CN109762658A - A kind of method of purification of refined fish oil - Google Patents
A kind of method of purification of refined fish oil Download PDFInfo
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- CN109762658A CN109762658A CN201910095838.6A CN201910095838A CN109762658A CN 109762658 A CN109762658 A CN 109762658A CN 201910095838 A CN201910095838 A CN 201910095838A CN 109762658 A CN109762658 A CN 109762658A
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Abstract
The invention discloses a kind of methods of purification of refined fish oil, it is related to fish oil purification technique field, crude fish oil is successively passed through to crude fish oil pretreatment, esterification step, dehydration and decolorization process, molecular distillation, absorption, it is dehydrated removing heavy-metal process, refining and distilling process prepares refined fish oil, use the peroxide value of the fish oil of GB5009.227 test preparation for 0.98moq/Kg, content using the EPA and DHA of GB5009.168 test is respectively 37.88% and 28.21%, higher than current normal level, the fish oil rate of recovery 97.1%, purity is greater than 90.03%, and whole process preparation method is simple.
Description
Technical field
The present invention relates to fish oil purification technique fields, particularly relate to a kind of method of purification of refined fish oil.
Background technique
With the improvement of living standards, people are also higher and higher to the attention rate of health, various health care products and nutriment
It is to come into being, fish oil is exactly the nutriment for being known as " human body gold oil ", also just because of this, the demand of fish oil is also increasingly
Greatly, the DHA in fish oil and EPA is substance needed for human brain development, and DHA and EPA content are also to measure fish oil nutritive value
Important indicator.
Refined fish oil contains the DHA and EPA of high-purity, is crude fish oil made of being refined as fish meal, by degumming, decoloration and
What the processes such as deodorization were prepared, inventor has found that the fish oil taken at present is mentioned when studying the method for purification of refined fish oil
There are the following problems for pure procedure, and (1) purification process is complex, and process is tedious；(2) rate of recovery of refined fish oil is lower；(3) it mentions
The purity of pure refined fish oil can not meet demand of the current people to fish oil purity.
Summary of the invention
In view of this, it is an object of the invention to propose a kind of method of purification of refined fish oil, to solve in the prior art
All or part of deficiency about refined fish oil purification.
Based on a kind of above-mentioned purpose method of purification of refined fish oil provided by the invention, the method includes following step
It is rapid:
1) crude fish oil pre-processes: crude fish oil being filtered, after dehydration by evaporation, free fatty acid is removed into distillation, obtains
Pre-process crude fish oil；
2) esterification step: will pretreatment crude fish oil and ethyl alcohol mix, catalyst is then added, and be heated to 92~98 DEG C into
Then esterised oil after reaction is washed, is dehydrated by row ester exchange reaction, obtain ethyl ester type fish oil；
3) molecular distillation, absorption: molecular distillation will be carried out after the preheating of ethyl ester type fish oil, obtained distillate is added to dense
In the ethanol solution of degree 90~98%, and urea is added, is heated to 68~76 DEG C of progress infinite reflux absorption, cools down after the completion of absorption
To 22~25 DEG C, separating liquid is dehydrated, the reaction of removing heavy-metal and de-oiling rouge, obtains degreasing oil by centrifuge separation；
4) refining and distilling: degreasing oil is subjected to vacuum molecular distillation purification & isolation, obtains refined fish oil.
In some optional embodiments, moisture≤1 ‰ of the pretreatment crude fish oil, acid value≤1mgKOH/g.
In some optional embodiments, the catalyst is the concentrated sulfuric acid of concentration 95~98%, and additive amount is 1.5~3%
.wt。
In some optional embodiments, dehydrating operations are that the esterised oil after washing adds 5 into dehydrating kettle in described (2)
~15%.wt carries out 100~110 DEG C of vacuum dehydrations of heating by the adsorbent that mass ratio is that the carclazyte of 1:1~5 and activated carbon mix,
Then it filters.
In some optional embodiments, the volume ratio of pretreatment crude fish oil and ethyl alcohol is 1:2~4.5 in described (2).
