CN105907456B - A kind of purification processing method of fish oil - Google Patents
A kind of purification processing method of fish oil Download PDFInfo
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- CN105907456B CN105907456B CN201610294092.8A CN201610294092A CN105907456B CN 105907456 B CN105907456 B CN 105907456B CN 201610294092 A CN201610294092 A CN 201610294092A CN 105907456 B CN105907456 B CN 105907456B
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- enzyme
- fish
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- 235000021323 fish oil Nutrition 0.000 title claims abstract description 76
- 238000003672 processing method Methods 0.000 title claims abstract description 20
- 238000000746 purification Methods 0.000 title claims description 10
- 102000004190 Enzymes Human genes 0.000 claims abstract description 67
- 108090000790 Enzymes Proteins 0.000 claims abstract description 67
- 239000007788 liquid Substances 0.000 claims abstract description 64
- 235000019476 oil-water mixture Nutrition 0.000 claims abstract description 40
- 230000008878 coupling Effects 0.000 claims abstract description 32
- 238000010168 coupling process Methods 0.000 claims abstract description 32
- 238000005859 coupling reaction Methods 0.000 claims abstract description 32
- 239000006260 foam Substances 0.000 claims abstract description 29
- 241000251468 Actinopterygii Species 0.000 claims abstract description 13
- 238000004140 cleaning Methods 0.000 claims abstract description 12
- 230000007071 enzymatic hydrolysis Effects 0.000 claims abstract description 12
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 claims abstract description 12
- 239000012535 impurity Substances 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000002893 slag Substances 0.000 claims abstract description 7
- 210000001835 viscera Anatomy 0.000 claims abstract description 7
- 230000008030 elimination Effects 0.000 claims abstract description 6
- 238000003379 elimination reaction Methods 0.000 claims abstract description 6
- 229940088598 enzyme Drugs 0.000 claims description 63
- 238000002156 mixing Methods 0.000 claims description 52
- 239000002245 particle Substances 0.000 claims description 36
- 239000002131 composite material Substances 0.000 claims description 32
- 229920001661 Chitosan Polymers 0.000 claims description 28
- 239000000725 suspension Substances 0.000 claims description 28
- 239000004964 aerogel Substances 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 20
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000002360 preparation method Methods 0.000 claims description 17
- 239000004365 Protease Substances 0.000 claims description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- 108090000526 Papain Proteins 0.000 claims description 11
- 235000019834 papain Nutrition 0.000 claims description 11
- 229940055729 papain Drugs 0.000 claims description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 229940056319 ferrosoferric oxide Drugs 0.000 claims description 10
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- 238000006073 displacement reaction Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 230000010355 oscillation Effects 0.000 claims description 8
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 6
- 239000004113 Sepiolite Substances 0.000 claims description 6
- 101000693530 Staphylococcus aureus Staphylokinase Proteins 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 238000007598 dipping method Methods 0.000 claims description 6
- 239000000839 emulsion Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 229910052624 sepiolite Inorganic materials 0.000 claims description 6
- 235000019355 sepiolite Nutrition 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 101100203596 Caenorhabditis elegans sol-1 gene Proteins 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 230000032683 aging Effects 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 5
- 239000000908 ammonium hydroxide Substances 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 5
- 239000004519 grease Substances 0.000 claims description 5
- 230000007062 hydrolysis Effects 0.000 claims description 5
- 238000006460 hydrolysis reaction Methods 0.000 claims description 5
- 238000011068 loading method Methods 0.000 claims description 5
- 239000005011 phenolic resin Substances 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000009423 ventilation Methods 0.000 claims description 5
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 4
- 230000008961 swelling Effects 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 210000000496 pancreas Anatomy 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 23
- 230000008569 process Effects 0.000 abstract description 10
- 238000011084 recovery Methods 0.000 abstract description 7
- 238000000605 extraction Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 235000013332 fish product Nutrition 0.000 abstract description 2
- 239000008279 sol Substances 0.000 description 8
- 238000000926 separation method Methods 0.000 description 7
- 235000019198 oils Nutrition 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000002781 deodorant agent Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000003995 emulsifying agent Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 235000020995 raw meat Nutrition 0.000 description 4
- 235000019733 Fish meal Nutrition 0.000 description 3
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 210000000170 cell membrane Anatomy 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000004467 fishmeal Substances 0.000 description 3
- 102000004169 proteins and genes Human genes 0.000 description 3
- 108090000623 proteins and genes Proteins 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 108091005804 Peptidases Proteins 0.000 description 2
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 description 2
- 206010042674 Swelling Diseases 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000009849 deactivation Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002255 enzymatic effect Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 235000019419 proteases Nutrition 0.000 description 2
