CN109370781A - A kind of high EPA, DHA content deep sea fish oil processing technology - Google Patents
A kind of high EPA, DHA content deep sea fish oil processing technology Download PDFInfo
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Abstract
The invention discloses the processing technologys of a kind of high EPA, the deep sea fish oil of DHA content, deep sea fish oil including techniques pair such as fish oil pretreatment, decoloration and deodorization, fractionation, winterization is handled, decoloration and deodorization is combined together by the technique, the refining for carrying out grease at a lower temperature shortens heating time simultaneously, effectively prevent DHA and EPA during deodorization decoloring in fish oil from decomposing and reducing a possibility that aoxidizing because temperature is excessively high, the generation for controlling the pollutants such as trans-fatty acid simultaneously, improves the content of the DHA and EPA of product；The content of DHA and EPA in fish oil are further increased by the process of refining and improved secondary winterization simultaneously, DHA in the fish oil that this method is handled and 3 times higher than common fish oil of EPA content or more are eventually passed through, health care product can be directly applied to, in baby food.
Description
Technical field
The present invention relates to the processing technologys of a kind of high EPA, the deep sea fish oil of DHA content, belong to the technology neck of fats and oils processing
Domain.
Background technique
Fish oil is the general designation of the intracorporal whole oily substances of fish, it includes body oil, liver oil and cerebrol, main fish oil be it is a kind of from
The grease that greasiness fish are extracted, is polyunsaturated fatty acid (DHA and EPA) rich in ω -3, has the health such as anti-inflammatory, adjusting blood lipid
Benefit.DHA germinates to brain development, brain neuroblastoma pipe, cranial nerve cell myelinization, controls the brain cell hair that information is transmitted
Educate, neuron extends and extension, neurotransmitter gradually forms has great importance, the fish oil rich in DHA is consumed deeply
Person likes.But fish oil is oxidized easily in process, DHA be easy is destroyed so that in fish oil finished product DHA content
It substantially reduces, such low content is not able to satisfy health care demand not only, and cannot achieve its good medical value, therefore, such as
Fruit will play DHA function well, need in fish oil DHA and EPA be further concentrated.
But the polyenoic fatty acid in deep sea fish oil, including DHA are to belong to heat and chemically unstable substance, are isolated purification
And its it is difficult, currently, the separating and purifying technology to DHA is mainly include the following types: 1, urea adduct method, mainly utilizes urea molecule
Stable crystal inclusion compound can be formed with linear saturated fatty acids or monounsaturated fatty acids in crystallization process to be precipitated, to obtain
The DHA product of high-purity, the disadvantage is that the reaction time is long, product yield is low, residual urea is serious；2, low-temperature solvent crystallisation,
Mainly using fatty acid (salt) different under low temperature in organic solvent the difference of solubility and isolate and purify.The disadvantage is that needing anti-
Long between seasonable, a large amount of organic solvents of recycling, separative efficiency be not high；3, lipase concentration method, to the triglycerides containing DHA/EPA
Carry out selective hydrolysis, it is final to be enriched with polyvalent unsaturated fatty acid triglycerides, the disadvantage is that the reaction time is long, be enriched with DHA and
EPA melting concn is 60% or more still more difficult；4, adsorption separation method, using the fatty acid of different saturation in adsorbent
Distribution coefficient on (such as silver ion) is different and separates.The disadvantage is that eluant, eluent be easy polluted product and separate scale compared with
It is small；5, supercritical CO2Extraction utilizes extractant CO2Possess excellent solvent in the state of certain temperature and certain pressure
Matter is separated using the difference of component of mixture molecular free path.The disadvantage is that equipment requirement is high, energy consumption is high；6, molecule
The way of distillation, its advantage is that operation is simple, at low cost, does not have dissolvent residual.
Therefore, general at present to be that method by molecular distillation improves content with the DHA and EPA that have kind, but fish
The general treatment process of oil is by pretreatment, decoloration and deodorization, molecular distillation and winterization etc., but in the technique in fish oil
DHA and EPA is usually oxidized decomposition because of the high temperature of decoloration and deodorization process, reduces the content of DHA and EPA in fish oil；Therefore, anxious
A kind of synthesis of need, the effective method for improving the content of DHA and EPA in fish oil.
Summary of the invention
In order to solve the above problem present in the prior art, the present invention provides a kind of high EPA, the deep-sea of DHA content
The processing technology of fish oil, by optimizing the techniques such as decoloration and deodorization, fractionation, winterization in fish oil to improve EPA, DHA in fish oil
Decoloration and deodorization is combined together by content, the technique, when carrying out the refining of grease at a lower temperature while shortening heating
Between, effectively prevent DHA and EPA during deodorization decoloring in fish oil from decomposing and reducing the possibility of oxidation because temperature is excessively high
Property, while the generation of the pollutants such as trans-fatty acid is controlled, improve the content of the DHA and EPA of product；Simultaneously by refining and
The process of improved secondary winterization further increases the content of DHA and EPA in fish oil, eventually passes through what this method was handled
3 times higher than common fish oil of DHA and EPA content or more in fish oil, health care product can be directly applied to, in baby food.
