CN111411019A - Deep sea fish oil with high EPA content and processing technology thereof - Google Patents
Deep sea fish oil with high EPA content and processing technology thereof Download PDFInfo
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Images
Classifications
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- 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
- C11B3/02—Refining fats or fatty oils by chemical reaction
- C11B3/06—Refining fats or fatty oils by chemical reaction with bases
-
- 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
- C11B3/006—Refining fats or fatty oils by extraction
-
- 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
- C11B3/10—Refining fats or fatty oils by adsorption
-
- 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
- C11B3/12—Refining fats or fatty oils by distillation
Abstract
The invention discloses a processing technology of deep sea fish oil with high EPA content, which comprises the processes of ethyl esterification, enrichment, purification, temperature reduction, vacuum filtration and the like; the technology introduces a fluidized bed chromatography technology, carries out deeper continuous separation on the fish oil, avoids the process that EPA is possibly oxidized due to high-temperature deodorization and the like, is simple in technological operation, effectively improves the EPA content in the fish oil, and ensures the effective components of the fish oil. The deep sea fish oil prepared by the process meets the national first-level standard. The EPA content is more than 3 times higher than that of common fish oil, and can be directly applied to health products, infant food and the like.
Description
Technical Field
The invention relates to deep sea fish oil with high EPA content and a processing technology thereof, belonging to the technical field of grease processing.
Background
Fish oil is a generic term for all oily substances in the fish body. The fish oil is extracted from fatty fish, is rich in various omega-3 polyunsaturated fatty acids (omega-3 PUFA), such as eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA, commonly known as NAOHUANGJIN), and has the effects of enhancing immunity, regulating blood pressure and blood lipid, clearing thrombus, preventing arteriosclerosis, etc. EPA has significant effects on treating autoimmune deficiency, promoting the health of human circulatory system and normal growth and development. Studies have shown that EPA plays a positive role in the treatment of lung disease, kidney disease, type 2 diabetes, large bowel ulcers and crohn's disease. In addition, EPA helps to reduce cholesterol and triglyceride levels in humans; promoting the metabolism of saturated fatty acid in vivo; lowering blood viscosity, promoting blood circulation, and preventing cardiovascular diseases such as atherosclerosis, cerebral thrombosis, cerebral hemorrhage, and hypertension. Therefore, the fish oil rich in high EPA is widely applied to the fields of health products, medicines, infant food and the like, and is deeply pursued by consumers.
Polyunsaturated fatty acids including EPA in the deep-sea fish oil belong to heat and chemically unstable substances and are extremely easy to oxidize in the processing process, so that the content of EPA in the fish oil finished product is greatly reduced, the health care requirement is difficult to meet, and the good medical value of EPA cannot be realized.
At present, the methods for separating and purifying fish oil reported in the prior art mainly comprise: molecular distillation, low-temperature crystallization, urea inclusion, lipase, supercritical fluid extraction, silver resin chromatography, silver nitrate complexation and high performance liquid chromatography. Among them, molecular distillation, low-temperature crystallization, urea inclusion, lipase and supercritical fluid extraction usually produce a mixture of EPA and DHA, and the monomer purity is low, and is difficult to reach 75% or more. The method for separating and purifying high-purity EPA and DHA mostly adopts silver resin chromatography, silver nitrate complexation and high performance liquid chromatography, and the silver resin chromatography and the silver nitrate complexation need to use a large amount of expensive silver nitrate, so that the production cost is relatively high, and the silver nitrate is difficult to recover and seriously pollutes. The conventional high performance liquid chromatography is difficult to directly separate and purify the low-purity fish oil crude product to prepare high-purity EPA-EE and DHA-EE, and a sample is highly diluted in the purification process, so that a great burden is brought to the post-treatment. Therefore, a fish oil enrichment process which can effectively improve the EPA content in the fish oil and has high efficiency, rapidness and simple operation is urgently needed.
