CN109593606B - Deep sea fish oil with high DHA content and processing technology thereof - Google Patents

Deep sea fish oil with high DHA content and processing technology thereof Download PDF

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CN109593606B
CN109593606B CN201910097898.1A CN201910097898A CN109593606B CN 109593606 B CN109593606 B CN 109593606B CN 201910097898 A CN201910097898 A CN 201910097898A CN 109593606 B CN109593606 B CN 109593606B
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fish oil
deep sea
dha content
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oil
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CN109593606A (en
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薛婷
黄倩
卢玉栋
吴阳
黄鹭强
刘宜锋
陈由强
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Fujian Normal University
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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
    • C11B3/008—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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Microbiology (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Fats And Perfumes (AREA)

Abstract

The invention discloses a processing technology of deep sea fish oil with high DHA content, which comprises alkali refining, fractionation, freezing and other technologies; the adsorbent adopts special food-grade silica gel, and solves the problems of low yield, soil odor and the like of the activated clay used in the traditional process. The deep sea fish oil prepared by the process technology meets the national first-level standard. The DHA content is more than 3 times higher than that of common fish oil, and can be directly applied to health products and infant food.

Description

Deep sea fish oil with high DHA content and processing technology thereof
Technical Field
The invention relates to deep sea fish oil with high DHA content and a processing technology thereof, belonging to the technical field of grease processing.
Background
The fish oil is a general name of all oil substances in fish bodies and comprises body oil, liver oil and naphtha, and the main fish oil is grease extracted from fatty fish, is rich in omega-3 polyunsaturated fatty acid (DHA and EPA), and has health benefits of resisting inflammation, regulating blood fat and the like. DHA has important significance on brain development, brain neural tube development, brain nerve cell myelination, brain cell development for controlling information transmission, neuron extension and expansion and nerve conduction substance gradual formation, and the fish oil rich in DHA is popular among consumers. However, the fish oil is easily oxidized in the processing process, and the DHA is easily damaged, so that the DHA content in the fish oil finished product is greatly reduced, and thus the low content of the DHA can not meet the health care requirement, and the good medical value of the DHA can not be realized, so that the DHA and the EPA in the fish oil need to be further concentrated if the DHA function is well exerted.
However, the polyene fatty acid in the deep sea fish oil, including DHA, is a thermally and chemically unstable substance, and is difficult to separate and purify, and at present, the separation and purification technologies for DHA mainly comprise the following steps: 1. the urea inclusion method mainly utilizes the stable crystal inclusion compound formed by urea molecules and straight-chain saturated fatty acid or monounsaturated fatty acid in the crystallization process to separate out, thereby obtaining a high-purity DHA product, and has the defects of long reaction time, low product yield and serious urea residue; 2. the low temperature solvent crystallization method mainly utilizes the difference of the solubility of different fatty acids (salts) in organic solvents at low temperature to separate and purify. The disadvantages are long reaction time, recovery of a large amount of organic solvent and low separation efficiency; 3. the lipase concentration method is used for selectively hydrolyzing triglyceride containing DHA/EPA to finally enrich polyvalent unsaturated fatty acid triglyceride, and has the defects of long reaction time and difficult enrichment of mixed concentration of DHA and EPA above 60%; 4. adsorption separation, which uses the difference of distribution coefficients of fatty acids with different saturation on an adsorbent (such as silver ions), has the disadvantages that the product is easily polluted by the eluent and the separation scale is small; 5. supercritical CO2By extraction with an extractant CO2The solvent has excellent solvent property under the condition of certain temperature and certain pressure, and is separated by utilizing the difference of the free paths of the molecules of the components of the mixture. The disadvantages are high equipment requirement and high energy consumption; 6. the molecular distillation method has the advantages of simple operation, low cost and no solvent residue. Although the molecular distillation method can simply and effectively improve the DHA content in the fish oil, the prior high-temperature deodorization treatment reduces the effective components such as DHA in the fish oil in the prior processing treatment process. Therefore, there is a high necessity for a process capable of performing deodorization treatment at a low temperature to further improve the effective components such as DHA in fish oil.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides the deep sea fish oil with high DHA content and the processing technology thereof, the deep sea fish oil rich in DHA prepared by the method meets the national first-level standard, the DHA content is more than 2 times higher than that of the raw material fish oil, high-temperature deodorization is not needed, the oxidative damage of active ingredients in the fish oil is avoided, activated clay in the traditional technology is not used, and the problems of soil odor and the like in the clay are avoided. The method has the advantages of simple process, high yield, and low cost.