Technical scheme is as follows:
A kind of high EPA, DHA content deep sea fish oil processing technology, include the following steps:
Crude fish oil is pumped into pretreatment tank by step 1, is pre-processed；
Step 2 through the pretreated fish oil of step 1 with citric acid is that 100:0.01-0.02 is mixed in mass ratio, described mixed
Close the various pieces that object is uniformly distributed to inner-tower filling material from the tower top of packed tower by distributor；Glacial acetic acid steam is by packed tower tower
Bottom enters, and the temperature of glacial acetic acid steam distillation is 115-125 DEG C, and glacial acetic acid vapor flux is 30gh-1·kg-1, absolute pressure
For 0.7kPa, cooling degree after 30-40min is kept to be reduced to 50-60 DEG C；It will treated that fish oil is pumped into elution tank by packed tower
In, turn on agitator, mixing speed is that 150-200 turns/hour；The high alkali liquid that mass fraction is 14%~16% is sprayed into, mixing
Fish oil temperature is rapidly increased to 70~75 DEG C afterwards, being kept stirring speed is that 150-200 turns/hour, mixing time 20-30min；
5-8 hours, separation removal lower part impurity component are settled after stirring；The filler is 80%-90%'s in the elution tank
The mixture of the meerschaum adsorbent of carclazyte and 10%-30%；
Step 3 separates the fish oil by decoloration, deodorization processing using step fractionation apparatus；
Step 4 finally carries out winterization processing to classification fish oil, and the deep sea fish oil of high EPA, DHA content are obtained after filtering.
Further, the concrete operations of the step 1 are as follows: crude fish oil being pumped into pretreatment tank, turn on agitator is stirred
Mixing speed is that 200-300 turns/hour；Steam heating is opened, when temperature reaches 70 DEG C -80 DEG C, sprays into 15%-25% mass concentration
Sodium hydrate aqueous solution, be kept stirring speed be 200-300r/h with -80 DEG C of temperature 70 C, mixing time 0.25-0.5h；
Temperature is down to 40-60 DEG C after stirring, settles 5-8 hours, separation removal lower part impurity component.
Further, the concrete operations of the step 3 are as follows:
S1, the vacuum pump for successively opening one-eight grade；Until absolute pressure≤100Pa of level-one destilling tower, two to eight grades of steamings
It evaporates tower and reaches 10Pa；It is de-gassed at this point, the fish oil of step 2 is pumped into degassing tank, degassing temperature reaches in degassing tank
100-110℃；
S2, until the removal of foam in degassing tank, after degassing, open feed pump so that fish oil enter level-one distillation
In tower, stabilization is walked to expect 0.25-1h, and the punishment in advance pump and transmission then opened between level-one destilling tower and secondary distillation tower switch, and makes
It obtains level-one distillate and enters secondary distillation tower；The discharging pump for being located at bottom in level-one destilling tower is opened simultaneously, so that level-one is cooling
The residue of tower bottom is discharged；It so repeats, so that fish oil successively passes through one-eight grade of destilling tower, is fractionated step by step；Described one
The vapo(u)rizing temperature of grade destilling tower is 100-110 DEG C, and vapo(u)rizing temperature increases 5-10 DEG C in every increase first stage tower.
Further, the concrete operations of the step 4 are as follows:
The fish oil that step 3 is handled well is pumped into first degree crystalline tank, and keeping the temperature in first degree crystalline tank is 30-35 DEG C,
20-35min is kept, the temperature in first degree crystalline tank is then cooled to 8-10 DEG C, keeping mixing speed in tank is 4-6 revs/min
Clock, cooling rate is 1-1.5 DEG C/h, and after keeping 6-10h, the wax and ester matter in oil removing are gone in filtering；By above-mentioned filtered fish
Oil pump enters in secondary crystallization tank, and temperature is cooled to -5-3 DEG C by 8-10 DEG C, and keeping mixing speed in tank is 2-4 revs/min, cooling
Rate is 0.5-1 DEG C/h, and after standing 15h-25h, filtering goes the wax and ester matter in oil removing, high EPA, DHA contain after being refined
The deep sea fish oil of amount.
Further, it is described mixing decolorising agent be composed of the following raw materials by weight: 85% carclazyte and 20% sepiolite
Adsorbent.
Further, the meerschaum adsorbent is made by following methods: sepiolite being crushed, adds water to be adjusted to moisture and contains
The sepiolite aqueous solution that amount is 26%, extrusion obtains sepiolite strip under conditions of 110 DEG C, screw speed 70r/mim
Object, in the case of dynamic is rolled, it is 20% aqueous hydrochloric acid solution that volumetric concentration is added by spraying by the 0.25% of sepiolite quality, using list
Screw extruding kneader permeates 45min in 70 DEG C of kneadings, 105 DEG C dry, pulverize after meerschaum adsorbent.
Further, the pH value for the sepiolite aqueous solution that mass fraction is 1% is in 7.5-8.5, X-ray fluorescence spectra
Instrument measures the percentage composition of MgO in the sepiolite not less than 6%.
Further, the revolving speed of the feed pump is 60r/min.
Further, the quality of the crude fish oil in step 1 and the sodium hydrate aqueous solution of 15%-25% mass concentration
Than for 1:35-55.
The invention has the following beneficial effects:
1, the deep sea fish oil prepared by the technology, meets national standard reference, and finished product yield is high.DHA content ratio
Common high 3 times of fish oil or more can directly apply to health care product, in baby food.Meanwhile decolorization is optimized, it improves
The decolorizing efficiency of fish oil.The processing technology is simple, and synthesis yield is higher, and production cost is low.
