil refinement technique of the U.S. and this art designing's skill of Belgian enlightening etc.From eighties of last century seventies, China has started the research to miscella refining technology, the main refining art at mixed cotton seed oil (number of patent application is CN200610140624 and CN201310067411), rice bran mixing oil (number of patent application is CN200810019740) and Semen Ricini oil (being coated with state, 2001) at present.
In the refining techniques field of microbial oil, miscella refining is not all had to apply both at home and abroad.The miscella refining of micro-algae DHA grease refers in extraction oil producing process, breaks through the method for common process " mixing oil-precipitation-come unstuck-depickling-decolouring-deodorization ", adopts the method for " depickling of first being come unstuck by mixing oil, then precipitation-decolouring-deodorization " to refine.
Summary of the invention
Object of the present invention provides a kind of miscella refining technology of micro-algae DHA grease, adopts miscella refining technology to refine micro-algae DHA grease and belongs to pioneering research.
Technical scheme of the present invention: directly carried out by the mixing oil of micro-algae DHA grease leached coming unstuck, depickling, carries out carrying out precipitation treatment again after centrifugation, finally carries out conventional decolouring, deodorization obtains processed oil.Central inventive research of the present invention is the process of " micro-algae DHA mixing oil-come unstuck-depickling-precipitation ", and decolouring and deodorization adopt common process.Accompanying drawing 1 is shown in its technical process.
The inventive method is with the micro-algae DHA mixing oil leached for raw material, and concrete technology step is:
(1) micro-algae DHA mixing oil pre-treatment: what obtain from leacher may also have a small amount of algae dregs of rice or other impurity, adopts the method for filtering to control below 0.2% by the solid impurity of micro-algae DHA mixing oil;
(2) micro-algae DHA mixing oil comes unstuck: by mixing oil heating temperatures to 45 ~ 60 DEG C, add appropriate acid solution under rapid stirring, adds rear evenly slow stirring 30 ~ 40min.Containing peptized impurities such as phosphatide in mixing oil, affect subsequent machining technology.Utilize the wetting ability of peptized impurities, in mixing oil, add appropriate acid solution, non-hydratable phospholipid is converted into hydrated phospholipid, the metal ion in grease can be removed simultaneously, add the oxidative stability of grease;
(3) micro-algae DHA mixing oil depickling (alkali refining): control temperature, at 45 ~ 60 DEG C, calculates according to mixing crude oil acid value and adds proper amount of edible sodium hydroxide, fully after mixing, evenly slowly stir 30 ~ 40min, obtain the mixture of oil and soap,
(4) oil is separated with soap: control at 50 ~ 55 DEG C by the mixture temperature of oil and soap, after stirring, and centrifugation mixing oil and soap stock;
(5) micro-algae DHA mixing oil precipitation: mixing oil is heated to 60 ~ 65 DEG C, carries out precipitation under the condition of vacuum bar degree 0.06 ~ 0.09Mpa;
(6) decolouring and deodorization: carry out successively according to a conventional method decolouring and deodorization.
In step (3) described in the inventive method, the acid solution added in the degumming technology of micro-algae DHA mixing oil to be the mass concentration of mixing oil oil heavy 0.1% ~ 1.0% be 35% ~ 55% food grade aqueous citric acid solution, or 0.1% ~ 0.5% mass concentration is the food grade phosphoric acid solution of 75% ~ 85%.
In step described in the inventive method (4), the concentration of lye added in the deacidifying process of micro-algae DHA mixing oil is 5% ~ 20%, and excess alkali quantity is that oil is heavy by 0.1% ~ 1.0%.According to the acid value of micro-algae DHA degummed oil, the theoretical amount of interpolation presses formula M
naOH=M
0* AV*40/56.11*10
-3calculate.In formula, M
naOHfor theoretical caustic dosage, M
0for degummed oil weight, AV is the acid value of degummed oil.
Beneficial effect of the present invention:
(1) effectively prevent the coking that traditional technology micro-algae DHA mixing oil causes the peptization material such as solidification, phosphatide of the heat-sensitive substances such as pigment in desolvation process, significantly improve product color, be beneficial to the carrying out of subsequent technique, so cost-saving.
(2) micro-algae DHA mix oil viscosity and proportion lower, not only reduce energy consumption, and improve alkali refining effect, acid value reduces, and then improves quality product.
(3) micro-algae DHA mixing oil is not easy emulsification, and decrease oil-containing in soap, improve refining yield, through repetition test, refining yield reaches more than 80%, higher than the refining yield (70% ~ 75%) of traditional technology.
(4) in micro-algae DHA miscella refining process, have be easy to oil with being separated of soap, save water washing process, the peptized impurities such as phosphatide are easy to the advantages such as sedimentation.