The technical scheme of the invention is as follows:
a processing technology of deep sea fish oil with high DHA content comprises the following steps: step 1, alkali refining is carried out on the pretreated fish oil; step 2, carrying out adsorption deodorization treatment on the decolored fish oil by using a refined adsorbent; step 3, separating the fish oil subjected to adsorption treatment by using cascade fractionation equipment; step 4, finally, freezing the graded fish oil, and filtering to obtain the deep sea fish oil with high DHA content; the refining adsorbent in the step 3 comprises the following components in percentage by weight: 200-500 mesh hydrophobic silica gel: 30-55 percent; 100-200 mesh hydrophobic silica gel: 20 to 35 percent; 60-100 mesh hydrophobic silica gel: 25 to 35 percent.
Further, the weight ratio of the refining adsorbent to the fish oil is 2-5%.
Further, the specific operation of step 1 is as follows: introducing the fish oil into an alkali treatment tank, starting a stirrer, and controlling the stirring speed at 200-300 r/h; starting steam to heat, spraying a 15% sodium hydroxide aqueous solution when the temperature reaches 70 ℃, keeping the stirring speed at 200-300 r/h and the temperature at 75 +/-5 ℃, and stirring for 0.25-0.5 h; and after stirring, reducing the temperature to 40-60 ℃, standing for 3-5 h, and performing oil-water separation.
Further, the specific operation of step 2 is as follows: introducing the alkali refined fish oil obtained in the step 1 into a refining kettle, keeping the temperature in the kettle not to exceed 80 ℃ at normal pressure; adding a refining adsorbent into a refining kettle while stirring, wherein the weight of the added refining adsorbent is 2-5% of that of the fish oil; the refining time is 30-60 min, the refining process is uniformly stirred, and the stirring speed is controlled to be 2500-3500 r/h; and filtering and separating the refining adsorbent by using an oil filter with the diameter of 2-3 mu m.
Further, the specific operation of step 3 is as follows:
s1, introducing the fish oil refined in the step 2 into a degassing tank, and degassing;
s2, after the foam in the degassing tank is eliminated, starting a feed pump at the rotating speed of 60r/min after the degassing is finished, so that the fish oil enters a primary cooling tower, the temperature in the primary cooling tower is 100-120 ℃, and after the material is stably discharged for 0.25-1 h, pumping the fish oil distillate in the primary cooling tower into a secondary cooling tower; the temperature in the secondary cooling tower is 105-130 ℃; after the material is stably fed for 0.25-1 h; pumping the fish oil distillate in the secondary cooling tower into a tertiary cooling tower; thus, the fish oil sequentially passes through one-eight stages of cooling towers to be fractionated step by step, the temperature in the towers is increased gradually at 5-10 ℃, and the stable material conveying time is 0.25-1 h;
s3, temporarily storing the fish oil processed in the step S2 in a buffer tank.
Further, the specific operation of step 4 is as follows:
and (3) introducing the fish oil obtained in the step (3) into a crystallizing tank, starting a refrigerator, cooling to the temperature of-5-3 ℃, allowing the fish oil to enter the crystallizing tank, standing for 20-35 hours, pumping the mixed oil subjected to freezing crystallization into a horizontal blade filter, filtering, and removing wax and ester in the oil to obtain the refined deep sea fish oil with high DHA content.
Further, the mass ratio of the fish oil in the step 1 to the 15% sodium hydroxide aqueous solution is 1: 35-55.