2, one step of decoloration and deodorization of the present invention is completed, and simplifies decoloration and deodorization technique, meanwhile, it, will during decoloration and deodorization
Fish oil is mixed with citric acid, and citric acid is as a kind of antioxidant, so that DHA and EPA is avoided because of decoloration and deodorization process in fish oil
High temperature and be oxidized decomposition, furthermore, the addition of citric acid, can with fish oil because environmental pollution or pretreatment etc. during accidentally
Mixed metal ion-chelant, to ensure that oil quality.Meanwhile the application using glacial acetic acid solution instead of aqueous solution into
Row steam distillation deodorizing technology, temperature are controlled at 120 DEG C or so, and the refining for carrying out grease at a lower temperature shortens simultaneously
Heating time effectively prevents DHA and EPA during deodorization decoloring in fish oil from decomposing and reducing oxidation because temperature is excessively high
A possibility that, while the generation of the pollutants such as trans-fatty acid is controlled, improve the content of the DHA and EPA of product.The application simultaneously
Fish oil is handled using high alkali liquid after decoloration and deodorization, on the one hand eliminates the impurity such as citric acid and glacial acetic acid,
On the other hand secondary alkali refining has been carried out to fish oil, secondary alkali refining uses sodium bicarbonate, and one time alkali refining uses sodium hydroxide, the alkali refining
The short mixed mixing alkali refining method of sodium bicarbonate concentrated base is mixed using the light alkali of sodium hydroxide is long, such complex processing technology can
Enough overcome in the long mixed treatment process of simple light alkali soap stock containing dilutional hyponatremia, alkali reacted with neutral oil and neutral oil hydrolysis caused by
Property oil loss, overcome in the short mixed treatment process of simple concentrated base poor lye dispersion degree, alkali, oil time of contact short aquation effect to pay no attention to
Think and be saponified the disadvantages of risk is high, and can be reduced the generation of carbonic acid gas in alkali-refining process, so that soap stock and fish oil layer is smooth
It is layered, dispersion degree of the lye in grease can be guaranteed using secondary alkali-refining process in the present invention, so that oily alkali uniformly contacts
And sufficiently reaction, shorten refining process time while reducing lye usage amount as far as possible, while also reducing saponification risk, mentions
High refining yield.
3, the application uses carclazyte during fish oil decoloration and deodorization and sepiolite decolourizes, while using sea
Afrodite is decolourized by the mixing of sepiolite and carclazyte instead of traditional active carbon, decolorizing effect better than traditional active carbon with
The effect of the mixing decoloration of carclazyte.
4, the type of the fatty acid group origin cause of formation fish of fish oil is different and have bigger difference, since saturated fatty acid content is different or
The reasons such as distribution of person's fatty acid in sweet three ester be different, there are bigger differences for physical behavior at normal temperature, at low temperature
Difference is then bigger.Therefore, the freezing point very different of different cultivars fish oil, requirement of the final products to freezing point are also different
It causes, which dictates that the fish oil of different cultivars or its winterization condition of the fish oil of different purposes are also different, when fish oil crystallizes, has supercooling
Perhaps oversaturated phenomenon crystallization temperature is too low or too fast, will lead to and forms many nucleus in fish oil, increases number of words viscosity
Add, so that crystalline growth is interfered, therefore, because the mixing fish oil that the fish oil of the application is deep-sea fish is taken through a large number of experiments
The technique for carrying out secondary winterization to fish oil: first stage fish oil temperature is cooled to 8-10 DEG C, and keeping mixing speed in tank is 4-6
Rev/min, cooling rate is 1-1.5 DEG C/h, there is largely rouge crystallization generation admittedly in fish oil at this time, and keeping temperature in tank is 8-10
DEG C 6-10h, this period is rearing crystal time, is then filtered, and wax and ester matter in oil removing are gone；The temperature of the crystallization of second stage
And rate of temperature fall is slow relative to the first stage, temperature is -5-3 DEG C, and cooling rate is 0.5-1 DEG C/h, stands 15h-25h
Afterwards.This is because the saturated fatty acid content of the deep sea fish oil of the use of the application is higher and requires the freezing point of final products
When higher, the technique that should select secondary winterization first passes through a winterization, removes the wax and ester matter for being easier to crystallization of part,
By secondary crystallization, further decrease crystallization temperature, thus further remove fish oil in wax and ester matter, obtain high EPA and
The fish oil of the content of DHA avoid a winterization temperature it is too low caused by final products yield whole knot that is very low, or even generating
The phenomenon that fish oil of brilliant tank freezes.The winterization process can not only reduce the freezing point of fish oil, can also change the fatty acid of fish oil
Composition, especially can be improved the content of the EPA and DHA of liquid oil, further increases the application value and economic value of fish oil.
5, in the application crystallization process, stirring power greatly accelerates crystallization rate, but if mixing speed is too slow, heat transfer
Slowly, it will lead to local nucleus；If mixing speed is too fast, and can be such that crystallization is shredded, so as to cause filtration difficulty, influence to produce
Quality and yield, it is more unfavorable, therefore the mixing speed of the application is controlled at 2~6 revs/min.
Specific embodiment
It is several embodiments of the present invention below, further illustrates the present invention, but the present invention is not limited only to this.