- 210000000697 sensory organ Anatomy 0.000 description 2
- 206010008132 Cerebral thrombosis Diseases 0.000 description 1
- 201000001429 Intracranial Thrombosis Diseases 0.000 description 1
- 108010009736 Protein Hydrolysates Proteins 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000008258 liquid foam Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- -1 matter Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 239000007764 o/w emulsion Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000003531 protein hydrolysate Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 230000010148 water-pollination Effects 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
- C11B1/02—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
- 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
-
- 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
- C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
-
- 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
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Biochemistry (AREA)
- Mechanical Engineering (AREA)
- Immobilizing And Processing Of Enzymes And Microorganisms (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The present invention relates to fish product manufacture fields, disclose a kind of exquisite processing method of fish oil, comprising: a, carry out cleaning impurity elimination to fish internal organ, smash to pieces, blank is made;B, blank is added in the enzymolysis liquid containing immobilization magnetic coupling enzyme and is digested, immobilization magnetic coupling enzyme is recycled with magnet after enzymatic hydrolysis;C, to enzymolysis liquid filtering and removing slag, layering, isolated upper layer fish oil and lower layer's oil-water mixture are then allowed to stand;D, oil-water mixture is transferred in foam fraction factor column, is ventilated to the bottom of foam fraction factor column, oil-water mixture upper layer generates froth bed, and froth bed is separated with liquid in time;E, oil-water mixture is centrifuged, obtains upper layer fish oil;F, the upper layer fish oil for obtaining step c and step e mixes, and obtains fish oil.For the present invention for the processing method simple process of fish oil, extraction efficiency and recovery rate are high, and the fish oil purity is high that processing obtains, no fishy smell, color are pure.
Description
Technical field
The present invention relates to the exquisite processing methods of fish product manufacture field more particularly to a kind of fish oil.
Background technique
Fish oil is one of important composition ingredient of fish, and fish oil has rich in a variety of unsaturated fatty acids such as EPA and DHA
Blood pressure lowering eliminates fatigue, prevention cerebral thrombosis, improves the functions such as memory.Therefore fish oil is widely used in food, medical treatment, feed
The fields such as industry.
The preparation method of fish oil is main at present are as follows: and 1, raw material is put into boiling water carries out boiling, then by upper layer floating
Fish oil is extracted by centrifugation or by organic solvent.The fish oil purity extracted by the above method is not high, easily by water, albumen
The impurity such as matter, colloid substance are brought into, need to carry out further Refining, are operated extremely complex.2, raw material is put into enzymolysis liquid
In digested, upper layer fish oil is taken after enzymatic hydrolysis, then decolourized to fish oil, deodorant, removal of impurities processing.
Such as application No. is 201410468003.8 Chinese patent, to disclose a kind of decoloration of fish meal processing byproduct fish oil de-
The method of raw meat decolourizes to low value fish oil using diatomite, can preferably remove fish meal processing byproduct fish oil color;Using ferment
Female powder carries out the deodorant of fish meal processing byproduct fish oil, is successfully realized the removing of fish oil fishy smell.
Such as application No. is 200710031626.9 Chinese patents to disclose a kind of enzymatic isolation method extraction fish processing fent
The technology of fish oil, method and step are pre-treatment: after the cleaning of fish processing fent, being blended;Protease hydrolytic: in use
Property the double enzymes of protease and papain hydrolyze simultaneously;Water-oil separating: hydrolyzate removes slag through centrifugal filtration, filtrate through centrifuge into
Row water-oil separating obtains fish oil and protein hydrolysate;Pyloric fat acid: fish oil obtains purification fish after degumming, depickling, decoloration and deodorization
Oil.
Above two method has been all made of second method to prepare fish oil, and the purity that fish oil is made is pure compared with first method
Du Genggao, but not ideal enough for the recovery rate of fish oil, and need to carry out subsequent decoloration, deodorant, removal of impurities processing, technique compared with
Be it is cumbersome, influence production efficiency.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides a kind of exquisite processing methods of fish oil.The present invention is for fish
The processing method simple process of oil, extraction efficiency and recovery rate are high, and the fish oil purity is high that processing obtains, no fishy smell, color
It is pure.
The specific technical proposal of the invention is: a kind of exquisite processing method of fish oil, sequentially includes the following steps:
A, cleaning impurity elimination is carried out to fish internal organ, smashed to pieces, blank is made.
B, the blank is added in the enzymolysis liquid containing immobilization magnetic coupling enzyme and is digested, wherein blank, enzyme
The mass ratio for solving liquid is 1:2.5-3.5, and the enzyme content in enzymolysis liquid is 0.05-0.2%, and hydrolysis temperature is 40-50 DEG C, when enzymatic hydrolysis
Between 2-6h, enzymolysis liquid pH control in 6.5-7;The immobilization magnetic coupling enzyme is recycled with magnet after enzymatic hydrolysis.