The invention has the following beneficial effects:
the deep sea fish oil prepared by the process technology meets the national first-level standard, and the finished product yield is high. The DHA content is more than 3 times higher than that of common fish oil, and can be directly applied to health products and infant food. High-temperature deodorization is not needed, the oxidative damage of active ingredients in the fish oil is avoided, activated clay in the traditional process is not used, and the problems of soil odor and the like in the clay are avoided. The method has the advantages of simple process, high synthesis yield, and low cost.
Detailed Description
The following are examples of the present invention, which are further illustrative of the present invention, but the present invention is not limited thereto.
The first embodiment is as follows:
a processing technology of deep sea fish oil with high DHA content comprises the following steps: step 1, introducing the fish oil into an alkali treatment tank, starting a stirrer, and controlling the stirring speed at 200 r/h; starting steam to heat, spraying 15% sodium hydroxide aqueous solution with mass concentration 35 times of the fish oil when the temperature reaches 70 ℃, and keeping the stirring speed at 200r/h and the temperature at 75 +/-5 ℃ for 0.25 h; cooling to 48 deg.C, standing for 4 hr, and separating oil and water. Step 2, introducing the alkali-refined fish oil obtained in the step 1 into a refining kettle, keeping the temperature in the kettle to be not more than 80 ℃ at normal pressure; adding a refining adsorbent into a refining kettle while stirring, wherein the weight of the added refining adsorbent is 2.5 percent of that of the fish oil; refining for 55min, uniformly stirring in the refining process, and controlling the stirring speed at 2500 r/h; filtering and separating the refining adsorbent by adopting an oil filter with the diameter of 2-3 microns, and introducing the fish oil into a transfer tank; 3, introducing the fish oil obtained in the step 2 into a degassing tank, starting steam, raising the temperature, and keeping the vacuum at 105 +/-5 ℃; when the foam in the degassing tank is eliminated, starting a feed pump after degassing is finished, and adjusting the rotating speed of the feed pump to be about 60r/min so that the fish oil enters a primary cooling tower and is stably discharged for 0.5h, wherein the temperature in the primary cooling tower is 100 ℃; then, a material passing pump and a transmission switch between the first-stage cooling tower and the second-stage cooling tower are started, so that the first-stage distillate enters the second-stage cooling tower; the temperature in the secondary cooling tower is 105 ℃; simultaneously starting a discharge pump positioned at the bottom in the primary cooling tower to discharge residues at the bottom of the primary cooling tower; the fish oil sequentially passes through a first-stage cooling tower to an eighth-stage cooling tower, the temperature in the tower is increased gradually at 5 ℃, and the stable material conveying time is 0.5 h; performing fractional distillation step by step; when the degassed oil gradually goes to a slag outlet in an eight-stage cooling tower, a heating switch is turned on, so that the degassed oil enters fractionation again; and temporarily storing the discharged semi-finished oil in a large buffer tank. And 4, introducing the fish oil obtained in the step 3 into a crystallizing tank, starting a refrigerator, cooling to the temperature of-5-3 ℃, allowing the fish oil to enter the crystallizing tank, standing for 25 hours, pumping the mixed oil subjected to freezing crystallization into a horizontal blade filter, filtering, and removing wax and ester in the oil to obtain the refined deep sea fish oil with high DHA content.
The refining adsorbent in the step 2 comprises the following components in percentage by weight: hydrophobic silica gel: 45 parts of 200-500 meshes; hydrophobic silica gel: 25 parts of 100-200 meshes; hydrophobic silica gel: 60-100 meshes, 30 parts.