Patent document CN102285880A discloses a method for preparing EPA ethyl ester and DHA ethyl ester, which realizes separation of 200-600 mg of crude fish oil in a laboratory, but it utilizes high performance preparative chromatography, and has a limited scope for small sample amount and industrial application, and the purified sample needs to be extracted for further concentration, and is not suitable for technical production.
Chinese patent application CN105272844B discloses a method for purifying high-purity fish oil EPA ethyl ester and DHA ethyl ester, which comprises the steps of primary purification, secondary purification, concentration and the like. According to the method, the separation and purification of the sample can be completed only through liquid-phase preparative chromatography, the concentration of the sample can be realized by matching with a rotary evaporator, the operation is simple, the industrial production is easy to realize, but the EPA content of the produced EPA is low, and the enrichment and purification of high EPA cannot be realized. Chinese patent application CN109022118A discloses a method for extracting fish oil from a byproduct of a large-mesh tuna and a method for purifying EPA thereof, but the process has the defects of complex operation, high energy consumption, high cost and the like. Chinese patent application CN108034488A discloses a method for refining deep sea fish oil, which comprises the steps of enriching crude fish oil by a saponification-urea saturation method, and then washing and drying to obtain high-content deep sea fish oil. The method only separates and purifies EPA by washing and drying, although the operation is simple, the phenomena that fish oil products and solvents cannot be completely separated and wax and ester in the products are too high exist, so that the extracted fish oil contains too many impurities and the fish oil quality is not high.
Disclosure of Invention
In order to solve the problems of high energy consumption, high cost, complex process, low product yield, low purity and the like in the process, the deep sea fish oil rich in EPA prepared by the method meets the national primary standard, the EPA content is higher than that of the raw material fish oil by more than 3 times, and the deep sea fish oil rich in EPA can be directly applied to health care products, infant food and the like. Partial process of the process can be automatically controlled, is simple to operate, has low energy consumption, is environment-friendly and pollution-free, and removes processes such as high-temperature deodorization, thereby maximally ensuring that active ingredients in the fish oil are not damaged by oxidation.
The technical scheme of the invention is as follows:
the invention relates to a processing technology of deep sea fish oil with high EPA content, which comprises the following steps:
(1) performing ethyl esterification on the pretreated crude fish oil by using an alkaline catalysis method;
(2) performing inclusion enrichment on the prepared fish oil ethyl ester by using a saturated ethanol solution of urea;
(3) utilizing fluidized bed equipment to separate and purify EPA in the enriched fish oil ethyl ester, and collecting a product which flows out from a raffinate port after separation and purification by a simulated moving bed;
(4) and (3) performing solvent dewaxing treatment on the fish oil subjected to the chromatographic separation by the fluidized bed, and then evaporating and removing the dewaxing solvent to obtain the deep sea fish oil with high EPA content.
Further, the specific steps of the step (1) are as follows: putting the pretreated crude fish oil and absolute ethyl alcohol into a reaction kettle according to the weight ratio of 1:6, adding a sodium hydroxide aqueous solution with the mass concentration of 15 percent and the mass ratio of 0.3 percent to the fish oil into the reaction kettle as an alkali catalyst for catalysis, controlling the temperature of the reaction kettle at 75-77 ℃ and the reaction time at 2 hours, and fully reacting to obtain the fish oil ethyl ester.
Further, the specific operation of the step (2) is as follows:
mixing urea and absolute ethyl alcohol, heating and stirring to dissolve the urea and the absolute ethyl alcohol to prepare urea saturated ethyl alcohol solution; heating, stirring and mixing the urea saturated ethanol solution and the fish oil ethyl ester treated in the step (1), wherein the stirring temperature is 55 ℃, the stirring time is 30min, naturally cooling the reactant to room temperature, transferring the reactant to a low-temperature constant-temperature reaction bath, and sealing and clathrating; after the inclusion is finished, taking the product, performing suction filtration by using a vacuum suction filtration pump, discarding a solid phase, collecting liquid phase components, transferring the liquid phase components to a rotary evaporator to remove ethanol, and collecting the product; and then washing the product twice with distilled water, separating liquid, and drying with anhydrous sodium sulfate to obtain an enriched product. Further, the weight ratio of the saturated ethanol solution of urea to the fish oil ethyl ester in the step (2) is 3: 1.