To sum up, the refinery practice of micro-algae DHA mixing oil is simple, there is not washing waste water problem, environmental protection and energy saving, refining consumption is low, and refining yield is high, and quality product is high, refining for micro-algae DHA grease creates the method for refining of new high efficiency, for the application of miscella refining technology in Rrefinement of Fungal Oil field lays the foundation.
Accompanying drawing explanation
The miscella refining technical process of the micro-algae DHA grease of Fig. 1.
Embodiment
The miscella refining method of embodiment 1 micro-algae DHA grease refines micro-algae DHA grease
The miscella refining concrete grammar that this experiment adopts is as follows:
(1) micro-algae DHA mixing oil pre-treatment: adopt the solid impurity of filter method mixing oil to control below 0.2%;
(2) micro-algae DHA mixing oil comes unstuck: by mixing oil heating temperatures to 45 DEG C, and the mass concentration adding 0.4% under rapid stirring is the food grade aqueous citric acid solution of 55%, and evenly slowly stirs 30min;
(3) micro-algae DHA mixing oil depickling (alkali refining): control temperature is at 45 DEG C, and the concentration of lye added is 12%, excess alkali quantity is that oil is heavy by 0.2%.After abundant mixing, evenly slowly stir 40min, obtain the mixture of oil and soap;
(4) oil is separated with soap: control below 50 DEG C by the mixture temperature of oil and soap, centrifugation mixing oil and soap stock;
(5) micro-algae DHA mixing oil precipitation: mixing oil is heated to 60 ~ 65 DEG C, carries out precipitation under the condition of vacuum bar degree 0.06 ~ 0.09Mpa;
(6) decolouring and deodorization: carry out successively according to a conventional method decolouring and deodorization.
Adopt this miscella refining method and traditional method of refining to obtain micro-algae DHA grease with the micro-algae DHA crude oil with a collection of leaching for raw material (acid value of this crude oil is 10.6mg KOH/g oil, phospholipids content 2.0%) simultaneously.The mass concentration of this experiment scouring processes employing 0.4% is the food grade aqueous citric acid solution of 55%.This experiment carries out index test (as shown in table 1) to refining micro-algae DHA grease, and each index of acid value, peroxide value, moisture, DHA content is all better than traditional method of refining.In addition, after decolorization terminates, from outward appearance, micro-algae DHA that miscella refining method obtains decolours cast of oil close to processed oil color, become golden yellow, and the bleached oil color that traditional method of refining obtains is scarlet.As can be seen here, micro-algae DHA miscella refining method is a kind of effective micro-algae DHA grease method of refining.
Micro-algae DHA grease index that table 1 miscella refining method is obtained
The miscella refining method of embodiment 2 micro-algae DHA grease refines micro-algae DHA grease
The miscella refining concrete grammar that this experiment adopts is as follows:
(1) micro-algae DHA mixing oil pre-treatment: adopt the solid impurity of filter method mixing oil to control below 0.2%;
(2) micro-algae DHA mixing oil comes unstuck: by mixing oil heating temperatures to 50 DEG C, and the mass concentration adding 0.2% under rapid stirring is the food grade phosphate aqueous solution of 75%, and evenly slowly stirs 20min;
(4) micro-algae DHA mixing oil depickling (alkali refining): control temperature is at 50 DEG C, and the concentration of lye added is 12%, excess alkali quantity is that oil is heavy by 0.2%.After abundant mixing, evenly slowly stir 30min, obtain the mixture of oil and soap;
(5) oil is separated with soap: control below 50 DEG C by the mixture temperature of oil and soap, centrifugation mixing oil and soap stock;
(6) micro-algae DHA mixing oil precipitation: mixing oil is heated to 60 ~ 65 DEG C, carries out precipitation under the condition of vacuum bar degree 0.06 ~ 0.09Mpa;
(7) decolouring and deodorization: carry out successively according to a conventional method decolouring and deodorization.
Adopt this miscella refining method and traditional method of refining to obtain micro-algae DHA grease with the micro-algae DHA crude oil with a collection of leaching for raw material (acid value of this crude oil is 9.8mg KOH/g oil, phospholipids content 2.2%) simultaneously.This experiment scouring processes adopts the food grade phosphate aqueous solution that the mass concentration adding 0.2% is 75%.This experiment carries out index test (as shown in table 2) to refining micro-algae DHA grease, and each index of acid value, peroxide value, moisture, DHA content is all better than traditional method of refining, and reaches the index request of GB26400-2011 completely.
Micro-algae DHA grease index that table 2 miscella refining method is obtained
To sum up, the refining yield of the miscella refining method of the inventive method-micro-algae DHA grease and quality product all reach the requirement of GB26400.The inventive method is a kind of effectively brand-new method of refining, for the Application Areas of miscella refining technology at microbial oil lays the first stone.