Blank is digested using immobilization magnetic coupling enzyme, since enzyme is supported on carrier in immobilization magnetic coupling enzyme
On, the fixed protection of carrier is received, is not easy to be protected from environmental and reduce enzymatic activity, therefore enzymolysis efficiency is higher;Another party
It face, only need to be using magnetic field by immobilization magnetic coupling after the completion of enzymatic hydrolysis containing magnetic nuclear particle in immobilization magnetic coupling enzyme
Enzyme is assembled, and is then separated and recovered, not only convenient separation, but also immobilization magnetic coupling enzyme can reuse, drop
Low cost.It needs to carry out high temperature enzyme deactivation to enzymolysis liquid after enzymatic hydrolysis in conventional method, and for fish oil, high-temperature process
In will lead to fish oil denaturation cracking, cause effective component to be lost, nutritive value decline.The method of the present invention is not necessarily to high temperature enzyme deactivation
Journey can utmostly retain fish oil effective component.
In addition, the carrier in immobilization magnetic coupling enzyme of the invention, has complicated three-dimensional net structure, have very high
Voidage, therefore adsorptivity is very strong, not only good to enzyme immobilizatio effect, but also while enzymatic hydrolysis, can be in fish
Raw meat substance (amine substance) and pigment in dirty are adsorbed, so that fish oil is decolourized, taken off simultaneously in enzymolysis process
Raw meat processing, a step are completed, and carry out relevant treatment again without subsequent, therefore the preparation efficiency of fish oil is higher.
C, to step b treated enzymolysis liquid filtering and removing slag, layering, isolated upper layer fish oil and lower layer's oil are then allowed to stand
Water mixed liquid.
In this step, the fish oil purity on upper layer is very high, can directly be separated, and in the oil water mixture of lower layer,
The stirring in presence and enzymolysis process, oscillation due to emulsion, form relatively stable oil-in-water emulsion systems, quiet
It sets, centrifugal treating can not effectively separate grease.
D, the oil-water mixture is transferred in foam fraction factor column, is ventilated to the bottom of the foam fraction factor column,
Oil-water mixture upper layer generates froth bed, and froth bed is separated with liquid in time;Wherein, Ventilation Rate 2-4L/min,
The processing time is 10-30min, and oil-water mixture temperature is 20-30 DEG C, and oil-water mixture pH is controlled in 6-7.
Foam fraction factor is carried out to oil-water mixture, in the foaming process of foam fraction factor, due to emulsifying in oil-water mixture
Substance has very strong surface tension, and the surface of foam is gas-liquid separation interface, therefore emulsifier can be gathered in foam table
Face is collected separation to foam, so as to separate emulsifier from oil-water mixture.When in oil-water mixture
After the content of emulsifier substantially reduces, the oil-in-water system in oil-water mixture is disintegrated, and water-oil separating difficulty substantially reduces.
E, by step d, treated that oil-water mixture is centrifuged, and obtains upper layer fish oil.
F, the upper layer fish oil for obtaining step c and step e mixes, and obtains fish oil.
Fish oil processing method of the invention, not only simple process, but also from the oil-water mixture for capableing of lower layer further
Fish oil is extracted, the recovery rate of fish oil is higher, and fish oil purity is also higher, and without fishy smell, color is transparent pure.
Preferably, before carrying out step b, the blank is pre-processed into crossing: in excessive temperature being 30-40 DEG C by blank
Water in dipping swelling 1-2h.
Dipping swelling treatment is carried out to blank before enzymatic hydrolysis, cell membrane is enabled to be in the state that swells, cell membrane more holds
It is fragile, to be conducive to digest.
Preferably, while digesting to blank, carrying out supersonic oscillations processing to enzymolysis liquid in step b.?
Supersonic oscillations processing is carried out in enzymolysis process, can speed up the breakage of cell membrane, improves enzymolysis efficiency.But it also brings simultaneously
Disadvantage: supersonic oscillations processing can reinforce the emulsifying effectiveness of enzymolysis liquid, so that water-oil separating difficulty increases, but pass through this hair
The foam fraction factor technique of bright subsequent process is able to solve this problem.