Further, the inclusion temperature in the step (2) is 0 ℃, and the inclusion time is 9 hours.
Further, the specific operation of the step (3) is as follows:
s1, setting the fixed conditions of the fluidized bed equipment, namely selecting methanol as a mobile phase, adopting PS/DVB polymer filler with the particle size of 10um and the pore diameter of 10nm, setting the flow rate to be 1m L/min, the sample injection mass concentration to be 1.0 g/L and controlling the temperature to be 40 ℃;
s2: dissolving the enriched product in the step (2) in methanol to prepare a solution; adding the prepared solution into a fluidized bed chromatography device, and performing EPA separation and purification under the condition of S1;
s3: and collecting the product which flows out from the raffinate port after being separated and purified by the simulated moving bed.
Further, the specific operation of the step (4) is as follows:
conveying the fish oil product collected in the step (3) into a crystallization tower, controlling the oil temperature to 15-20 ℃, then flowing into a crystal growing tank, staying for 10-15 hours, and pumping for 3.0m3The flow of the solvent is sent into a mixer, and after the solvent is fully mixed with cold solvent ethanol which accounts for 40 percent of the oil mass and is input into a pre-coated vacuum filter, the wax and the oil are separated. And separating the filtered dewaxed oil from the solvent gas by a receiving tank, pumping the dewaxed oil into a mixed oil storage tank by a pump, filtering the dewaxed oil by a mixed oil filter, pumping the dewaxed oil into a mixed oil evaporator and a stripping tower by the pump to remove the solvent by evaporation, and dehydrating and drying the dewaxed oil by a drying tower to obtain the refined deep sea fish oil with high EPA content. Further, the temperature of the coolant ethanol is 18-20 ℃.
The invention has the following beneficial effects:
1. the deep sea fish oil prepared by the process technology meets the national first-level standard, and the finished product yield is high. The EPA content is more than 3 times higher than that of common fish oil, the processes of high-temperature deodorization and the like are avoided, the active ingredients in the fish oil are prevented from being damaged by oxidation to the maximum extent, and the fish oil can be directly applied to health care products and infant food. The processing technology is simple to operate, part of flow can be automatically controlled, the product purity is high, and the production cost is relatively low.
2. The technology utilizes a urea inclusion method to enrich EPA in fish oil, the separation principle is mainly based on the characteristics of unsaturated degree of fatty acid and different lengths of carbon chains, and some saturated fatty acid, low unsaturated fatty acid and short chain fatty acid in the product after ethyl esterification of the fish oil can be well removed, so that the purpose of EPA enrichment is achieved.
3. The process applies moving bed chromatographic separation technology (SMB) to the separation and purification process of fish oil, adopts single-factor experiment to determine the optimal elution flow rate and temperature of the fish oil, does not need to adjust the structure of equipment in the actual production process, only needs to set equipment operation parameters, and greatly reduces the difficulty of production operation. The technology mainly comprises 4 to 24 columns, 3 to 5 pumps and connecting columns and valves of various pipelines, improves the defect of intermittent separation of the classical chromatography, and is a continuous preparative chromatography technology. SMB separation has the advantages of high product purity and recovery rate, high stationary phase utilization rate, low solvent consumption, automatic control, etc.
4. The process adopts a method that the product is firstly put into a crystal growing tank for crystallization and then is input into a vacuum filter for filtration, wax and ester in the fish oil can be effectively removed according to different crystallization degrees of all components in the product, and then the fish oil is pumped into a mixed oil evaporator and a stripping tower for evaporation, and the solvent can be effectively removed according to different boiling points of the fish oil and the solvent, so that the fish oil with higher purity and better quality is obtained.
Drawings
FIG. 1 is a flow chart of a processing technology of deep sea fish oil with high EPA content.