Embodiment one:
A kind of high EPA, DHA content deep sea fish oil processing technology, include the following steps:
Crude fish oil is pumped into pretreatment tank by step 1, and turn on agitator, mixing speed is 200 turns/hour；Open steam
Heating when temperature reaches 70 DEG C, sprays into the sodium hydrate aqueous solution of 15% mass concentration, and being kept stirring speed is 200-300r/h
With -80 DEG C of temperature 70 C, mixing time 0.25-0.5h；Temperature is down to 40-60 DEG C after stirring, settles 5-8 hours, divides
It leaves away except lower part impurity component；The mass ratio of the crude fish oil and the sodium hydrate aqueous solution of 15%-25% mass concentration is 1:
35。
Step 2 through the pretreated fish oil of step 1 with citric acid is that 100:0.01 is mixed in mass ratio, the mixture
The various pieces of inner-tower filling material are uniformly distributed to by distributor from the tower top of packed tower；Glacial acetic acid steam by packed tower tower bottom into
Enter, the temperature of glacial acetic acid steam distillation is 115 DEG C, and glacial acetic acid vapor flux is 30gh-1·kg-1, absolute pressure is
0.7kPa keeps cooling degree after 30min to be reduced to 50 DEG C；It will be opened by packed tower treated fish oil is pumped into elution tank
Blender, mixing speed are 150 turns/hour；The high alkali liquid that mass fraction is 14% is sprayed into, rises fish oil temperature rapidly after mixing
To 70 DEG C, being kept stirring speed is 150 turns/hour, mixing time 20min；5 hours, separation removal are settled after stirring
Lower part impurity component；The filler is the mixture of 80% carclazyte and 10% meerschaum adsorbent in the elution tank；
Step 3, S1, the vacuum pump for successively opening one-eight grade；Until absolute pressure≤100Pa of level-one destilling tower, two are arrived
Eight grades of destilling towers reach 10Pa；At this point, the fish oil of step 2 is pumped into degassing tank, steam heating is opened, is kept in degassing tank
Vacuum, while temperature in degassing tank being made to reach 100 DEG C；S2, until the removal of foam in degassing tank, after degassing, open
Feed pump is opened, the revolving speed of feed pump is 60r/min；So that fish oil enters in level-one destilling tower, stabilization is walked to expect 0.25h, then opens
The punishment in advance pump and transmission switch between level-one destilling tower and secondary distillation tower are opened, so that level-one distillate enters secondary distillation tower；
The discharging pump for being located at bottom in level-one destilling tower is opened simultaneously, so that the residue of a grade cooling tower bottom is discharged；It so repeats, makes
The destilling tower that fish oil successively passes through one-eight grade is obtained, is fractionated step by step；The vapo(u)rizing temperature of the level-one destilling tower is 100 DEG C, often
Increase vapo(u)rizing temperature in first stage tower and increases by 5 DEG C.
Step 4, the fish oil for handling step 3 well are pumped into first degree crystalline tank, and keeping the temperature in first degree crystalline tank is 30
DEG C, 20min is kept, the temperature in first degree crystalline tank is then cooled to 8 DEG C, keeping mixing speed in tank is 4 revs/min, cold
But rate is 1 DEG C/h, and after keeping 6h, the wax and ester matter in oil removing are gone in filtering；Above-mentioned filtered fish oil is pumped into secondary knot
In brilliant tank, temperature is cooled to -5 DEG C, and keeping mixing speed in tank is 2 revs/min, and cooling rate is 0.5 DEG C/h, after standing 15h,
Filtering, goes the wax and ester matter in oil removing, the deep sea fish oil of high EPA after being refined, DHA content.
Further, mixing decolorising agent be composed of the following raw materials by weight: 80% carclazyte and 20% sepiolite absorption
Agent.The clay absorbent is made by following methods: sepiolite being crushed, water is added to be adjusted to the sepiolite that moisture content is 26%
Aqueous solution, extrusion obtains sepiolite bar, dynamic rolling situation under conditions of 110 DEG C, screw speed 70r/mim
Under, it is 20% aqueous hydrochloric acid solution that volumetric concentration is added by spraying by the 0.25% of sepiolite quality, squeezes kneader using single screw rod
Permeate 45min in 70 DEG C of kneadings, 105 DEG C dry, pulverize after meerschaum adsorbent.
Sepiolite selects: mass fraction for 1% the sepiolite aqueous solution pH value in 7.5-8.5, x-ray fluorescence
The percentage composition that spectrometer measures MgO is not less than 6%.
Embodiment two:
A kind of high EPA, DHA content deep sea fish oil processing technology, include the following steps:
Crude fish oil is pumped into pretreatment tank by step 1, and turn on agitator, mixing speed is 250 turns/hour；Open steam
Heating when temperature reaches 75 DEG C, sprays into the sodium hydrate aqueous solution of 20% mass concentration, and being kept stirring speed is 250r/h and temperature
75 DEG C of degree, mixing time 0.35h；Temperature is down to 50 DEG C after stirring, settles 7 hours, separation removal lower part impurity component；
The mass ratio of the crude fish oil and sodium hydroxide solution is 1:40.
Step 2 through the pretreated fish oil of step 1 with citric acid is that 100:0.015 is mixed in mass ratio, the mixture
The various pieces of inner-tower filling material are uniformly distributed to by distributor from the tower top of packed tower；Glacial acetic acid steam by packed tower tower bottom into
Enter, the temperature of glacial acetic acid steam distillation is 120 DEG C, and glacial acetic acid vapor flux is 30gh-1·kg-1, absolute pressure is
0.7kPa keeps cooling degree after 35min to be reduced to 55 DEG C；It will be opened by packed tower treated fish oil is pumped into elution tank
Blender, mixing speed are 150 turns/hour；The high alkali liquid that mass fraction is 15% is sprayed into, rises fish oil temperature rapidly after mixing
To 70 DEG C, being kept stirring speed is 150 turns/hour, mixing time 25min；7 hours, separation removal are settled after stirring
Lower part impurity component；The filler is the mixture of 85% carclazyte and 20% meerschaum adsorbent in the elution tank；
Step 3, S1, the vacuum pump for successively opening one-eight grade；Until absolute pressure≤100Pa of level-one destilling tower, two are arrived
Eight grades of destilling towers reach 10Pa；At this point, the fish oil of step 2 is pumped into degassing tank, steam heating is opened, is kept in degassing tank
Vacuum, while temperature in degassing tank being made to reach 100 DEG C；S2, until the removal of foam in degassing tank, after degassing, open
Feed pump is opened, the revolving speed of feed pump is 60r/min；So that fish oil enters in level-one destilling tower, stabilization is walked to expect 0.5h, then opens
Punishment in advance pump and transmission switch between level-one destilling tower and secondary distillation tower, so that level-one distillate enters secondary distillation tower；Together
Shi Kaiqi is located at the discharging pump of bottom in level-one destilling tower, so that the residue of a grade cooling tower bottom is discharged；So repeat, so that
Fish oil successively passes through one-eight grade of destilling tower, is fractionated step by step；The vapo(u)rizing temperature of the level-one destilling tower is 100 DEG C, every increasing
Vapo(u)rizing temperature in first stage tower is added to increase by 8 DEG C.