Preferably, the immobilization magnetic coupling enzyme the preparation method comprises the following steps: dissolving the chitosan in the second of 8-12wt%
In acid solution, the chitosan solution that concentration is 2-3wt% is made;Composite aerogel particle and four oxygen are added into chitosan solution
Change three iron particles, mixing suspension is made;Wherein, the quality of composite aerogel particle is 0.5-1.5 times of chitosan, four oxidations
The quality of three iron particles is 0.5-1 times of chitosan;The department that quality is mixing suspension 3-5% is added dropwise into mixing suspension
Disk -80 simultaneously carries out ultrasonic wave dispersion and emulsion, and then first addition volume is mixing suspension 0.1-0.3% in backward mixing suspension
Glutaraldehyde and volume be 0.5-1 times of mixing suspension 4wt% sodium hydroxide solution and stir evenly, then use magnet into
After separating liquid, Magnetic Microspheres-Carrier is made in row absorption after being cleaned, being freeze-dried to solid matter;The magnetism is micro-
Balloon borne body is dispersed in the solution that complex enzyme content is 0.1-0.3wt%, and 1-3h is stirred at 25-35 DEG C, forms immobilization magnetic
Property complex enzyme, with magnet by immobilization magnetic coupling enzyme adsorbing separation, cleaning, drying;Wherein, the quality of Magnetic Microspheres-Carrier is
0.1-0.4 times of complex enzyme quality.
The Magnetic Microspheres-Carrier of the method for the present invention preparation, by chitosan, composite aerogel particle and ferroso-ferric oxide particle
Carry out it is compound, using ferroso-ferric oxide particle as magnetic core, with chitosan be coating carrier, composite aerogel particle be compound
" inlaying " in chitosan, after the crosslinking by glutaraldehyde, compound fastness is higher, recently after the activation of sodium hydroxide,
The Magnetic Microspheres-Carrier of formation has coating property well to enzyme material, and itself has very high porosity, can be right
Raw meat substance, pigment, heavy metal ion in enzymolysis liquid are effectively adsorbed, and adsorption rate is high, and adsorption capacity is big, so as to one
Step realizes enzymatic hydrolysis, deodorant, decolorization, improves extraction efficiency.
Preferably, the composite aerogel particle the preparation method comprises the following steps: by furfural, water soluble phenol resin, sepiolite
Powder and water 4-6:1:0.4-0.6:100 in mass ratio mixing, obtain mixed liquor after mixing evenly, are by concentration under agitation
The ammonium hydroxide of 0.5mol/L is added drop-wise in mixed liquor until mixed liquor is in neutrality;Then 10-20h is reacted at 55-65 DEG C, is answered
Close charcoal colloidal sol;Activated carbon composite colloidal sol is mixed with TiO 2 sol 1:0.5-1.5 in mass ratio, obtains mixing after mixing evenly molten
Glue, after mixed sols is stood aging 1-2 days at room temperature, first with dehydrated alcohol to mixed sols solvent displacement 12-24h, then
Solvent displacement 6-12h is carried out to mixed sols with n-hexane, plural gel is made after removing n-hexane;Finally use carbon dioxide
Supercritical fluid, which carries out crushing after being dried plural gel, obtains composite aerogel particle.
The composite aerogel particle of the method for the present invention preparation is charcoal/sepiolite/titanium dioxide composite aerogel, the compound gas
Gel possesses the porosity of superelevation, and pore-size is different, distribution is wide, can adsorb to different substances, and adsorption efficiency is high,
Deodorant, decoloration effectively can be carried out to enzymolysis liquid.And there is preferable hydrophily, fish oil will not be adsorbed.
Preferably, the complex enzyme is the mixture of neutral proteinase, trypsase and papain.Compound protein
Enzyme can greatly improve enzymolysis efficiency.
Preferably, the mass ratio of the neutral proteinase, trypsase and papain is 1:1-2:1.
Preferably, adding the sodium chloride that quality is enzymolysis liquid 4-6wt% into enzymolysis liquid in step b.Sodium chloride adds
Enter the separating degree that can increase grease, so that grease is more easily separated.
Preferably, the internal diameter of the foam fraction factor column is 40-50mm, the loading of oil water mixture is high in foam fraction factor column
Degree is 40-50cm.The specification of foam fraction factor column of the invention is to can be improved bubble according to the specific setting of fish internal organ enzymolysis liquid
Foam separative efficiency, farthest isolates emulsifier.
It is compared with the prior art, the beneficial effects of the present invention are: the present invention proposes the processing method simple process of fish oil
Take efficiency and recovery rate high, and the fish oil purity is high that processing obtains, no fishy smell, color are pure.
Specific embodiment
The present invention will be further described with reference to the examples below.