Detailed Description
The first embodiment is as follows:
a processing technology of deep sea fish oil with high EPA content comprises the following steps:
step 1, putting fish oil and absolute ethyl alcohol into a reaction kettle according to a molar ratio of 1:7, adding a 15 mass percent sodium hydroxide aqueous solution with a mass ratio of 0.3 percent of the fish oil for alkali catalysis, and fully reacting at 75-77 ℃ to esterify the fish oil.
Step 2, mixing urea and absolute ethyl alcohol according to a certain proportion, heating and stirring to dissolve the urea to prepare a saturated ethyl alcohol solution of the urea; adding the prepared saturated ethanol solution of urea and fish oil ethyl ester into an instant heating type constant-temperature heating magnetic stirrer according to the ratio of 3:1, stirring at 55 ℃ for 30min, naturally cooling to room temperature, and then transferring to a low-temperature constant-temperature reaction bath for sealing inclusion at 0 ℃ for 9 hours. And (3) carrying out suction filtration by using a vacuum suction filtration pump, discarding a solid phase, removing ethanol from a liquid phase by using a rotary evaporator, washing the product twice by using distilled water, separating the liquid, and drying by using anhydrous sodium sulfate to obtain an enriched product.
And 3, S1, setting the fixed conditions of the simulated moving bed equipment, namely selecting methanol as a mobile phase, adopting PS/DVB polymer filler with the particle size of 10um and the pore diameter of 10nm, and carrying out the steps of 1m L/min of flow speed, 1.0 g/L of sample introduction mass concentration and 40 ℃ of operation temperature.
S2, dissolving the enriched product in the step 2 in methanol to prepare a solution; and (4) adding the prepared solution into a simulated moving bed chromatographic equipment to perform EPA separation and purification under the condition of S1.
And S3, collecting the product flowing out from a raffinate port after the separation and purification of the simulated moving bed.
Step 4, conveying the fish oil product obtained in the step 3 into a crystallization tower, starting a refrigerating machine to control the oil temperature to 15-20 ℃, then conveying the fish oil product into a crystal growing tank, staying for 10-15 hours, and pumping the fish oil product at a speed of 3.0m3The flow of the mixture is sent into a mixer at a flow rate of/h, and the mixture is fully mixed with cold solvent ethanol (18-20 ℃) which accounts for 40% of the oil mass and is input into a pre-coated vacuum filter to separate wax and oil. The filtered dewaxed oil is separated from the solvent gas by a receiving tank, then is pumped into a mixed oil storage tank by a pump, is filtered by a mixed oil filter and then is filtered by a mixed oil filterPumping into a mixed oil evaporator and a stripping tower to evaporate and remove the solvent, and dehydrating and drying in a drying tower to obtain the refined deep sea fish oil with high EPA content.
Example two:
a processing technology of deep sea fish oil with high EPA content comprises the following steps:
step 1, putting fish oil and absolute ethyl alcohol into a reaction kettle according to a molar ratio of 1:6, adding a 15 mass percent sodium hydroxide aqueous solution with a mass ratio of 0.3 percent of the fish oil for alkali catalysis, and fully reacting at 75-77 ℃ to esterify the fish oil.
Step 2, mixing urea and absolute ethyl alcohol according to a certain proportion, heating and stirring to dissolve the urea to prepare a saturated ethyl alcohol solution of the urea; adding the prepared saturated ethanol solution of urea and fish oil ethyl ester into an instant heating type constant-temperature heating magnetic stirrer according to the ratio of 2:1, stirring at 55 ℃ for 30min, naturally cooling to room temperature, and then transferring to a low-temperature constant-temperature reaction bath for sealing inclusion at 0 ℃ for 9 hours. And (3) carrying out suction filtration by using a vacuum suction filtration pump, discarding a solid phase, removing ethanol from a liquid phase by using a rotary evaporator, washing the product twice by using distilled water, separating the liquid, and drying by using anhydrous sodium sulfate to obtain an enriched product.
