CN103351946B - Preparation method of moderately processed ARA (Arachidonic acid) microalgae grease - Google Patents

Preparation method of moderately processed ARA (Arachidonic acid) microalgae grease Download PDF

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CN103351946B
CN103351946B CN201310254172.7A CN201310254172A CN103351946B CN 103351946 B CN103351946 B CN 103351946B CN 201310254172 A CN201310254172 A CN 201310254172A CN 103351946 B CN103351946 B CN 103351946B
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oil
ara
microalgae grease
refining
grease
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CN103351946A (en
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白长军
宁超美
白红超
戚桂斌
初跃峰
李玉玲
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QINGDAO HAIZHIYUAN LIFE TECHNOLOGY CO., LTD.
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QINGDAO HAIZHIYUAN LIFE TECHNOLOGY Co Ltd
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Abstract

The invention provides a preparation method of moderately processed ARA (Arachidonic acid) microalgae grease. The method comprises the following steps of: first, degumming to remove colloid and impurities in microalgae grease; after degumming, refining alkali and neutralizing at low temperature to remove free acids; then, decoloring in a low temperature vacuum condition to remove residual soap, phosphorus, pigments and the like; and finally, deodorizing through combination of a packed tower and a plate tower, and thermosensitively decoloring to remove fatty acid and small molecular stink substances, wherein the generation amount of trans-fatty acids can be reduced, the energy is saved and the consumption is reduced, and the quality of grease products is improved. Due to the adoption of the method, the ARA microalgae grease with low content of trans-fatty acids (less than 1.0%) can be prepared.