Step 4, the fish oil for handling step 3 well are pumped into first degree crystalline tank, and keeping the temperature in first degree crystalline tank is 35
DEG C, 20min is kept, the temperature in first degree crystalline tank is then cooled to 9 DEG C, keeping mixing speed in tank is 5 revs/min, cold
But rate is 1 DEG C/h, and after keeping 8h, the wax and ester matter in oil removing are gone in filtering；Above-mentioned filtered fish oil is pumped into secondary knot
In brilliant tank, temperature is cooled to 0 DEG C, and keeping mixing speed in tank is 3 revs/min, and cooling rate is 0.5 DEG C/h, after standing 20h,
Filtering, goes the wax and ester matter in oil removing, the deep sea fish oil of high EPA after being refined, DHA content.
Further, mixing decolorising agent be composed of the following raw materials by weight: 85% carclazyte and 15% sepiolite absorption
Agent.The clay absorbent is made by following methods: sepiolite being crushed, water is added to be adjusted to the sepiolite that moisture content is 26%
Aqueous solution, extrusion obtains sepiolite bar, dynamic rolling situation under conditions of 110 DEG C, screw speed 70r/mim
Under, it is 20% aqueous hydrochloric acid solution that volumetric concentration is added by spraying by the 0.25% of sepiolite quality, squeezes kneader using single screw rod
Permeate 45min in 70 DEG C of kneadings, 105 DEG C dry, pulverize after meerschaum adsorbent.
Sepiolite selects: mass fraction for 1% the sepiolite aqueous solution pH value in 7.5-8.5, x-ray fluorescence
The percentage composition that spectrometer measures MgO is not less than 6%.
Embodiment three:
A kind of high EPA, DHA content deep sea fish oil processing technology, include the following steps:
Crude fish oil is pumped into pretreatment tank by step 1, and turn on agitator, mixing speed is 300 turns/hour；Open steam
Heating when temperature reaches 80 DEG C, sprays into the sodium hydrate aqueous solution of 25% mass concentration, and being kept stirring speed is 200r/h and temperature
70 DEG C of degree, mixing time 0.25h；Temperature is down to 40 DEG C after stirring, settles 5 hours, separation removal lower part impurity component；
The mass ratio of the crude fish oil and sodium hydroxide solution is 1:55.
Step 2 through the pretreated fish oil of step 1 with citric acid is that 100:0.02 is mixed in mass ratio, the mixture
The various pieces of inner-tower filling material are uniformly distributed to by distributor from the tower top of packed tower；Glacial acetic acid steam by packed tower tower bottom into
Enter, the temperature of glacial acetic acid steam distillation is 125 DEG C, and glacial acetic acid vapor flux is 30gh-1·kg-1, absolute pressure is
0.7kPa keeps cooling degree after 40min to be reduced to 60 DEG C；It will be opened by packed tower treated fish oil is pumped into elution tank
Blender, mixing speed are 200 turns/hour；The high alkali liquid that mass fraction is 16% is sprayed into, rises fish oil temperature rapidly after mixing
To 75 DEG C, being kept stirring speed is 200 turns/hour, mixing time 30min；8 hours, separation removal are settled after stirring
Lower part impurity component；The filler is the mixture of 0% carclazyte and 30% meerschaum adsorbent in the elution tank；
Step 3, S1, the vacuum pump for successively opening one-eight grade；Until absolute pressure≤100Pa of level-one destilling tower, two are arrived
Eight grades of destilling towers reach 10Pa；At this point, the fish oil of step 2 is pumped into degassing tank, steam heating is opened, is kept in degassing tank
Vacuum, while temperature in degassing tank being made to reach 110 DEG C；S2, until the removal of foam in degassing tank, after degassing, open
Feed pump is opened, the revolving speed of feed pump is 60r/min；So that fish oil enters in level-one destilling tower, stabilization is walked to expect 1h, then opens one
Punishment in advance pump and transmission between grade destilling tower and secondary distillation tower switch, so that level-one distillate enters secondary distillation tower；Simultaneously
The discharging pump for being located at bottom in level-one destilling tower is opened, so that the residue of a grade cooling tower bottom is discharged；It so repeats, so that fish
Oil successively passes through one-eight grade of destilling tower, is fractionated step by step；The vapo(u)rizing temperature of the level-one destilling tower is 110 DEG C, every increase
Vapo(u)rizing temperature increases by 10 DEG C in first stage tower.
Step 4, the fish oil for handling step 3 well are pumped into first degree crystalline tank, and keeping the temperature in first degree crystalline tank is 35
DEG C, 35min is kept, the temperature in first degree crystalline tank is then cooled to 10 DEG C, keeping mixing speed in tank is 6 revs/min, cold
But rate is 1.5 DEG C/h, and after keeping 10h, the wax and ester matter in oil removing are gone in filtering；Above-mentioned filtered fish oil is pumped into two
In secondary crystallizing tank, temperature is cooled to 3 DEG C by 10 DEG C, and keeping mixing speed in tank is 4 revs/min, and cooling rate is 1 DEG C/h, quiet
After setting 25h, the wax and ester matter in oil removing are gone in filtering, the deep sea fish oil of high EPA after being refined, DHA content.
Further, mixing decolorising agent be composed of the following raw materials by weight: 90% carclazyte and 10% sepiolite absorption
Agent.The clay absorbent is made by following methods: sepiolite being crushed, water is added to be adjusted to the sepiolite that moisture content is 26%
Aqueous solution, extrusion obtains sepiolite bar, dynamic rolling situation under conditions of 110 DEG C, screw speed 70r/mim
Under, it is 20% aqueous hydrochloric acid solution that volumetric concentration is added by spraying by the 0.25% of sepiolite quality, squeezes kneader using single screw rod
Permeate 45min in 70 DEG C of kneadings, 105 DEG C dry, pulverize after meerschaum adsorbent.