Example two:
a processing technology of deep sea fish oil with high DHA content comprises the following steps: step 1, introducing the fish oil into an alkali treatment tank, starting a stirrer, and controlling the stirring speed at 250 r/h; starting steam to heat, spraying 15% sodium hydroxide aqueous solution with mass concentration 40 times of fish oil when the temperature reaches 70 ℃, and keeping the stirring speed at 250r/h and the temperature at 75 +/-5 ℃ for 0.25 h; cooling to 48 deg.C, standing for 4 hr, and separating oil and water; step 2, introducing the alkali-refined fish oil obtained in the step 1 into a refining kettle, keeping the temperature in the kettle to be not more than 80 ℃ at normal pressure; adding a refining adsorbent into a refining kettle while stirring, wherein the weight of the added refining adsorbent is 2.5 percent of that of the fish oil; refining for 55min, uniformly stirring in the refining process, and controlling the stirring speed at 2500 r/h; filtering and separating the refining adsorbent by using an oil filter with the diameter of 2-3 microns, and introducing the fish oil into a transfer tank; step 3, introducing the fish oil obtained in the step 2 into a degassing tank, starting steam to heat, and keeping vacuum at the temperature of 105 +/-5 ℃; when the foam in the degassing tank is eliminated, starting a feed pump after degassing is finished, and adjusting the rotating speed of the feed pump to be about 60r/min so that the fish oil enters a primary cooling tower and is stably discharged for 0.5h, wherein the temperature in the primary cooling tower is 100 ℃; then, a material passing pump and a transmission switch between the first-stage cooling tower and the second-stage cooling tower are started, so that the first-stage distillate enters the second-stage cooling tower; the temperature in the secondary cooling tower is 105 ℃; simultaneously starting a discharge pump positioned at the bottom in the primary cooling tower to discharge residues at the bottom of the primary cooling tower; the fish oil sequentially passes through a first-stage cooling tower to an eighth-stage cooling tower, the temperature in the tower is increased by 5 ℃, and the stable material conveying time is 0.5 h; fractional distillation step by step; when the degassed oil gradually goes to a slag outlet in an eight-stage cooling tower, a heating switch is turned on, so that the degassed oil enters fractionation again; and temporarily storing the discharged semi-finished oil in a large buffer tank. And 4, introducing the fish oil obtained in the step 3 into a crystallizing tank, starting a refrigerator, cooling to the temperature of-5-3 ℃, allowing the fish oil to enter the crystallizing tank, standing for 25 hours, pumping the mixed oil subjected to freezing crystallization into a horizontal blade filter, filtering, removing wax and ester in the oil, and obtaining the refined deep sea fish oil with high DHA content
The refining adsorbent in the step 2 comprises the following components in percentage by weight: hydrophobic silica gel: 200-500 meshes, 35 parts; hydrophobic silica gel: 30 parts of 100-200 meshes; hydrophobic silica gel: 60-100 meshes and 35 parts.
Example three:
a processing technology of deep sea fish oil with high DHA content comprises the following steps: step 1, introducing the fish oil into an alkali treatment tank, starting a stirrer, and controlling the stirring speed at 300 r/h; starting steam to heat, spraying 15% sodium hydroxide aqueous solution with mass concentration 40 times of fish oil when the temperature reaches 70 ℃, and keeping the stirring speed at 300r/h and the temperature at 75 +/-5 ℃ for 0.25 h; cooling to 48 deg.C, standing for 4 hr, and separating oil from water. Step 2, introducing the alkali-refined fish oil obtained in the step 1 into a refining kettle, keeping the temperature in the kettle to be not more than 80 ℃ at normal pressure; adding a refining adsorbent into a refining kettle while stirring, wherein the weight of the added refining adsorbent is 5% of that of the fish oil; the refining time is 55min, the refining process is uniformly stirred, and the stirring speed is controlled at 3500 r/h; filtering and separating the refining adsorbent by using an oil filter with the diameter of 2-3 microns, and introducing the fish oil into a transfer tank; 3, introducing the fish oil obtained in the step 2 into a degassing tank, starting steam, raising the temperature, and keeping the vacuum at 105 +/-5 ℃; when the foam in the degassing tank is eliminated, starting a feed pump after degassing is finished, and adjusting the rotating speed of the feed pump to be about 60r/min so that the fish oil enters a primary cooling tower and is stably discharged for 0.5h, wherein the temperature in the primary cooling tower is 100 ℃; then, a material