In some optional embodiments, the volume ratio of described (3) intermediate distillates and ethyl alcohol is 1:4~8, urea and distillate
Solid-liquid ratio be 3.5~4.5:1.
In some optional embodiments, the operation of dehydration, removing heavy-metal and the reaction of de-oiling rouge is as follows in described (3): will be through
The absorption oil for crossing absorption preparation is added dehydrating kettle, 100~110 DEG C of agitating and heating, is dried under vacuum state, add 3~
Then 12%.wt is filtered, then vacuum suck freezes by the adsorbent that mass ratio is that 1~6:1 carclazyte and activated carbon mix
Crystallization kettle, in kettle cool down -10~-12 DEG C crystallized, growing the grain, then filter filters pressing, obtain degreasing oil.
In some optional embodiments, the vacuum degree of vacuum molecular distillation is 0.01~0.03Mpa in described (3).
From the above it can be seen that a kind of method of purification of refined fish oil provided by the invention, crude fish oil is successively passed through thick
Fish oil pretreatment, esterification step, dehydration and decolorization process, molecular distillation, absorption, dehydration removing heavy-metal process, refining and distilling process
Refined fish oil is prepared, uses the peroxide value of the fish oil of GB5009.227 test preparation for 0.98moq/Kg, uses
The content of the EPA and DHA of GB5009.168 test are respectively 37.88% and 28.21%, are higher than current normal level, and fish oil returns
Yield 97.1%, purity is greater than 90.03%, and whole process preparation method is simple.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, to this hair
Bright further description.
Complex in order to solve (1) purification process in the prior art, process is tedious；(2) rate of recovery of refined fish oil compared with
It is low；(3) it is insufficient in whole or in part to can not meet demand of the current people to fish oil purity for the purity of the refined fish oil purified, this
A kind of method of purification for refined fish oil that inventive embodiments provide, the method include the following steps:
1) crude fish oil pre-processes: crude fish oil being filtered, after dehydration by evaporation, free fatty acid is removed into distillation, obtains
Pre-process crude fish oil；
2) esterification step: will pretreatment crude fish oil and ethyl alcohol mix, catalyst is then added, and be heated to 92~98 DEG C into
Then esterised oil after reaction is washed, is dehydrated by row ester exchange reaction, obtain ethyl ester type fish oil；
3) molecular distillation, absorption: molecular distillation will be carried out after the preheating of ethyl ester type fish oil, obtained distillate is added to dense
In the ethanol solution of degree 90~98%, and urea is added, is heated to 68~76 DEG C of progress infinite reflux absorption, cools down after the completion of absorption
To 22~25 DEG C, separating liquid is dehydrated, the reaction of removing heavy-metal and de-oiling rouge, obtains degreasing oil by centrifuge separation；
4) refining and distilling: degreasing oil is subjected to vacuum molecular distillation purification & isolation, obtains refined fish oil.
Passage capacity test data makees further a kind of method of purification of refined fish oil provided in an embodiment of the present invention
It illustrates.