Embodiment 1
Early period reagent preparation:
The preparation of composite aerogel particle: by furfural, water soluble phenol resin, sepiolite powder and water 5:1 in mass ratio:
0.5:100 mixing, obtains mixed liquor after mixing evenly, and the ammonium hydroxide that concentration is 0.5mol/L is added drop-wise to mixing under agitation
Until mixed liquor is in neutrality in liquid;Then 15h is reacted at 60 DEG C, obtains activated carbon composite colloidal sol;By activated carbon composite colloidal sol and titanium dioxide
Titanium colloidal sol 1:1 in mass ratio mixing, obtains mixed sols after mixing evenly, mixed sols is stood to aging 1.5 days at room temperature
Afterwards, first with dehydrated alcohol to mixed sols solvent displacement 18h, then with n-hexane solvent displacement 9h is carried out to mixed sols, removed
Plural gel is made after n-hexane;It is crushed i.e. after being finally dried using Co 2 supercritical fluid to plural gel
Composite aerogel particle is made.
The preparation of immobilization magnetic coupling enzyme: dissolving the chitosan in the acetic acid solution of 10wt%, and obtained concentration is
The chitosan solution of 2.5wt%;Composite aerogel particle and ferroso-ferric oxide particle are added into chitosan solution, and mixing is made
Suspension;Wherein, the quality of composite aerogel particle is 1 times of chitosan, and the quality of ferroso-ferric oxide particle is chitosan
0.75 times;The Arlacel-80 that quality is mixing suspension 4% is added dropwise into mixing suspension and carries out ultrasonic wave dispersion and emulsion, so
First addition volume is the glutaraldehyde of mixing suspension 0.2% in backward mixing suspension afterwards and volume is 0.75 times of mixing suspension
4wt% sodium hydroxide solution and stir evenly, then adsorbed with magnet, separate liquid after, to solid matter carry out
Magnetic Microspheres-Carrier is made after cleaning, freeze-drying;It is 0.2wt%'s that the Magnetic Microspheres-Carrier, which is dispersed in complex enzyme content,
In solution, stir 2h at 30 DEG C, form immobilization magnetic coupling enzyme, with magnet by immobilization magnetic coupling enzyme adsorbing separation,
Cleaning, drying;Wherein, the quality of Magnetic Microspheres-Carrier is 0.25 times of complex enzyme quality.
Wherein, the complex enzyme is the mixture of neutral proteinase, trypsase and papain, and neutral protein
The mass ratio of enzyme, trypsase and papain is 1:1.5:1.
A kind of exquisite processing method of fish oil, sequentially includes the following steps:
A, cleaning impurity elimination is carried out to fish internal organ, smashed to pieces, blank is made, by blank in the water that excessive temperature is 35 DEG C
Dipping is swollen 1.5h, then spare.
B, the blank is added in the enzymolysis liquid containing immobilization magnetic coupling enzyme, under the conditions of supersonic oscillations into
Row enzymatic hydrolysis, wherein blank, enzymolysis liquid mass ratio be 1:3, the enzyme content in enzymolysis liquid is 0.125%, and hydrolysis temperature is 45 DEG C,
Enzymolysis time 4h, enzymolysis liquid pH are controlled in 6.5-7;The immobilization magnetic coupling enzyme is recycled with magnet after enzymatic hydrolysis.
C, to step b treated enzymolysis liquid filtering and removing slag, layering, isolated upper layer fish oil and lower layer's oil are then allowed to stand
Water mixed liquid.
D, the oil-water mixture is transferred in foam fraction factor column, is ventilated to the bottom of the foam fraction factor column,
Oil-water mixture upper layer generates froth bed, and froth bed is separated with liquid in time;Wherein, Ventilation Rate 3L/min, place
The reason time is 20min, and oil-water mixture temperature is 25 DEG C, and oil-water mixture pH is controlled in 6-7.The internal diameter of the foam fraction factor column
For 45mm, the loading height of oil water mixture is 45cm in foam fraction factor column.
E, by step d, treated that oil-water mixture is centrifuged, and obtains upper layer fish oil.
F, the upper layer fish oil for obtaining step c and step e mixes, and obtains fish oil.
Embodiment 2
Early period reagent preparation:
The preparation of composite aerogel particle: by furfural, water soluble phenol resin, sepiolite powder and water 4:1 in mass ratio:
0.4:100 mixing, obtains mixed liquor after mixing evenly, and the ammonium hydroxide that concentration is 0.5mol/L is added drop-wise to mixing under agitation
Until mixed liquor is in neutrality in liquid;Then 20h is reacted at 55 DEG C, obtains activated carbon composite colloidal sol;By activated carbon composite colloidal sol and titanium dioxide
Titanium colloidal sol 1:0.5 in mass ratio mixing, obtains mixed sols after mixing evenly, mixed sols is stood to aging 1 day at room temperature
Afterwards, first with dehydrated alcohol to mixed sols solvent displacement 12h, then with n-hexane solvent displacement 12h is carried out to mixed sols, removed
Plural gel is made after n-hexane;It is crushed i.e. after being finally dried using Co 2 supercritical fluid to plural gel
Composite aerogel particle is made.