Sepiolite selects: mass fraction for 1% the sepiolite aqueous solution pH value in 7.5-8.5, x-ray fluorescence
The percentage composition that spectrometer measures MgO is not less than 6%.
1, refined fish oil's ingredient
Not to untreated fish oil (sample 1) fish oil of the application, the refining treatment by the step 3 in embodiment 2
The fish oil (sample 2) of winterization processing by step 4, the fish oil (sample 3) by the winterization processing in embodiment 2, reality
It applies in the fish oil (sample 6) that the fish oil (sample 4) of the processing of example 1, the fish oil (sample 5) of the processing of embodiment 2 and embodiment 3 are handled
Water nonvolatile matter, acid value, peroxide value, unsaponifiable matter, iodine number, DHA content and EPA content detected, testing result is such as
Under:
Table 1
| Project | Sample 1 | Sample 2 | Sample 3 | Sample 4 | Sample 5 | Sample 6 |
| Water nonvolatile matter, % | 0.88 | 0.13 | 0.12 | 0.15 | 0.12 | 0.11 |
| Acid value, mg/g | 3.7 | 0.45 | 0.35 | 0.52 | 0.32 | 0.30 |
| Peroxide value, mmol/kg | 9.5 | 2.2 | 2.1 | 1.2 | 2.1 | 1.6 |
| Unsaponifiable matter, % | 2.3 | 2.1 | 2.1 | 2.1 | 2.1 | 2.1 |
| Iodine number, g/100g | 142 | 185 | 186 | 185 | 188 | 189 |
| DHA content, % | 12 | 30 | 34 | 38 | 36 | 38 |
| EPA content, % | 14 | 38 | 42 | 43 | 45 | 44 |
As shown in Table 1, the deep sea fish oil prepared by the technology, meets national standard reference；Pass through sample 1 and sample
The result of product 2 is it is found that DHA and EPA content by giving in the fish oil of the process are 3 times higher than untreated fish oil
More than；By sample 2, sample 3 and sample 5 result it is found that the fish oil by winterization than the fish oil without winterization DHA and
EPA content increases, meanwhile, fish oil by secondary winterization than a winterization fish oil being capable of DHA and EPA content
It is higher, it follows that the winterization of fish oil can not only reduce the freezing point of fish oil, it can also improve the EPA's and DHA of liquid oil
Content further improves the application value and economic value of fish oil.
2, mixing decolorising agent proportion selection
Experiment condition: being warming up to 110 DEG C for oil with the speed of 8 DEG C/min, be added the mixing decolorising agent of fish oil weight 8% into
Oil temperature is risen to 115 DEG C, cools down after keeping 35min, fish oil is pumped into deodorizing tank after filtering and is carried out at deodorization by row decolorization
Reason is cooled to 80 DEG C after deodorization processing.
Percent of decolourization measurement: fish oil is dissolved in petroleum ether, full wavelength scanner is carried out at 1900-1100nm, obtains maximum suction
Wavelength 440nm is received as Detection wavelength, using petroleum ether as reference, calculates the percent of decolourization of fish oil decoloration front and back.Formula is as follows:
Percent of decolourization (%)=(A0-A1)/A0×100
Wherein, A0For preceding absorbance of decolourizing, A1For absorbance after decoloration.
Color measuring: it refers to GBT 22460-2008 " measurement of animal and plant fat Lovibond color "
Mix the following different proportion of decolorising agent selection, the percent of decolourization obtained and color (red value and yellow value) result such as following table
2
Table 2
| Decolorising agent proportion | Percent of decolourization (%) | Red value | Huang value |
| Carclazyte: sepiolite=1:0 | 92 | 3.6 | 40 |
| Carclazyte: sepiolite=9:1 | 91.5 | 4.5 | 42 |
| Carclazyte: sepiolite=8:2 | 91.2 | 4.7 | 42.5 |
| Carclazyte: sepiolite=7:3 | 82 | 4.8 | 43 |
| Carclazyte: sepiolite=6:4 | 75 | 4.9 | 44 |
| Carclazyte: active carbon=8:2 | 84 | 3.5 | 38 |
As seen from the above table, when with the weight proportion of carclazyte and sepiolite between 8-9:1-2, percent of decolourization exists
90% or more, good decolorizing effect, but when continuing growing the ratio of carclazyte, red value is significantly reduced with yellow value, and is taken off
Although color rate has promotion by a small margin, this is because soap, phosphatide (including fish body albumen and colloid), secondary oxidation product in oil
Equal substances have stronger polarity relative to pigment, can be better than by the absorption of carclazyte, and extra carclazyte just carries out the suction of pigment
It is attached, therefore, though being conducive to the removal of pigment in the additive amount for improving carclazyte, equally also improve oil consumption；Therefore, it is imitated in decoloration
In situation similar in fruit, select the weight proportion of carclazyte and sepiolite in 8-9:1-2.
3, bleaching time selects
Experiment condition: oil is warming up to 125 DEG C with the speed of 8 DEG C/min, the mixing decolorising agent of fish oil weight 8% is added
(80% carclazyte and 20% meerschaum adsorbent) carries out decolorization, and oil temperature is risen to 115 DEG C, keep respectively 15min,
Cool down after 20min, 25min, 30min, 35min, 40min, 45min, fish oil is pumped into deodorizing tank after filtering and is carried out at deodorization
Reason is cooled to 80 DEG C after deodorization processing.