Description

A kind of preparation method of ARA microalgae grease of appropriateness processing
Technical field
The present invention relates to fats and Oils Refining Technology field, specifically relate to a kind of preparation method of ARA microalgae grease of appropriateness processing.
Technical background
Along with the development of food scientific technology, various functional grease constantly enters the life of the people, plays significant role to the nutrition and health improving the people.ARA microalgae grease, as new resource food, simultaneously as functional grease, is rich in ARA, has hypermnesis and thinking ability, improve intelligence and promote the effects such as brain development.
For producing qualified ARA microalgae grease and ensureing its shelf-lives, need to come unstuck to ARA microalgae grease crude oil, depickling, the process such as deodorization, with except the colloid, free acid, heavy metal ion etc. in deoiling, but the phenomenon of overprocessing is there is in current grease precision work field, not only cause the waste of resource and the energy, but also the natural loss being present in useful micro-nutrients in grease can be caused, also can generate accompaniment human body being unfavorable for HUMAN HEALTH, as trans fatty acid.
The present invention by coming unstuck in the ARA microalgae grease course of processing, depickling, the optimizing research of the operation machined parameters such as deodorization and practice, can on the basis ensureing oil quality and safety, reduce the generation of trans fatty acid in the course of processing, realize the appropriateness processing of ARA microalgae grease.
Summary of the invention
Technical purpose of the present invention is to provide a kind of preparation method of ARA microalgae grease of appropriateness processing, its when alkali-refining deacidification temperature compared with low (35-45 DEG C), caustic dosage compared with little, discoloring agent addition is few (4-8kg/T oil), deodorization temperature low (being no more than 230 DEG C), deodorization time short (being no more than 45 minutes), the ARA microalgae grease product content of trans fatty acids adopting working method of the present invention to obtain is less than or equal to 1.0% of weight concentration, content of trans fatty acids is low, and product quality is high.
For reaching above-mentioned technical purpose, the technical solution used in the present invention is:
A preparation method for the ARA microalgae grease of appropriateness processing, comprises the following steps:
(1) come unstuck: add citric acid to ARA microalgae grease crude oil, make the non-hydratable phospholipid in crude oil be converted into hydrated phospholipid, then add alkali lye and remove colloid as flocculation agent, the oil after coming unstuck obtains degummed oil and oil foot through centrifugal treating;
(2) alkali refining neutralization: above-mentioned degummed oil to add in alkali lye and free fatty acids in excessive citric acid and oil at low temperatures, obtains neutralization oil through centrifugal treating;
(3) decolour: in above-mentioned neutralization oil, add discoloring agent, decolour at certain temperature and vacuum degree condition after stirring;
(4) deodorization: by bleached oil through packing tower and tray column, deodorization under the effect of dry steam air lift.
Above-mentioned working method, with the trans fatty acid in product for index, can optimize and revise technique and parameter (temperature, time, auxiliary material addition) further.
According to optimal enforcement modes more of the present invention, working method of the present invention wherein step (1) is preferably carried out at 50-75 DEG C; Citric acid is mass concentration is 20-30%; Alkali lye mass concentration is 2.0-3.0%.
Wherein step (2) is preferably carried out at 35-45 DEG C; Alkali lye mass concentration is 5.0-9.0%.
Wherein step (3) preferably 85-100 DEG C, carry out under vacuum tightness-0.08 ~-0.09Mpa; Discoloring agent (discoloring agent is gac and atlapulgite mixture, and quality of activated carbon is than being 1-100%) addition is 4-8kg/T; Bleaching time 15-30min;
Wherein step (4) by bleached oil after deaerator deoxygenation, through entering packing tower with deodorizing tower discharging deodorised oil heat exchange to 160-180 DEG C, with high pressure steam or other heating medium for heating to 200-230 DEG C, 0.3% open steam air lift 5-10min, carries out air lift depickling, then tray column is pumped into, with high pressure steam or other heating medium for heating to 200-230 DEG C, 0.6% open steam air lift 25-35min, carries out temperature-sensitive decolouring, finally oil cooling is carried out essence filter after 30-45 DEG C, obtain refining oil.
Appropriate preparation for processing provided by the invention, most preferred process comprises the following steps:
(1) come unstuck: DHA crude oil is warmed up to 70-75 DEG C, adding concentration according to the content of stock oil non-hydratable phospholipid is the citric acid of 20-30%, at souring tank reaction 25-40min, add the alkali lye flocculation of 2.0-3.0%, add the hot soft water of the heavy 1.0-2.0% of oil simultaneously, in hydration tank, react 45-60min, be warming up to 80-90 DEG C of centrifugation and obtain oil foot and degummed oil, dry degummed oil removes moisture and residual molten;
(2) alkali refining neutralization: degummed oil oil temperature is down to 35-45 DEG C, then adding concentration is that the alkaline reaction 50-65min of 5.0-9.0% carries out alkali-refining deacidification; Be warming up to 85 DEG C of centrifugations, and wash by the soft water that the 5-8% that oil is heavy adds 85-92 DEG C, centrifugation, must neutralize oil;
(3) decolour: neutralization oil is carried out drying at 90-100 DEG C, then (discoloring agent is gac and atlapulgite mixture to re-add about 4-8kg/T oil discoloring agent mixing according to oil, quality of activated carbon is than being 1-100%), under vacuum tightness-0.08 ~-0.09Mpa condition, decolouring 20-30min, filter discoloring agent, obtain bleached oil;
(4) deodorization: by bleached oil at 130 DEG C, under the condition of vacuum tightness-0.08 ~-0.09Mpa, through deaerator deoxygenation; Then packing tower is entered with deodorizing tower discharging deodorised oil heat exchange to 160-180 DEG C, with high pressure steam or other heating medium for heating to 200-230 DEG C, 0.3% open steam air lift 5-10min, carry out air lift depickling, then pump into tray column, with high pressure steam or other heating medium for heating to 200-230 DEG C, 0.6% open steam air lift 25-35min, carry out temperature-sensitive decolouring, finally oil cooling is carried out essence filter after 30-45 DEG C, obtain refining oil.