The preparation of immobilization magnetic coupling enzyme: dissolving the chitosan in the acetic acid solution of 8wt%, and obtained concentration is
The chitosan solution of 2wt%;Composite aerogel particle and ferroso-ferric oxide particle are added into chitosan solution, and it is outstanding that mixing is made
Turbid;Wherein, the quality of composite aerogel particle is 0.5 times of chitosan, and the quality of ferroso-ferric oxide particle is chitosan
0.5 times;The Arlacel-80 that quality is mixing suspension 3% is added dropwise into mixing suspension and carries out ultrasonic wave dispersion and emulsion, then
First addition volume is the glutaraldehyde of mixing suspension 0.1% in backward mixing suspension and volume is 0.5 times of mixing suspension
The sodium hydroxide solution of 4wt% simultaneously stirs evenly, and is then adsorbed with magnet, after separating liquid, carries out to solid matter clear
Magnetic Microspheres-Carrier is made after washing, being freeze-dried;It is the molten of 0.1wt% that the Magnetic Microspheres-Carrier, which is dispersed in complex enzyme content,
In liquid, 3h is stirred at 25 DEG C, form immobilization magnetic coupling enzyme, with magnet by immobilization magnetic coupling enzyme adsorbing separation, clear
It washes, dry;Wherein, the quality of Magnetic Microspheres-Carrier is 0.1 times of complex enzyme quality.
Wherein, the complex enzyme is the mixture of neutral proteinase, trypsase and papain, and neutral protein
The mass ratio of enzyme, trypsase and papain is 1:1:1.
A kind of exquisite processing method of fish oil, sequentially includes the following steps:
A, cleaning impurity elimination is carried out to fish internal organ, smashed to pieces, blank is made, by blank in the water that excessive temperature is 30 DEG C
Dipping is swollen 2h, then spare.
B, the blank is added in the enzymolysis liquid containing immobilization magnetic coupling enzyme, quality is added into enzymolysis liquid is
The sodium chloride of enzymolysis liquid 4wt%.Digested under the conditions of supersonic oscillations, wherein blank, enzymolysis liquid mass ratio be 1:
2.5, the enzyme content in enzymolysis liquid is 0.05%, and hydrolysis temperature is 40 DEG C, enzymolysis time 6h, enzymolysis liquid pH controls in 6.5-7;Enzyme
Xie Houyong magnet recycles the immobilization magnetic coupling enzyme.
C, to step b treated enzymolysis liquid filtering and removing slag, layering, isolated upper layer fish oil and lower layer's oil are then allowed to stand
Water mixed liquid.
D, the oil-water mixture is transferred in foam fraction factor column, is ventilated to the bottom of the foam fraction factor column,
Oil-water mixture upper layer generates froth bed, and froth bed is separated with liquid in time;Wherein, Ventilation Rate 2L/min, place
The reason time is 30min, and oil-water mixture temperature is 20 DEG C, and oil-water mixture pH is controlled in 6-7.The internal diameter of the foam fraction factor column
For 40mm, the loading height of oil water mixture is 40cm in foam fraction factor column.
E, by step d, treated that oil-water mixture is centrifuged, and obtains upper layer fish oil.
F, the upper layer fish oil for obtaining step c and step e mixes, and obtains fish oil.
Embodiment 3
Early period reagent preparation:
The preparation of composite aerogel particle: by furfural, water soluble phenol resin, sepiolite powder and water 6:1 in mass ratio:
0.6:100 mixing, obtains mixed liquor after mixing evenly, and the ammonium hydroxide that concentration is 0.5mol/L is added drop-wise to mixing under agitation
Until mixed liquor is in neutrality in liquid;Then 10h is reacted at 65 DEG C, obtains activated carbon composite colloidal sol;By activated carbon composite colloidal sol and titanium dioxide
Titanium colloidal sol 1:1.5 in mass ratio mixing, obtains mixed sols after mixing evenly, mixed sols is stood to aging 2 days at room temperature
Afterwards, first mixed sols solvent is replaced for 24 hours with dehydrated alcohol, then solvent displacement 6h is carried out to mixed sols with n-hexane, removed
Plural gel is made after n-hexane;It is crushed i.e. after being finally dried using Co 2 supercritical fluid to plural gel
Composite aerogel particle is made.