Percent of decolourization measurement: fish oil is dissolved in petroleum ether, full wavelength scanner is carried out at 1900-1100nm, obtains maximum suction
Wavelength 440nm is received as Detection wavelength, using petroleum ether as reference, calculates the percent of decolourization of fish oil decoloration front and back.Formula is as follows:
Percent of decolourization (%)=(A0-A1)/A0×100
Wherein, A0For preceding absorbance of decolourizing, A1For absorbance after decoloration.
Color measuring: it refers to GBT 22460-2008 " measurement of animal and plant fat Lovibond color ".
Mix the following different proportion of decolorising agent selection, the percent of decolourization obtained and color (red value and yellow value) result such as following table
3:
Table 3
| Bleaching time (min) | Percent of decolourization (%) | Red value | Huang value |
| 15 | 65 | 5.1 | 50 |
| 20 | 75 | 5.1 | 49 |
| 25 | 85 | 5.0 | 47 |
| 30 | 87 | 4.8 | 48 |
| 35 | 89 | 4.7 | 47 |
| 40 | 90 | 4.6 | 47 |
| 45 | 90.5 | 4.7 | 47 |
As shown in Table 3, with the extension of bleaching time, fish oil color is gradually decreased, and percent of decolourization is improved extremely by 65%
90.5%, at first 25 minutes, percent of decolourization was raised very fast, about increased 25.5%, at latter 20 minutes, percent of decolourization was only improved
5.5%, and the red value in this period and yellow value are kept approximately constant, therefore, from the point of view of raising decolorizing efficiency,
Bleaching time is controlled within a shortest time, therefore selects bleaching time for 30-40 minutes.
4, bleaching temperature selects
Experiment condition: oil is warming up to 125 DEG C with the speed of 8 DEG C/min, the mixing decolorising agent of fish oil weight 8% is added
(80% carclazyte and 20% meerschaum adsorbent) carries out decolorization, oil temperature is risen to respectively 90 DEG C, 100 DEG C, 110 DEG C,
115 DEG C, 120 DEG C, 125 DEG C cool down after keeping 35min, fish oil are pumped into deodorizing tank after filtering and carries out deodorization processing, at deodorization
80 DEG C are cooled to after reason.
Percent of decolourization measurement: fish oil is dissolved in petroleum ether, full wavelength scanner is carried out at 1900-1100nm, obtains maximum suction
Wavelength 440nm is received as Detection wavelength, using petroleum ether as reference, calculates the percent of decolourization of fish oil decoloration front and back.Formula is as follows:
Percent of decolourization (%)=(A0-A1)/A0×100
Wherein, A0For preceding absorbance of decolourizing, A1For absorbance after decoloration.
Color measuring: it refers to GBT 22460-2008 " measurement of animal and plant fat Lovibond color "
Mix the following different proportion of decolorising agent selection, the percent of decolourization obtained and color (red value and yellow value) result such as following table
4:
Table 4
| Bleaching temperature (DEG C) | Percent of decolourization (%) | Red value | Huang value |
| 95 | 62 | 5.1 | 48 |
| 105 | 85 | 5.0 | 47 |
| 115 | 91 | 5.0 | 47 |
| 125 | 92 | 4.8 | 46 |
| 130 | 85 | 4.8 | 46 |
| 135 | 76 | 4.7 | 47 |
As seen from the above table, with the raising of bleaching temperature, decoloration takes the lead in reducing after increasing, and temperature is decolourized at 130 DEG C, color
Damp rebound significantly, yellow value and red value increased, this is because a small amount of newborn pigment can be generated during high temperature decoloration,
It if chlorophyll can generate redness of the skin or complexion substance at high temperature, furthermore remains gummed paper and heavy metal also be easy to cause color to solidify, these are former
Because leading to grease color reversion.Therefore select bleaching temperature for 115-125 DEG C.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright description is applied directly or indirectly in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (9)
1. a kind of processing technology of the deep sea fish oil of high EPA, DHA content, which comprises the steps of:
Crude fish oil is pumped into pretreatment tank by step 1, is pre-processed；
Step 2 through the pretreated fish oil of step 1 with citric acid is that 100:0.01-0.02 is mixed in mass ratio, the mixture
The various pieces of inner-tower filling material are uniformly distributed to by distributor from the tower top of packed tower；Glacial acetic acid steam by packed tower tower bottom into
Enter, the temperature of glacial acetic acid steam distillation is 115-125 DEG C, and glacial acetic acid vapor flux is 30gh-1·kg-1, absolute pressure is
0.7kPa keeps cooling degree after 30-40min to be reduced to 50-60 DEG C；It will treated that fish oil is pumped into elution tank by packed tower
In, turn on agitator, mixing speed is that 150-200 turns/hour；The high alkali liquid that mass fraction is 14% ~ 16% is sprayed into, it will after mixing
Fish oil temperature is rapidly increased to 70 ~ 75 DEG C, and being kept stirring speed is that 150-200 turns/hour, mixing time 20-30min；Stirring
After settle 5-8 hours, separation removal lower part impurity component；In the elution tank filler be 80%-90% carclazyte and
The mixture of the meerschaum adsorbent of 10%-30%；
Step 3 separates the fish oil by decoloration, deodorization processing using step fractionation apparatus；
Step 4 finally carries out winterization processing to classification fish oil, and the deep sea fish oil of high EPA, DHA content are obtained after filtering.
2. the processing technology of the deep sea fish oil of a kind of high EPA as described in claim 1, DHA content, which is characterized in that described
The concrete operations of step 1 are as follows: by crude fish oil be pumped into pretreatment tank in, turn on agitator, mixing speed be 200-300 turn/it is small
When；Steam heating is opened, when temperature reaches 70 DEG C -80 DEG C, the sodium hydrate aqueous solution of 15%-25% mass concentration is sprayed into, keeps
Mixing speed is 200-300 r/h and -80 DEG C of temperature 70 C, mixing time 0.25-0.5h；Temperature is down to after stirring
40-60 DEG C, settle 5-8 hours, separation removal lower part impurity component.