Through above-mentioned preferably after, working method of the present invention can obtain the ARA microalgae grease refined product that content of trans fatty acids is 0.2-1.0%.
Index determining foundation:
The mensuration of trans fatty acid: with reference to the mensuration of GB/T221100-2008 Trans-fatty Acids in Foods, vapor-phase chromatography.
The present invention is by the research of a kind of ARA microalgae grease preparation method and practice, especially by coming unstuck, alkali refining neutralization, decolouring, the optimizing and revising of the refining procedure such as deodorization, high-boiling-point impurity in removal ARA microalgae greases as far as possible many under the prerequisite ensureing quality product, achieve low-temperature short-time deodorization, thus form the method for a kind of ARA microalgae grease appropriateness processing.By this technique, refining is carried out to ARA microalgae grease, the functional ingredient in ARA microalgae grease can be retained to greatest extent, reduce harmful content of trans fatty acids, improve quality and the quality of ARA microalgae grease, energy consumption and enterprise's production cost can be reduced simultaneously.
Embodiment:
For further illustrating the present invention, illustrate with the following Examples:
Embodiment 1:
ARA microalgae grease crude oil is warmed up to 70 DEG C through interchanger, refuel heavy 0.3% concentration be the citric acid of 28%, at souring tank reaction 30min, add 2.0% alkali lye flocculation, refuel heavy 1.8% hot soft water, in hydration tank, react 50min, be warming up to 85 DEG C of centrifugation oil foots and degummed oil, dry degummed oil removes moisture and residual molten.
Degummed oil oil temperature is down to 40 DEG C, then add concentration be 6.5% alkaline reaction 50-65min carry out alkali-refining deacidification; Be warming up to 85 DEG C of centrifugations, and wash by 7.0% soft water adding 90 DEG C that oil is heavy, centrifugation, must neutralize oil;
By in alkali refining and after ARA microalgae grease carry out drying at 100 DEG C, then mix with discoloring agent that (discoloring agent is gac and atlapulgite mixture, the mass ratio of gac is 40%), discoloring agent addition is 4.5kg/T oil, under vacuum tightness-0.09Mpa condition, decolouring 22min, filters carclazyte, obtains bleached oil.
By bleached oil at 130 DEG C, through deaerator deoxygenation, 170 DEG C are heated to through interchanger, enter packing tower, under the condition of vacuum tightness-0.087Mpa, with high pressure steam heating to 210 DEG C, enter packing tower, air lift depickling, 0.3% (steam consumption with elaeometer) open steam air lift 10min, then packing tower is pumped into, with high pressure steam heating to 210 DEG C, 0.6% (with the steam consumption of elaeometer, namely steam consumption is 0.6% of weight of oil) open steam air lift 25min, carry out temperature-sensitive decolouring, through interchanger by oil cooling to 45 DEG C after carry out essence filter, obtain refining oil.
Detect refining oil index, result is as follows: content of trans fatty acids: 0.42%.
Embodiment 2
ARA microalgae grease crude oil is warmed up to 75 DEG C through interchanger, refuel heavy 0.3% concentration be the citric acid of 30%, at souring tank reaction 25min, add 2.2% alkali lye flocculation, refuel heavy 1.0% hot soft water, in hydration tank, react 45min, be warming up to 88 DEG C of centrifugation oil foots and degummed oil, dry degummed oil removes moisture and residual molten.
Degummed oil oil temperature is down to 40 DEG C, then add concentration be 6.0% alkaline reaction 58min carry out alkali-refining deacidification; Be warming up to 85 DEG C of centrifugations, and wash by 6.0% soft water adding 90 DEG C that oil is heavy, centrifugation, must neutralize oil;
By in alkali refining and after ARA microalgae grease carry out drying at 100 DEG C, then mix with discoloring agent that (discoloring agent is the white scholar's mixture of gac and activity, the mass ratio of gac is 30%), discoloring agent addition is 6.0kg/T oil, under vacuum tightness-0.09Mpa condition, decolouring 20min, filters carclazyte, obtains bleached oil.
By bleached oil at 130 DEG C, through deaerator deoxygenation, 170 DEG C are heated to through interchanger, enter packing tower, under the condition of vacuum tightness-0.087Mpa, with high pressure steam heating to 220 DEG C, enter packing tower, air lift depickling, 0.3% (steam consumption with elaeometer) open steam air lift 10min, then packing tower is pumped into, with high pressure steam heating to 220 DEG C, 0.6% (with the steam consumption of elaeometer, namely steam consumption is 0.6% of weight of oil) open steam air lift 25min, carry out temperature-sensitive decolouring, through interchanger by oil cooling to 45 DEG C after carry out essence filter, obtain refining oil.
Detect refining oil index, result is as follows: content of trans fatty acids: 0.56%.
Embodiment 3
ARA microalgae grease crude oil is warmed up to 75 DEG C through interchanger, refuel heavy 0.3% concentration be the citric acid of 25%, at souring tank reaction 25min, add 2.0% alkali lye flocculation, refuel heavy 2.0% hot soft water, in hydration tank, react 45min, be warming up to 88 DEG C of centrifugation oil foots and degummed oil, dry degummed oil removes moisture and residual molten.
Degummed oil oil temperature is down to 40 DEG C, then add concentration be 6.0% alkaline reaction 50-65min carry out alkali-refining deacidification; Be warming up to 85 DEG C of centrifugations, and wash by 6.5% soft water adding 90 DEG C that oil is heavy, centrifugation, must neutralize oil;
By in alkali refining and after ARA microalgae grease carry out drying at 100 DEG C, then mix with discoloring agent that (discoloring agent is gac and atlapulgite mixture, the mass ratio of gac is 50%), discoloring agent addition is 5.0kg/T oil, under vacuum tightness-0.09Mpa condition, decolouring 20min, filters carclazyte, obtains bleached oil.
By bleached oil at 130 DEG C, through deaerator deoxygenation, 170 DEG C are heated to through interchanger, enter packing tower, under the condition of vacuum tightness-0.087Mpa, with high pressure steam heating to 230 DEG C, enter packing tower, air lift depickling, 0.3% (steam consumption with elaeometer) open steam air lift 10min, then packing tower is pumped into, with high pressure steam heating to 230 DEG C, 0.6% (with the steam consumption of elaeometer, namely steam consumption is 0.6% of weight of oil) open steam air lift 25min, carry out temperature-sensitive decolouring, through interchanger by oil cooling to 45 DEG C after carry out essence filter, obtain refining oil.
Detect refining oil index, result is as follows: content of trans fatty acids: 0.69%.