Be more than in conjunction with specific embodiments son the present invention is done further describe.The technician of the industry should understand, and the present invention is not restricted to the described embodiments, and without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, and these changes and improvements are all in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (4)
1. the miscella refining method of a micro-algae DHA grease, it is characterized in that: before the mixing micro-algae DHA crude oil evaporation precipitation leached, first carry out coming unstuck and depickling, then carry out carrying out precipitation treatment, last decolouring and the deodorization process conventionally carrying out grease, obtained refining micro-algae DHA grease.
2. the miscella refining method of a kind of micro-algae DHA grease according to claim 1, is characterized in that: described processing step comprises:
(1) micro-algae DHA mixing oil pre-treatment: adopt the method for filtering to control below 0.2% by the solid impurity of micro-algae DHA mixing oil;
(2) micro-algae DHA mixing oil comes unstuck: by mixing oil heating temperatures to 40 ~ 60 DEG C, add appropriate acid solution under rapid stirring, adds rear evenly slow stirring 30 ~ 40min;
(3) micro-algae DHA mixing oil depickling: control temperature, at 40 ~ 60 DEG C, calculates according to mixing crude oil acid value and adds proper amount of edible sodium hydroxide, fully after mixing, evenly slowly stir 30 ~ 40min, obtain the mixture of oil and soap;
(4) micro-algae DHA mixing oil is separated: control at 40 ~ 65 DEG C by the mixture temperature of oil and soap, after stirring, and centrifugation mixing oil and soap stock;
(5) micro-algae DHA mixing oil precipitation: mixing oil is heated to 60 ~ 65 DEG C, carries out precipitation under the condition of vacuum bar degree 0.06 ~ 0.09Mpa;
(6) decolouring and deodorization: carry out successively according to a conventional method decolouring and deodorization.
3. the miscella refining method of a kind of micro-algae DHA grease described by claim 1 or 2, it is characterized in that: in described step (3), to add acid solution be the mass concentration of mixing oil oil heavy 0.1% ~ 1.0% be 35% ~ 55% food grade aqueous citric acid solution, or 0.1% ~ 0.5% mass concentration is the food grade phosphoric acid solution of 75% ~ 85%.
4. the miscella refining method of a kind of micro-algae DHA grease described by claim 1 or 2, is characterized in that: in described step (4), and the concentration of lye added is 5% ~ 20%, and excess alkali quantity is that oil is heavy by 0.1% ~ 1.0%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107760440A (en) * | 2017-12-07 | 2018-03-06 | 河西学院 | A kind of method of purification of microalgae grease |
| CN108753458A (en) * | 2018-08-03 | 2018-11-06 | 梁云 | Improve the refinery practice of microbial grease stability and safety |
| CN108753457A (en) * | 2018-08-03 | 2018-11-06 | 梁云 | The method for improving microbial grease stability and safety |
| CN112300864A (en) * | 2020-10-22 | 2021-02-02 | 安徽天凯生物科技有限公司 | Method for improving stability of docosahexaenoic acid |
| CN114343021A (en) * | 2021-12-22 | 2022-04-15 | 嘉必优生物技术（武汉）股份有限公司 | Application of DHA (docosahexaenoic acid) algae oil with improved fishy smell in edible oil |
| CN115109648A (en) * | 2022-06-09 | 2022-09-27 | 嘉必优生物技术（武汉）股份有限公司 | Desolventizing method of microbial oil and microbial oil |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107760440A (en) * | 2017-12-07 | 2018-03-06 | 河西学院 | A kind of method of purification of microalgae grease |
| CN108753458A (en) * | 2018-08-03 | 2018-11-06 | 梁云 | Improve the refinery practice of microbial grease stability and safety |
| CN108753457A (en) * | 2018-08-03 | 2018-11-06 | 梁云 | The method for improving microbial grease stability and safety |
| CN112300864A (en) * | 2020-10-22 | 2021-02-02 | 安徽天凯生物科技有限公司 | Method for improving stability of docosahexaenoic acid |
| CN114343021A (en) * | 2021-12-22 | 2022-04-15 | 嘉必优生物技术（武汉）股份有限公司 | Application of DHA (docosahexaenoic acid) algae oil with improved fishy smell in edible oil |
| CN114343021B (en) * | 2021-12-22 | 2024-04-05 | 嘉必优生物技术（武汉）股份有限公司 | Application of DHA algae oil for improving fishy smell in edible oil |
| CN115109648A (en) * | 2022-06-09 | 2022-09-27 | 嘉必优生物技术（武汉）股份有限公司 | Desolventizing method of microbial oil and microbial oil |
| CN115109648B (en) * | 2022-06-09 | 2024-04-19 | 嘉必优生物技术（武汉）股份有限公司 | Desolventizing method of microbial oil and microbial oil |
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