And 3, S1, setting the fixed conditions of the simulated moving bed equipment, namely selecting methanol as a mobile phase, adopting PS/DVB polymer filler with the particle size of 15um and the pore diameter of 10nm, and carrying out the steps of 1m L/min of flow speed, 1.0 g/L of sample introduction mass concentration and 40 ℃ of operation temperature.
S2, dissolving the enriched product in the step 2 in methanol to prepare a solution; and (4) adding the prepared solution into a simulated moving bed chromatographic equipment to perform EPA separation and purification under the condition of S1.
And S3, collecting the product flowing out from a raffinate port after the separation and purification of the simulated moving bed.
Step 4, conveying the fish oil product obtained in the step 3 into a crystallization tower, starting a refrigerating machine to control the oil temperature to 15-20 ℃, then conveying the fish oil product into a crystal growing tank, staying for 10-15 hours, and pumping the fish oil product at a speed of 3.0m3The flow of the mixture is sent into a mixer at a flow rate of/h, and the mixture is fully mixed with cold solvent ethanol (18-20 ℃) which accounts for 40% of the oil mass and is input into a pre-coated vacuum filter to separate wax and oil. Filtering outThe dewaxed oil is separated from the solvent gas by a receiving tank, then is conveyed into a mixed oil storage tank by a pump, is filtered by a mixed oil filter, is conveyed into a mixed oil evaporator and a stripping tower by the pump to remove the solvent by evaporation, and is dehydrated and dried by a drying tower to obtain the refined deep sea fish oil with high EPA content.
Example three:
a processing technology of deep sea fish oil with high EPA content comprises the following steps:
step 1, putting fish oil and absolute ethyl alcohol into a reaction kettle according to a molar ratio of 1:7, adding a 15 mass percent sodium hydroxide aqueous solution with a mass ratio of 0.4 percent of the fish oil for alkali catalysis, and fully reacting at 75-77 ℃ to esterify the fish oil.
Step 2, mixing urea and absolute ethyl alcohol according to a certain proportion, heating and stirring to dissolve the urea to prepare a saturated ethyl alcohol solution of the urea; adding the prepared saturated ethanol solution of urea and fish oil ethyl ester into an instant heating type constant-temperature heating magnetic stirrer according to the ratio of 2:1, stirring at 55 ℃ for 30min, naturally cooling to room temperature, and then transferring to a low-temperature constant-temperature reaction bath for sealing inclusion at 0 ℃ for 9 hours. And (3) carrying out suction filtration by using a vacuum suction filtration pump, discarding a solid phase, removing ethanol from a liquid phase by using a rotary evaporator, washing the product twice by using distilled water, separating the liquid, and drying by using anhydrous sodium sulfate to obtain an enriched product.
And 3, S1, setting the fixed conditions of the simulated moving bed equipment, namely selecting methanol as a mobile phase, adopting PS/DVB polymer filler with the particle size of 15um and the pore diameter of 10nm, and carrying out the steps of 1m L/min of flow speed, 1.0 g/L of sample introduction mass concentration and 40 ℃ of operation temperature.
S2, dissolving the enriched product in the step 2 in methanol to prepare a solution; and (4) adding the prepared solution into a simulated moving bed chromatographic equipment to perform EPA separation and purification under the condition of S1.
And S3, collecting the product flowing out from a raffinate port after the separation and purification of the simulated moving bed.
Step 4, conveying the fish oil product obtained in the step 3 into a crystallization tower, starting a refrigerating machine to control the oil temperature to 15-20 ℃, then conveying the fish oil product into a crystal growing tank, staying for 10-15 hours, and pumping the fish oil product at a speed of 3.0m3The flow rate of/h is fed into the mixer and pumped by the solvent pumpAnd (3) fully mixing cold solvent ethanol (18-20 ℃) accounting for 40% of the oil mass, and inputting the mixture into a pre-coated vacuum filter to separate wax and oil. And separating the filtered dewaxed oil from the solvent gas by a receiving tank, pumping the dewaxed oil into a mixed oil storage tank by a pump, filtering the dewaxed oil by a mixed oil filter, pumping the dewaxed oil into a mixed oil evaporator and a stripping tower by the pump to remove the solvent by evaporation, and dehydrating and drying the dewaxed oil by a drying tower to obtain the refined deep sea fish oil with high EPA content.