A kind of method of purification for refined fish oil that one embodiment of the present invention provides, the method include the following steps:
1) crude fish oil pre-processes: crude fish oil being filtered, after thin film evaporator dehydration, removes and swims into short-distance distiller
It from fatty acid, is pre-processed into crossing, makes the control of crude fish oil moisture≤1 ‰, acid value≤1mgKOH/g, guarantee esterification work in next step
Sequence reaction, obtains pretreatment crude fish oil；
2) esterification step: by the ethyl alcohol of tank area, pre-processing crude fish oil, 1:3 squeezes into corresponding high-order meter respectively by volume
In measuring tank, then by ethyl alcohol, pre-processes crude fish oil and be added in reaction kettle, add the concentrated sulfuric acid of 2%.wt concentration 98%, and
92~98 DEG C of progress ester exchange reactions are heated to, water washing pan then is added in the esterised oil after reaction or butterfly centrifugal machine carries out
After washing, into dehydrating kettle, the adsorbent that 12%.wt is mixed by mass ratio for 1:3.5 carclazyte and activated carbon is added, is heated
100~110 DEG C of vacuum dehydrations, are then filtered, and obtain ethyl ester type fish oil；
3) molecular distillation, absorption: ethyl ester type fish oil addition preheating device is heated, filtered pre- hot oil enters and divides
Sub- distilling apparatus is decolourized, is deodorized, purification processes, and the temperature of distillation is 8~120 DEG C, by obtained distillate by with ethyl alcohol
Volume ratio be 1:5.5 ratio be added in the ethanol solution of concentration 95%, and be by the solid-liquid ratio of urea and distillate
Urea is added in 3.9:1, is all added in reaction kettle, dissolves by heating, and is heated to 68~76 DEG C of progress infinite reflux absorption, and absorption is completed
After be cooled to 22~25 DEG C, dehydrating kettle, agitating and heating 100~110 is added in the absorption oil by absorption preparation by centrifuge separation
DEG C, it is dried under vacuum state, adds the adsorbent that 9.4%.wt is mixed by mass ratio for 4.5:1 carclazyte and activated carbon,
Then be filtered, then vacuum suck freezing and crystallizing kettle, cool down -10~-12 DEG C in kettle crystallized, growing the grain, then mistake
Filtering pressure filter obtains degreasing oil；
4) refining and distilling: degreasing oil is subjected to vacuum molecular distillation purification & isolation in vacuum degree for 0.01~0.03Mpa, is obtained
Refined fish oil.Product 1.
Purity judgement is carried out according to SC/T 3503-2000 Fish oil standard of articles, through the purity for detecting refined fish oil
93.01%.
The present invention secondly embodiment with one embodiment of the present invention, the difference is that a kind of purification provided in an embodiment of the present invention
In the method for purification of fish oil:
(2) esterification step: ethyl alcohol, 1:2, the additive amount of the concentrated sulfuric acid are 1.5%.wt to pretreatment crude fish oil by volume, are inhaled
Attached dose: mass ratio 1:1 carclazyte and activated carbon mixture, additive amount 5%.wt；
(3) molecular distillation, absorption: the volume ratio of distillate and ethyl alcohol is 1:4, and the solid-liquid ratio of urea and distillate is 3.5:
1, adsorbent: mass ratio 1:1 carclazyte and activated carbon mixture, additive amount 3%.wt.Product 2.
Purity judgement is carried out according to SC/T 3503-2000 Fish oil standard of articles, through the purity for detecting refined fish oil
90.03%.
The present invention thirdly embodiment with one embodiment of the present invention, the difference is that a kind of purification provided in an embodiment of the present invention
In the method for purification of fish oil:
(2) esterification step: ethyl alcohol, 1:4.5, the additive amount of the concentrated sulfuric acid are 3%.wt to pretreatment crude fish oil by volume, are inhaled
Attached dose: mass ratio 1:5 carclazyte and activated carbon mixture, additive amount 15%.wt；
(3) molecular distillation, absorption: the volume ratio of distillate and ethyl alcohol is 1:8, and the solid-liquid ratio of urea and distillate is 4.5:
1, adsorbent: mass ratio 6:1 carclazyte and activated carbon mixture, additive amount 12%.wt.Product 3.
Purity judgement is carried out according to SC/T 3503-2000 Fish oil standard of articles, through the purity for detecting refined fish oil
92.11%.
Its of the invention four embodiment with the present invention secondly embodiment, unlike a kind of purification provided in an embodiment of the present invention
In the method for purification of fish oil:
(3) molecular distillation, absorption: the volume ratio of distillate and ethyl alcohol is 1:8, and the solid-liquid ratio of urea and distillate is 4.5:
1, adsorbent: mass ratio 6:1 carclazyte and activated carbon mixture, additive amount 12%.wt.Product 4.
Purity judgement is carried out according to SC/T 3503-2000 Fish oil standard of articles, through the purity for detecting refined fish oil
92.54%.