The preparation of immobilization magnetic coupling enzyme: dissolving the chitosan in the acetic acid solution of 12wt%, and obtained concentration is
The chitosan solution of 3wt%;Composite aerogel particle and ferroso-ferric oxide particle are added into chitosan solution, and it is outstanding that mixing is made
Turbid;Wherein, the quality of composite aerogel particle is 1.5 times of chitosan, and the quality of ferroso-ferric oxide particle is the 1 of chitosan
Times;The Arlacel-80 that quality is mixing suspension 5% is added dropwise into mixing suspension and carries out ultrasonic wave dispersion and emulsion, then first
Addition volume is the glutaraldehyde of mixing suspension 0.3% and the 4wt% that volume is 1 times of mixing suspension in backward mixing suspension
Sodium hydroxide solution and stir evenly, then adsorbed with magnet, separate liquid after, solid matter is cleaned, is cold
Dry rear obtained Magnetic Microspheres-Carrier is lyophilized;The Magnetic Microspheres-Carrier is dispersed in the solution that complex enzyme content is 0.3wt%,
Stir 1h at 35 DEG C, form immobilization magnetic coupling enzyme, with magnet by immobilization magnetic coupling enzyme adsorbing separation, cleaning, do
It is dry;Wherein, the quality of Magnetic Microspheres-Carrier is 0.4 times of complex enzyme quality.
Wherein, the complex enzyme is the mixture of neutral proteinase, trypsase and papain, and neutral protein
The mass ratio of enzyme, trypsase and papain is 1:2:1.
A kind of exquisite processing method of fish oil, sequentially includes the following steps:
A, cleaning impurity elimination is carried out to fish internal organ, smashed to pieces, blank is made, by blank in the water that excessive temperature is 40 DEG C
Dipping is swollen 1h, then spare.
B, the blank is added in the enzymolysis liquid containing immobilization magnetic coupling enzyme, quality is added into enzymolysis liquid is
The sodium chloride of enzymolysis liquid 6wt%.Digested under the conditions of supersonic oscillations, wherein blank, enzymolysis liquid mass ratio be 1:
3.5, the enzyme content in enzymolysis liquid is 0.2%, and hydrolysis temperature is 50 DEG C, enzymolysis time 2h, enzymolysis liquid pH controls in 6.5-7;Enzyme
Xie Houyong magnet recycles the immobilization magnetic coupling enzyme.
C, to step b treated enzymolysis liquid filtering and removing slag, layering, isolated upper layer fish oil and lower layer's oil are then allowed to stand
Water mixed liquid.
D, the oil-water mixture is transferred in foam fraction factor column, is ventilated to the bottom of the foam fraction factor column,
Oil-water mixture upper layer generates froth bed, and froth bed is separated with liquid in time;Wherein, Ventilation Rate 4L/min, place
The reason time is 10min, and oil-water mixture temperature is 30 DEG C, and oil-water mixture pH is controlled in 6-7.The internal diameter of the foam fraction factor column
For 50mm, the loading height of oil water mixture is 50cm in foam fraction factor column.
E, by step d, treated that oil-water mixture is centrifuged, and obtains upper layer fish oil.
F, the upper layer fish oil for obtaining step c and step e mixes, and obtains fish oil.
The recovery rate of fish oil made from embodiment 1-3, purity, fishy smell sense organ, color are as shown in the table:
Recovery rate | Purity | Fishy smell sense organ | Color | |
Embodiment 1 | 90.3% | 94.4% | 0 | Clear pale yellow color |
Embodiment 2 | 95.2% | 96.6% | 0 | Clear pale yellow color |
Embodiment 3 | 92.8% | 95.9% | 0 | Clear pale yellow color |
Wherein, fishy smell subjective appreciation is classified are as follows: without fishy smell 0, slightly fishy smell 1, fishy smell weaker 2, has fishy smell 3, fishy smell is general
4, fishy smell lays particular stress on 5, and fishy smell heavier 6, fishy smell weighs 7 very much.
Raw materials used in the present invention, equipment is unless otherwise noted the common raw material, equipment of this field;In the present invention
Method therefor is unless otherwise noted the conventional method of this field.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way, it is all according to the present invention
Technical spirit any simple modification, change and equivalent transformation to the above embodiments, still fall within the technology of the present invention side
The protection scope of case.