3. the processing technology of the deep sea fish oil of a kind of high EPA as described in claim 1, DHA content, it is characterised in that: described
The concrete operations of step 3 are as follows:
S1, the vacuum pump for successively opening one-eight grade；Until absolute pressure≤100Pa of level-one destilling tower, two to eight grades of destilling towers
Reach 10Pa；It is de-gassed at this point, the fish oil of step 2 is pumped into degassing tank, degassing temperature reaches 100-110 in degassing tank
℃；
S2, until the removal of foam in degassing tank, after degassing, open feed pump so that fish oil enters in level-one destilling tower,
Stabilization is walked to expect 0.25-1h, then opens the punishment in advance pump between level-one destilling tower and secondary distillation tower and be driven switch, so that level-one
Distillate enters secondary distillation tower；The discharging pump for being located at bottom in level-one destilling tower is opened simultaneously, so that a grade cooling tower bottom
Residue discharge；It so repeats, so that fish oil successively passes through one-eight grade of destilling tower, is fractionated step by step；The level-one distillation
The vapo(u)rizing temperature of tower is 100-110 DEG C, and vapo(u)rizing temperature increases 5-10 DEG C in every increase first stage tower.
4. the processing technology of the deep sea fish oil of a kind of high EPA as claimed in claim 3, DHA content, it is characterised in that: described
The concrete operations of step 4 are as follows:
The fish oil that step 3 is handled well is pumped into first degree crystalline tank, and keeping the temperature in first degree crystalline tank is 30-35 DEG C, is kept
Temperature in first degree crystalline tank is then cooled to 8-10 DEG C by 20-35min, and keeping mixing speed in tank is 4-6 revs/min, cold
But rate is 1-1.5 DEG C/h, and after keeping 6-10h, the wax and ester matter in oil removing are gone in filtering；Above-mentioned filtered fish oil is pumped
Enter in secondary crystallization tank, temperature is cooled to -5-3 DEG C by 8-10 DEG C, and keeping mixing speed in tank is 2-4 revs/min, cooling rate
For 0.5-1 DEG C/h, after standing 15h-25h, the wax and ester matter in oil removing are gone in filtering, high EPA after being refined, DHA content
Deep sea fish oil.
5. the processing technology of the deep sea fish oil of a kind of high EPA as claimed in claim 4, DHA content, which is characterized in that described
Mixing decolorising agent be composed of the following raw materials by weight: 85% carclazyte and 20% meerschaum adsorbent.
6. the processing technology of the deep sea fish oil of a kind of high EPA as claimed in claim 5, DHA content, which is characterized in that described
Meerschaum adsorbent is made by following methods: sepiolite being crushed, adds water to be adjusted to the sepiolite that moisture content is 26% water-soluble
Liquid, extrusion obtains sepiolite bar under conditions of 110 DEG C, screw speed 70r/mim, dynamically in the case of rolling, presses
It is 20% aqueous hydrochloric acid solution that volumetric concentration, which is added, in the 0.25% of sepiolite quality by spraying, squeezes kneader in 70 DEG C using single screw rod
Mediate infiltration 45min, 105 DEG C dry, pulverize after meerschaum adsorbent.
7. the processing technology of the deep sea fish oil of a kind of high EPA as claimed in claim 5, DHA content, it is characterised in that: quality
The pH value for the sepiolite aqueous solution that score is 1% measures MgO in the sepiolite in 7.5-8.5, Xray fluorescence spectrometer
Percentage composition be not less than 6%.
8. the processing technology of the deep sea fish oil of a kind of high EPA as claimed in claim 3, DHA content, it is characterised in that: described
The revolving speed of feed pump is 60r/min.
9. the processing technology of the deep sea fish oil of a kind of high EPA as claimed in claim 2, DHA content, it is characterised in that: step 1
In the crude fish oil and 15%-25% mass concentration sodium hydrate aqueous solution mass ratio be 1:35-55.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111040873A (en) * | 2019-12-19 | 2020-04-21 | 安徽省新洲海洋生物制品有限公司 | Fish oil processing, refining and filtering process |
| CN112552998A (en) * | 2020-12-29 | 2021-03-26 | 福建天马科技集团股份有限公司 | Fish oil winterization process with secondary slow cooling and filtering equipment used by fish oil winterization process |
| CN113717789A (en) * | 2021-09-18 | 2021-11-30 | 广州市珺琳轩生物科技有限公司 | Antioxidant refining and purifying method of fish oil |
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| CN102847508A (en) * | 2012-06-13 | 2013-01-02 | 江南大学 | Clay adsorbent used in edible vegetable oil decolorization |
| US20180273877A1 (en) * | 2015-12-01 | 2018-09-27 | Nippon Suisan Kaisha, Ltd. | Docosahexaenoic acid-containing oil and method for producing same |
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| CN102847508A (en) * | 2012-06-13 | 2013-01-02 | 江南大学 | Clay adsorbent used in edible vegetable oil decolorization |
| US20180273877A1 (en) * | 2015-12-01 | 2018-09-27 | Nippon Suisan Kaisha, Ltd. | Docosahexaenoic acid-containing oil and method for producing same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111040873A (en) * | 2019-12-19 | 2020-04-21 | 安徽省新洲海洋生物制品有限公司 | Fish oil processing, refining and filtering process |
| CN112552998A (en) * | 2020-12-29 | 2021-03-26 | 福建天马科技集团股份有限公司 | Fish oil winterization process with secondary slow cooling and filtering equipment used by fish oil winterization process |
| CN113717789A (en) * | 2021-09-18 | 2021-11-30 | 广州市珺琳轩生物科技有限公司 | Antioxidant refining and purifying method of fish oil |
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