Example four:
a processing technology of deep sea fish oil with high EPA content comprises the following steps:
step 1, putting fish oil and absolute ethyl alcohol into a reaction kettle according to a molar ratio of 1:6, adding a 15 mass percent sodium hydroxide aqueous solution with a mass ratio of 0.4 percent of the fish oil for alkali catalysis, and fully reacting at 75-77 ℃ to esterify the fish oil.
Step 2, mixing urea and absolute ethyl alcohol according to a certain proportion, heating and stirring to dissolve the urea to prepare a saturated ethyl alcohol solution of the urea; adding the prepared saturated ethanol solution of urea and fish oil ethyl ester into an instant heating type constant-temperature heating magnetic stirrer according to the ratio of 3:1, stirring at 55 ℃ for 30min, naturally cooling to room temperature, and then transferring to a low-temperature constant-temperature reaction bath for sealing inclusion at 0 ℃ for 9 hours. And (3) carrying out suction filtration by using a vacuum suction filtration pump, discarding a solid phase, removing ethanol from a liquid phase by using a rotary evaporator, washing the product twice by using distilled water, separating the liquid, and drying by using anhydrous sodium sulfate to obtain an enriched product.
And 3, S1, setting the fixed conditions of the simulated moving bed equipment, namely selecting methanol as a mobile phase, adopting PS/DVB polymer filler with the particle size of 10um and the pore diameter of 10nm, and carrying out the steps of 1m L/min of flow speed, 1.0 g/L of sample introduction mass concentration and 40 ℃ of operation temperature.
S2, dissolving the enriched product in the step 2 in methanol to prepare a solution; and (4) adding the prepared solution into a simulated moving bed chromatographic equipment to perform EPA separation and purification under the condition of S1.
And S3, collecting the product flowing out from a raffinate port after the separation and purification of the simulated moving bed.
Step 4, conveying the fish oil product obtained in the step 3 into a crystallization tower, starting a refrigerating machine to control the oil temperature to 15-20 ℃,then conveying the mixture into a crystal growing tank, staying for 10-15 hours, and pumping for 3.0m3The flow of the mixture is sent into a mixer at a flow rate of/h, and the mixture is fully mixed with cold solvent ethanol (18-20 ℃) which accounts for 40% of the oil mass and is input into a pre-coated vacuum filter to separate wax and oil. And separating the filtered dewaxed oil from the solvent gas by a receiving tank, pumping the dewaxed oil into a mixed oil storage tank by a pump, filtering the dewaxed oil by a mixed oil filter, pumping the dewaxed oil into a mixed oil evaporator and a stripping tower by the pump to remove the solvent by evaporation, and dehydrating and drying the dewaxed oil by a drying tower to obtain the refined deep sea fish oil with high EPA content.
Comparative example one:
a processing technology of deep sea fish oil with high EPA content comprises the following steps:
step 1, putting fish oil and absolute ethyl alcohol into a reaction kettle according to a molar ratio of 1:6, adding a 15 mass percent sodium hydroxide aqueous solution with a mass ratio of 0.3 percent of the fish oil for alkali catalysis, and fully reacting at 75-77 ℃ to esterify the fish oil.
And 2, dissolving urea in 95% ethanol, stirring in a water bath at 65 ℃ until the mixed solution is clear, and preparing a urea saturated solution of ethanol. Reacting the fish oil (the urea of the fish oil: 3:2, w/w) subjected to multi-stage flow division for 0.5h, stopping heating, standing at a low temperature for a period of time, performing vacuum filtration, removing filtrate through rotary evaporation, washing the fish oil for 2-3 times, and performing vacuum dehydration to obtain the purified fish oil.