passing pump and a transmission switch between the first-stage cooling tower and the second-stage cooling tower are started, so that the first-stage distillate enters the second-stage cooling tower; the temperature in the secondary cooling tower is 110 ℃; simultaneously starting a discharge pump positioned at the bottom in the primary cooling tower to discharge residues at the bottom of the primary cooling tower; the fish oil sequentially passes through a first-stage cooling tower to an eighth-stage cooling tower, the temperature in the tower is increased progressively at 10 ℃, and the stable material conveying time is 0.5 h; performing fractional distillation step by step; when the degassing oil gradually goes to a slag outlet in the eight-stage cooling tower, a heating switch is turned on, so that the degassing oil enters the fractionation again; and temporarily storing the discharged semi-finished oil in a large buffer tank. And 4, introducing the fish oil obtained in the step 3 into a crystallizing tank, starting a refrigerator, cooling to the temperature of-5-3 ℃, allowing the fish oil to enter the crystallizing tank, standing for 25 hours, pumping the mixed oil subjected to freezing crystallization into a horizontal blade filter, filtering, removing wax and ester in the oil, and obtaining the refined deep sea fish oil with high DHA content
The refining adsorbent in the step 1 comprises the following components in percentage by weight: hydrophobic silica gel: 42 parts of 200-500 meshes; hydrophobic silica gel: 28 parts of 100-200 meshes; hydrophobic silica gel: 60-100 meshes, 30 parts.
Example four:
a processing technology of deep sea fish oil with high DHA content comprises the following steps: step 1, introducing the fish oil into an alkali treatment tank, starting a stirrer, and controlling the stirring speed at 300 r/h; starting steam to heat, spraying 15% sodium hydroxide aqueous solution with mass concentration 55 times of fish oil when the temperature reaches 70 ℃, and keeping the stirring speed at 300r/h and the temperature at 75 +/-5 ℃ for 0.25 h; cooling to 48 deg.C, standing for 4 hr, and separating oil and water. Step 2, introducing the alkali-refined fish oil obtained in the step 1 into a refining kettle, keeping the temperature in the kettle to be not more than 80 ℃ at normal pressure; adding a refining adsorbent into a refining kettle while stirring, wherein the weight of the added refining adsorbent is 3% of that of the fish oil; the refining time is 55min, the refining process is uniformly stirred, and the stirring speed is controlled at 3500 r/h; filtering and separating the refining adsorbent by using an oil filter with the diameter of 2-3 microns, and introducing the fish oil into a transfer tank; 3, introducing the fish oil obtained in the step 2 into a degassing tank, starting steam, raising the temperature, and keeping the vacuum at 105 +/-5 ℃; when the foam in the degassing tank is eliminated, starting a feed pump after degassing is finished, and adjusting the rotating speed of the feed pump to about 60r/min so that the fish oil enters a primary cooling tower and is stably fed for 1h, wherein the temperature in the primary cooling tower is 120 ℃; then, a material passing pump and a transmission switch between the inside of the first-stage cooling tower and the second-stage cooling tower are started, so that the first-stage distillate enters the second-stage cooling tower; the temperature in the secondary cooling tower is 130 ℃; simultaneously starting a discharge pump positioned at the bottom in the primary cooling tower to discharge residues at the bottom of the primary cooling tower; the fish oil sequentially passes through a first-stage cooling tower to an eighth-stage cooling tower, the temperature in the tower is increased progressively at 10 ℃, and the stable material conveying time is 1 h; performing fractional distillation step by step; when the degassing oil gradually goes to a slag outlet in the eight-stage cooling tower, a heating switch is turned on, so that the degassing oil enters the fractionation again; and temporarily storing the discharged semi-finished oil in a large buffer tank. And 4, introducing the fish oil obtained in the step 3 into a crystallizing tank, starting a refrigerator, cooling to the temperature of-5-3 ℃, allowing the fish oil to enter the crystallizing tank, standing for 25 hours, pumping the mixed oil subjected to freezing crystallization into a horizontal blade filter, filtering, removing wax and ester in the oil, and obtaining the refined deep sea fish oil with high DHA content
The refining adsorbent in the step 2 comprises the following components in percentage by weight: hydrophobic silica gel: 200-500 meshes, 35 parts; hydrophobic silica gel: 35 parts of 100-200 meshes; hydrophobic silica gel: 30 portions of 60 to 100 meshes.