Claims (7)
1. a kind of purification processing method of fish oil, it is characterised in that sequentially include the following steps:
A, cleaning impurity elimination is carried out to fish internal organ, smashed to pieces, blank is made;
B, the blank is added in the enzymolysis liquid containing immobilization magnetic coupling enzyme and is digested, matter is added into enzymolysis liquid
Amount is the sodium chloride of enzymolysis liquid 4-6wt%;While digesting to blank, supersonic oscillations processing is carried out to enzymolysis liquid;Its
Middle blank, enzymolysis liquid mass ratio be 1:2.5-3.5, the enzyme content in enzymolysis liquid is 0.05-0.2%, hydrolysis temperature 40-50
DEG C, enzymolysis time 2-6h, enzymolysis liquid pH are controlled in 6.5-7;The immobilization magnetic coupling enzyme is returned with magnet after enzymatic hydrolysis
It receives;
C, to step b treated enzymolysis liquid filtering and removing slag, it is then allowed to stand layering, isolated upper layer fish oil and lower layer's grease are mixed
Close liquid;
D, the oil-water mixture is transferred in foam fraction factor column, is ventilated to the bottom of the foam fraction factor column, grease
Mixed liquor upper layer generates froth bed, and froth bed is separated with liquid in time;Wherein, Ventilation Rate 2-4L/min, processing
Time is 10-30min, and oil-water mixture temperature is 20-30 DEG C, and oil-water mixture pH is controlled in 6-7;
E, by step d, treated that oil-water mixture is centrifuged, and obtains upper layer fish oil;
F, the upper layer fish oil for obtaining step c and step e mixes, and obtains fish oil.
2. a kind of purification processing method of fish oil as described in claim 1, which is characterized in that described before carrying out step b
Blank is pre-processed into crossing: in excessive temperature being dipping swelling 1-2h in 30-40 DEG C of water by blank.
3. a kind of purification processing method of fish oil as described in claim 1, which is characterized in that the immobilization magnetic coupling
Enzyme the preparation method comprises the following steps: dissolve the chitosan in the acetic acid solution of 8-12wt%, it is molten that the chitosan that concentration is 2-3wt% is made
Liquid;Composite aerogel particle and ferroso-ferric oxide particle are added into chitosan solution, and mixing suspension is made;Wherein, compound
The quality of aerogel particle is 0.5-1.5 times of chitosan, and the quality of ferroso-ferric oxide particle is 0.5-1 times of chitosan;To
The Arlacel-80 that quality is mixing suspension 3-5% is added dropwise in mixing suspension and carries out ultrasonic wave dispersion and emulsion, it is then first backward
Addition volume is the glutaraldehyde of mixing suspension 0.1-0.3% in mixing suspension and volume is 0.5-1 times of mixing suspension
The sodium hydroxide solution of 4wt% simultaneously stirs evenly, and is then adsorbed with magnet, after separating liquid, carries out to solid matter clear
Magnetic Microspheres-Carrier is made after washing, being freeze-dried;It is 0.1-0.3wt% that the Magnetic Microspheres-Carrier, which is dispersed in complex enzyme content,
Solution in, stir 1-3h at 25-35 DEG C, form immobilization magnetic coupling enzyme, inhaled immobilization magnetic coupling enzyme with magnet
Fufen is from, cleaning, dry;Wherein, the quality of Magnetic Microspheres-Carrier is 0.1-0.4 times of complex enzyme quality.
4. a kind of purification processing method of fish oil as claimed in claim 3, which is characterized in that the composite aerogel particle
The preparation method comprises the following steps: furfural, water soluble phenol resin, sepiolite powder and water 4-6:1:0.4-0.6:100 in mass ratio are mixed
Close, obtain mixed liquor after mixing evenly, under agitation by concentration be 0.5mol/L ammonium hydroxide be added drop-wise in mixed liquor until
Mixed liquor is in neutrality;Then 10-20h is reacted at 55-65 DEG C, obtains activated carbon composite colloidal sol;By activated carbon composite colloidal sol and titanium dioxide
Colloidal sol 1:0.5-1.5 in mass ratio mixing, obtains mixed sols after mixing evenly, mixed sols is stood to aging 1- at room temperature
After 2 days, solvent displacement 6- first is carried out to mixed sols to mixed sols solvent displacement 12-24h, then with n-hexane with dehydrated alcohol
Plural gel is made after removing n-hexane in 12h;Finally plural gel is dried using Co 2 supercritical fluid laggard
Row crushes and obtains composite aerogel particle.
5. a kind of purification processing method of fish oil as claimed in claim 3, which is characterized in that the complex enzyme is neutral egg
The mixture of white enzyme, trypsase and papain.
6. a kind of purification processing method of fish oil as claimed in claim 5, which is characterized in that the neutral proteinase, pancreas egg
The mass ratio of white enzyme and papain is 1:1-2:1.
7. a kind of purification processing method of fish oil as described in claim 1, which is characterized in that the foam fraction factor column it is interior
Diameter is 40-50mm, and the loading height of oil water mixture is 40-50cm in foam fraction factor column.
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