And 3, introducing the product subjected to multi-stage flow division into a deodorization tank for deodorization treatment, keeping the pressure at 0.27-0.40KPa in the reaction process, controlling the temperature at 180-210 ℃, and reacting for 3-8 h.
And 4, introducing the deodorized fish oil into a decoloring tank for decoloring, wherein activated clay is used as a decoloring adsorbent, the dosage of the activated clay is 0.3-2.5% of the grease, the temperature is controlled to be 60-110 ℃, the time is 1-3 hours, and then the adsorbent is removed through a plate and frame filter.
And 5, introducing the fish oil product obtained in the step 4 into a crystallizing tank, starting a refrigerator, cooling to the temperature of-5-3 ℃, entering the crystallizing tank, standing for 20-35 h, pumping the mixed oil subjected to freezing crystallization into a horizontal blade filter, filtering, and removing wax and ester in the fish oil to obtain the refined deep sea fish oil with high EPA content.
Comparative example:
the difference from the example 1 is that the steps 3 and 4 of the comparative example are to deodorize and decolor the fish oil by adopting the prior art; the specific deodorization and decoloration steps are as follows:
deodorizing: introducing the fish oil into a deodorization tank, keeping the pressure at 0.27-0.40KPa, the temperature at 180-210 ℃, and the time at 3-8 h.
And (3) decoloring: introducing deodorized fish oil into a decolorizing tank, adopting activated clay as a decolorizing adsorbent, wherein the dosage of the activated clay is 0.3-2.5% of the oil amount, the temperature is 60-110 ℃, and the time is 1-3h, and then removing the adsorbent by a plate and frame filter.
The fish oils of examples 1 to 4 and comparative examples were subjected to the quality test data shown in Table 1.
TABLE 1 Change in fish oil quality before and after refining in examples
According to the data, the deep sea fish oil prepared by the process technology meets the national first-level standard; the EPA content of the fish oil before refining is 25.9 percent, while the EPA content of the fish oil after refining is more than 80 percent, and the EPA content of the fish oil after refining is more than 3 times of that of the common fish oil, so the fish oil can be directly applied to health care products and infant food.
The above examples are intended to illustrate the invention the following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art, and the raw materials used are all commercially available products, but are not intended to limit the scope of the present invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art, and the raw materials used are commercially available products.
Claims (10)
1. A processing technology of deep sea fish oil with high EPA content is characterized by comprising the following steps:
(1) performing ethyl esterification on the pretreated crude fish oil by using an alkaline catalysis method;
(2) performing inclusion enrichment on the prepared fish oil ethyl ester by using a saturated ethanol solution of urea;
(3) utilizing fluidized bed equipment to separate and purify EPA in the enriched fish oil ethyl ester, and collecting a product which flows out from a raffinate port after separation and purification by a simulated moving bed;
(4) and (3) performing solvent dewaxing treatment on the fish oil subjected to the chromatographic separation by the fluidized bed, and then evaporating and removing the dewaxing solvent to obtain the deep sea fish oil with high EPA content.
2. The process for processing the deep sea fish oil with high EPA content according to claim 1, wherein the deep sea fish oil with high EPA content is prepared from the following raw materials in parts by weight: in the process of the step (1), in the ethyl esterification reaction, the molar ratio of the fish oil to the absolute ethyl alcohol is 1: 6; the reaction temperature is 75-77 ℃; the mass ratio of the sodium hydroxide aqueous solution with the catalyst dosage of 15 percent mass concentration to the fish oil is 0.3 percent.
3. The process for processing the deep sea fish oil with high EPA content according to claim 1, wherein the deep sea fish oil with high EPA content is prepared from the following raw materials in parts by weight: the specific steps of the step (1) are as follows: putting the pretreated crude fish oil and absolute ethyl alcohol into a reaction kettle according to the molar ratio of 1:6, adding a 15 mass percent sodium hydroxide aqueous solution with the mass ratio of 0.3 percent to the fish oil into the reaction kettle as an alkali catalyst, controlling the temperature of the reaction kettle between 75 and 77 ℃ and the reaction time to be 2 hours, and fully reacting to obtain the fish oil ethyl ester.