Example five:
a processing technology of deep sea fish oil with high DHA content comprises the following steps: step 1, introducing the fish oil into an alkali treatment tank, starting a stirrer, and controlling the stirring speed at 300 r/h; starting steam to raise the temperature, spraying 15% sodium hydroxide aqueous solution with the mass concentration of 55 times of the fish oil when the temperature reaches 70 ℃, and keeping the stirring speed at 300r/h and the temperature at 75 +/-5 ℃ for 0.25 h; cooling to 48 deg.C, standing for 4 hr, and separating oil from water. Step 2, introducing the alkali-refined fish oil obtained in the step 1 into a refining kettle, keeping the temperature in the kettle to be not more than 80 ℃ at normal pressure; adding a refining adsorbent into a refining kettle while stirring, wherein the weight of the added refining adsorbent is 2% of that of the fish oil; the refining time is 55min, the refining process is uniformly stirred, and the stirring speed is controlled at 3000 r/h; filtering and separating the refining adsorbent by using an oil filter with the diameter of 2-3 microns, and introducing the fish oil into a transfer tank; 3, introducing the fish oil obtained in the step 2 into a degassing tank, starting steam, raising the temperature, and keeping the vacuum at 105 +/-5 ℃; when the foam in the degassing tank is eliminated, starting a feed pump after degassing is finished, and adjusting the rotating speed of the feed pump to be about 60r/min so that the fish oil enters a primary cooling tower and is stably discharged for 0.5h, wherein the temperature in the primary cooling tower is 110 ℃; then, a material passing pump and a transmission switch between the inside of the first-stage cooling tower and the second-stage cooling tower are started, so that the first-stage distillate enters the second-stage cooling tower; the temperature in the secondary cooling tower is 115 ℃; simultaneously, a discharge pump positioned at the bottom in the primary cooling tower is started, so that residues at the bottom of the primary cooling tower are discharged; the fish oil sequentially passes through a first-stage cooling tower to an eighth-stage cooling tower, the temperature in the tower is increased gradually at 5 ℃, and the stable material conveying time is 0.5 h; performing fractional distillation step by step; when the degassing oil gradually goes to a slag outlet in the eight-stage cooling tower, a heating switch is turned on, so that the degassing oil enters the fractionation again; and temporarily storing the discharged semi-finished oil in a large buffer tank. And 4, introducing the fish oil obtained in the step 3 into a crystallizing tank, starting a refrigerator, cooling to the temperature of-5-3 ℃, allowing the fish oil to enter the crystallizing tank, standing for 25 hours, pumping the mixed oil subjected to freezing crystallization into a horizontal blade filter, filtering, removing wax and ester in the oil, and obtaining the refined deep sea fish oil with high DHA content
The refining adsorbent in the step 2 comprises the following components in percentage by weight: hydrophobic silica gel: 200-500 meshes, 40 parts; hydrophobic silica gel: 28 parts of 100-200 meshes; hydrophobic silica gel: 60-100 meshes, 32 parts.
Comparative example:
the difference from the example 1 is that the deodorization and decoloration treatment of the fish oil in the step 3 of the comparative example is to perform deodorization and decoloration 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.
Table 1 shows the change in fish oil quality before and after refining in examples
Figure BDA0001964907450000101
According to the data, the deep sea fish oil prepared by the process technology meets the national first-level standard; the DHA content in the fish oil before refining is 12%, while the DHA content in the fish oil after refining is more than 36%, and the DHA content is more than 3 times higher than that of common fish oil, so the fish oil can be directly applied to health care products and infant food.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.