Its of the invention five embodiment with the present invention thirdly embodiment, unlike a kind of purification provided in an embodiment of the present invention
In the method for purification of fish oil:
(3) molecular distillation, absorption: the volume ratio of distillate and ethyl alcohol is 1:4, and the solid-liquid ratio of urea and distillate is 3.5:
1, adsorbent: mass ratio 1:1 carclazyte and activated carbon mixture, additive amount 3%.wt.Product 5.
Purity judgement is carried out according to SC/T 3503-2000 Fish oil standard of articles, through the purity for detecting refined fish oil
92.67%.
Its six embodiment of the invention is with one embodiment of the present invention, the difference is that a kind of purification provided in an embodiment of the present invention
In the method for purification of fish oil:
(2) esterification step: ethyl alcohol, 1:2, the additive amount of the concentrated sulfuric acid are 1.5%.wt to pretreatment crude fish oil by volume, are inhaled
Attached dose: mass ratio 1:1 carclazyte and activated carbon mixture, additive amount 5%.wt, product 6.
Purity judgement is carried out according to SC/T 3503-2000 Fish oil standard of articles, through the purity for detecting refined fish oil
91.85%.
Its seven embodiment of the invention is with one embodiment of the present invention, the difference is that a kind of purification provided in an embodiment of the present invention
In the method for purification of fish oil:
(2) esterification step: ethyl alcohol, 1:4.5, the additive amount of the concentrated sulfuric acid are 3%.wt to pretreatment crude fish oil by volume, are inhaled
Attached dose: mass ratio 1:5 carclazyte and activated carbon mixture, additive amount 15%.wt, product 7.
Purity judgement is carried out according to SC/T 3503-2000 Fish oil standard of articles, through the purity for detecting refined fish oil
92.78%.
Product 1~7 is taken, carries out performance measurement according to the measurement standard of table 1, it is as shown in the table for test result.
The measurement standard and measurement result of 1 refined fish oil of table
The processing of esterification step and molecular distillation, absorption is to influence the committed step of refined fish oil, can by the data of table 1
To find out, by the comparison of product 1,6 and 7, esterification optimal processes are ethyl alcohol, pre-process crude fish oil 1:3 by volume, dense
The additive amount of sulfuric acid is 2%.wt, and adsorbent: mass ratio 1:3.5 carclazyte and activated carbon mixture, additive amount 12%.wt pass through
The comparison of product 1,4,5,6 and 7, molecular distillation, absorption: the volume ratio of distillate and ethyl alcohol is 1:5.5, urea and distillate
Solid-liquid ratio is 3.9:1, adsorbent: mass ratio 4.5:1 carclazyte and activated carbon mixture, additive amount 9.4%.wt.
Then the measurement of the rate of recovery and purity, the rate of recovery calculation formula of refined fish oil are carried out to product 1~7 are as follows:In formula: m1For fish oil quality (g) after purification, m2For crude fish oil quality (g).Final recovery rate
=fish oil recovery rate × fish oil the rate of recovery.Test result is shown in Table 2.
The rate of recovery of 2 refined fish oil of table and final recovery rate
| Product 1 | Product 2 | Product 3 | Product 4 | Product 5 | Product 6 | Product 7 | The prior art | |
| The rate of recovery/% | 97.1 | 82.35 | 88.57 | 85.56 | 91.12 | 84.56 | 94.56 | 80.45 |
| Final recovery rate/% | 48.56 | 32.15 | 43.56 | 38.44 | 45.12 | 37.45 | 46.88 | 30.78 |
Crude fish oil is successively passed through to crude fish oil pretreatment, esterification step, dehydration and decolorization process, molecular distillation, absorption, dehydration
Removing heavy-metal process, refining and distilling process prepare refined fish oil, using the peroxidating of the fish oil of GB5009.227 test preparation
Value is 0.98moq/Kg, and the content using the EPA and DHA of GB5009.168 test is respectively 37.88% and 28.21%, is higher than
Normal level at present, the fish oil rate of recovery 97.1%, purity is greater than 90.03%, and whole process preparation method is simple.