4. The process for processing the deep sea fish oil with high EPA content according to claim 1, wherein the deep sea fish oil with high EPA content is prepared from the following raw materials in parts by weight: the specific operation of the step (2) is as follows:
mixing urea and absolute ethyl alcohol, heating and stirring to dissolve the urea and the absolute ethyl alcohol to prepare urea saturated ethyl alcohol solution; heating, stirring and mixing the urea saturated ethanol solution and the fish oil ethyl ester treated in the step (1), wherein the stirring temperature is 55 ℃, the stirring time is 30min, naturally cooling the reactant to room temperature, transferring the reactant to a low-temperature constant-temperature reaction bath, and sealing and clathrating; after the inclusion is finished, taking the product, performing suction filtration by using a vacuum suction filtration pump, discarding a solid phase, collecting liquid phase components, transferring the liquid phase components to a rotary evaporator to remove ethanol, and collecting the product; and then washing the product twice with distilled water, separating liquid, and drying with anhydrous sodium sulfate to obtain an enriched product.
5. The process for processing the deep sea fish oil with high EPA content according to claim 1, wherein the deep sea fish oil with high EPA content is prepared from the following raw materials in parts by weight: the weight ratio of the saturated ethanol solution of urea to the fish oil ethyl ester in the step (2) is 2-3: 1.
6. The process for processing the deep sea fish oil with high EPA content according to claim 1, wherein the deep sea fish oil with high EPA content is prepared from the following raw materials in parts by weight: the inclusion temperature in the step (2) is 0 ℃, and the inclusion time is 9 hours.
7. The process for processing the deep sea fish oil with high EPA content according to claim 1, wherein the deep sea fish oil with high EPA content is prepared from the following raw materials in parts by weight: the specific operation of the step (3) is as follows:
s1, setting fixed conditions of fluidized bed equipment, namely selecting methanol as a mobile phase, adopting PS/DVB polymer filler with the particle size of 10um and the pore diameter of 10nm, setting the flow rate to be 1m L/min, the sample injection mass concentration to be 1.0 g/L, and controlling the temperature to be 40 ℃;
s2, dissolving the enriched product in the step (2) in methanol to prepare a solution; adding the prepared solution into a fluidized bed chromatography device, and performing EPA separation and purification under the condition of S1;
and S3, collecting the product flowing out from a raffinate port after the separation and purification of the simulated moving bed.
8. The process for processing the deep sea fish oil with high EPA content according to claim 1, wherein the deep sea fish oil with high EPA content is prepared from the following raw materials in parts by weight: the specific operation of the step (4) is as follows:
conveying the fish oil product collected in the step (3) into a crystallization tower, controlling the oil temperature to 15-20 ℃, then flowing into a crystal growing tank, staying for 10-15 hours, and pumping for 3.0m3Flow rate feed mixingThe device is fully mixed with cold solvent ethanol which accounts for 40 percent of the oil mass and is input by a solvent pump, and then the mixture is input into a pre-coated vacuum filter to separate wax and oil. And separating the filtered dewaxed oil from the solvent gas by a receiving tank, pumping the dewaxed oil into a mixed oil storage tank by a pump, filtering the dewaxed oil by a mixed oil filter, pumping the dewaxed oil into a mixed oil evaporator and a stripping tower by the pump to remove the solvent by evaporation, and dehydrating and drying the dewaxed oil by a drying tower to obtain the refined deep sea fish oil with high EPA content.
9. The process for processing the deep sea fish oil with high EPA content according to claim 7, wherein the deep sea fish oil with high EPA content is prepared from the following raw materials in parts by weight: the temperature of the coolant ethanol is 18-20 ℃.
10. A high EPA content deep sea fish oil produced by the process of any of claims 1 to 9.
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