Claims (6)

1. A processing technology of deep sea fish oil with high DHA content is characterized by comprising the following steps: step 1, alkali refining the pretreated fish oil; step 2, carrying out adsorption treatment on the alkali-refined fish oil by using a refining adsorbent; step 3, separating the fish oil subjected to adsorption treatment by using cascade fractionation equipment; step 4, finally, freezing the graded fish oil, and filtering to obtain the deep sea fish oil with high DHA content; the refining adsorbent in the step 2 comprises the following components in percentage by weight: 200-500 mesh hydrophobic silica gel: 30-55 percent; 100-200 mesh hydrophobic silica gel: 20 to 35 percent; 60-100 mesh hydrophobic silica gel: 25 to 35 percent; the specific operation of the step 2 is as follows:
introducing the alkali refined fish oil obtained in the step 1 into a refining kettle, keeping the temperature in the kettle not to exceed 80 ℃ at normal pressure; adding a refining adsorbent into a refining kettle, and stirring while adding the refining adsorbent; the refining time is 30-60 min, the refining process is uniformly stirred, and the stirring speed is controlled to be 2500-3500 r/h; and filtering and separating the refining adsorbent by using an oil filter with the diameter of 2-3 mu m.
2. The process for processing the deep sea fish oil with high DHA content according to claim 1, wherein the deep sea fish oil with high DHA content is prepared by the following steps: the weight ratio of the refining adsorbent to the fish oil is 2-5%.
3. The process for processing the deep sea fish oil with high DHA content according to claim 1, wherein the deep sea fish oil with high DHA content is prepared by the following steps: the specific operation of the step 1 is as follows:
introducing the fish oil into an alkali treatment tank, starting a stirrer, and controlling the stirring speed at 200-300 r/h; starting steam to heat, spraying a 15% sodium hydroxide aqueous solution when the temperature reaches 70 ℃, keeping the stirring speed at 200-300 r/h and the temperature at 75 +/-5 ℃, and stirring for 0.25-0.5 h; and after stirring, reducing the temperature to 40-60 ℃, standing for 3-5 h, and performing oil-water separation.
4. The process for processing the deep sea fish oil with high DHA content according to claim 1, wherein the deep sea fish oil with high DHA content is prepared by the following steps: the specific operation of step 3 is as follows:
s1, introducing the fish oil refined in the step 2 into a degassing tank, and degassing;
s2, after the foam in the degassing tank is eliminated, starting a feed pump at the rotating speed of 60r/min after degassing is finished, so that the fish oil enters a primary cooling tower, the temperature in the primary cooling tower is 100 plus 120 ℃, and after stable material transportation is carried out for 0.25-1 h, pumping the fish oil distillate in the primary cooling tower into a secondary cooling tower; the temperature in the secondary cooling tower is 105-130 ℃; after the material is stably fed for 0.25-1 h; pumping the fish oil distillate in the secondary cooling tower into a tertiary cooling tower; thus, the fish oil sequentially passes through one-eight stages of cooling towers to be fractionated step by step, the temperature in the towers is increased gradually at 5-10 ℃, and the stable material conveying time is 0.25-1 h;
s3, temporarily storing the fish oil processed in the step S2 in a buffer tank.
5. The process for processing the deep sea fish oil with high DHA content according to claim 1, wherein the deep sea fish oil with high DHA content is prepared by the following steps: the specific operation of the step 4 is as follows:
and (3) introducing the fish oil obtained in the step (3) into a crystallizing tank, starting a refrigerator, cooling to the temperature of-5-3 ℃, allowing the fish oil to enter the crystallizing tank, standing for 20-35 hours, pumping the mixed oil subjected to freezing crystallization into a horizontal blade filter, filtering, and removing wax and ester in the oil to obtain the refined deep sea fish oil with high DHA content.
6. The process for processing the deep sea fish oil with high DHA content according to claim 1, wherein the deep sea fish oil with high DHA content is prepared by the following steps: the mass ratio of the fish oil in the step 1 to the sodium hydroxide aqueous solution with the mass concentration of 15% is 1: 35-55.
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