It should be understood by those ordinary skilled in the art that: the discussion of any of the above embodiment is exemplary only, not
It is intended to imply that the scope of the present disclosure (including claim) is limited to these examples；Under thinking of the invention, above embodiments
Or can also be combined between the technical characteristic in different embodiments, step can be realized with random order, and be existed such as
Many other variations of the upper different aspect of the invention, for simplicity, they are not provided in details.
The embodiment of the present invention be intended to cover fall into all such replacements within the broad range of appended claims,
Modifications and variations.Therefore, all within the spirits and principles of the present invention, any omission, modification, equivalent replacement, the improvement made
Deng should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of method of purification of refined fish oil, which is characterized in that the method includes the following steps:
1) crude fish oil pre-processes: crude fish oil being filtered, after dehydration by evaporation, free fatty acid is removed into distillation, obtains pre- place
Manage crude fish oil；
2) esterification step: pretreatment crude fish oil and ethyl alcohol are mixed, catalyst is then added, and be heated to 92~98 DEG C of progress esters
Then esterised oil after reaction is washed, is dehydrated by exchange reaction, obtain ethyl ester type fish oil；
3) molecular distillation, absorption: molecular distillation will be carried out after the preheating of ethyl ester type fish oil, obtained distillate is added to concentration 90
In~98% ethanol solution, and urea is added, is heated to 68~76 DEG C of progress infinite reflux absorption, 22 are cooled to after the completion of absorption
~25 DEG C, separating liquid is dehydrated, the reaction of removing heavy-metal and de-oiling rouge, obtains degreasing oil by centrifuge separation；
4) refining and distilling: degreasing oil is subjected to vacuum molecular distillation purification & isolation, obtains refined fish oil.
2. the method for purification of refined fish oil according to claim 1, which is characterized in that the moisture of the pretreatment crude fish oil
≤ 1 ‰, acid value≤1mgKOH/g.
3. the method for purification of refined fish oil according to claim 1, which is characterized in that the catalyst be concentration 95~
98% concentrated sulfuric acid, additive amount are 1.5~3%.wt.
4. the method for purification of refined fish oil according to claim 1, which is characterized in that in (2) dehydrating operations be by
Esterised oil after washing, into dehydrating kettle, the absorption for adding 5~15%.wt to be mixed by mass ratio for the carclazyte of 1:1~5 and activated carbon
Agent carries out 100~110 DEG C of vacuum dehydrations of heating, then filters.
5. the method for purification of refined fish oil according to claim 1, which is characterized in that pre-process crude fish oil in (2)
Volume ratio with ethyl alcohol is 1:2~4.5.
6. the method for purification of refined fish oil according to claim 1, which is characterized in that (3) intermediate distillates and ethyl alcohol
Volume ratio be 1:4~8, the solid-liquid ratio of urea and distillate is 3.5~4.5:1.
7. the method for purification of refined fish oil according to claim 1, which is characterized in that dehydration, removing heavy-metal in (3)
The operation reacted with de-oiling rouge is as follows: the absorption by absorption preparation is oily, addition dehydrating kettle, and 100~110 DEG C of agitating and heating,
It is dried under vacuum state, adds the adsorbent that 3~12%.wt is mixed by mass ratio for 1~6:1 carclazyte and activated carbon,
Then be filtered, then vacuum suck freezing and crystallizing kettle, cool down -10~-12 DEG C in kettle crystallized, growing the grain, then mistake
Filtering pressure filter obtains degreasing oil.
8. the method for purification of any refined fish oil according to claim 1~7, which is characterized in that vacuum point in (3)
The vacuum degree of son distillation is 0.01~0.03Mpa.
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| CN115154486A (en) * | 2022-07-07 | 2022-10-11 | 四川欣美加生物医药有限公司 | Method for reducing oligomer content in fish oil |
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Application publication date: 20190517 |