Claims (2)

1. a preparation method for the ARA microalgae grease of appropriateness processing, is characterized in that: comprise the following steps:
(1) come unstuck: ARA microalgae grease crude oil is warmed up to 55-60 DEG C, adding concentration according to the content of stock oil non-hydratable phospholipid is the citric acid of 20-25%, at souring tank reaction 25-40min, add the alkali lye flocculation of 2.0-3.0%, add the hot soft water of the heavy 1.0-2.0% of oil simultaneously, in hydration tank, react 45-60min, be warming up to 80-90 DEG C of centrifugation and obtain oil foot and degummed oil, dry degummed oil removes moisture and residual molten;
(2) alkali refining neutralization: degummed oil oil temperature is down to 30-40 DEG C, then adding concentration is that the alkaline reaction 50-65min of 5.0-7.0% carries out alkali-refining deacidification; Be warming up to 85 DEG C of centrifugations, and wash by the soft water that the 5-8% that oil is heavy adds 88-92 DEG C, centrifugation, must neutralize oil;
(3) decolour: neutralization oil is carried out drying at 90-100 DEG C, then re-add the discoloring agent mixing about 4-8kg/T oil according to oil, described discoloring agent is the mixture of gac and atlapulgite, and wherein quality of activated carbon is than being 1-90%; Under vacuum tightness-0.08 ~-0.09Mpa condition, decolouring 20-30min, filters discoloring agent, obtains bleached oil;
(4) deodorization: by bleached oil at 130 DEG C, under the condition of vacuum tightness-0.08 ~-0.09Mpa, through deaerator deoxygenation; Then packing tower is entered with deodorizing tower discharging deodorised oil heat exchange to 165-180 DEG C, with high pressure steam or other heating medium for heating to 215-230 DEG C, 0.3% open steam air lift 5-10min, carry out air lift depickling, then pump into tray column, with high pressure steam or other heating medium for heating to 215-230 DEG C, 0.6% open steam air lift 25-35min, carry out temperature-sensitive decolouring, finally oil cooling is carried out essence filter after 30-45 DEG C, obtain refining oil.
2. the ARA microalgae grease that obtains of preparation method according to claim 1, is characterized in that: content of trans fatty acids≤1.0% in described microalgae grease.
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CN104263509A (en) * 2014-08-21 2015-01-07 青岛海智源生命科技有限公司 DHA micro-algal oil degumming method
JP6226089B2 (en) * 2015-04-27 2017-11-08 不二製油株式会社 Method for producing long-chain polyunsaturated fatty acid-containing oil

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