CN107446693B - Method for extracting grease by ultrasonic-vapor-liquid coexisting state ethanol fluid - Google Patents

Method for extracting grease by ultrasonic-vapor-liquid coexisting state ethanol fluid Download PDF

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CN107446693B
CN107446693B CN201710816528.XA CN201710816528A CN107446693B CN 107446693 B CN107446693 B CN 107446693B CN 201710816528 A CN201710816528 A CN 201710816528A CN 107446693 B CN107446693 B CN 107446693B
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liquid
extraction
temperature
reaction kettle
ultrasonic
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CN201710816528.XA
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Chinese (zh)
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CN107446693A (en
Inventor
刘义军
张帆
李积华
陈民
刘洋洋
周延德
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中国热带农业科学院农产品加工研究所
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING (PRESSING, EXTRACTION), REFINING AND PRESERVING FATS, FATTY SUBSTANCES (e.g. LANOLIN), FATTY OILS AND WAXES, INCLUDING EXTRACTION FROM WASTE MATERIALS; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • C11B1/04Pretreatment of vegetable raw material
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING (PRESSING, EXTRACTION), REFINING AND PRESERVING FATS, FATTY SUBSTANCES (e.g. LANOLIN), FATTY OILS AND WAXES, INCLUDING EXTRACTION FROM WASTE MATERIALS; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting
    • C11B1/106Production of fats or fatty oils from raw materials by extracting using ultra-sounds
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING (PRESSING, EXTRACTION), REFINING AND PRESERVING FATS, FATTY SUBSTANCES (e.g. LANOLIN), FATTY OILS AND WAXES, INCLUDING EXTRACTION FROM WASTE MATERIALS; ESSENTIAL OILS; PERFUMES
    • C11B3/00Refining fats or fatty oils
    • C11B3/001Refining fats or fatty oils by a combination of two or more of the means hereafter
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING (PRESSING, EXTRACTION), REFINING AND PRESERVING FATS, FATTY SUBSTANCES (e.g. LANOLIN), FATTY OILS AND WAXES, INCLUDING EXTRACTION FROM WASTE MATERIALS; ESSENTIAL OILS; PERFUMES
    • C11B3/00Refining fats or fatty oils
    • C11B3/008Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING (PRESSING, EXTRACTION), REFINING AND PRESERVING FATS, FATTY SUBSTANCES (e.g. LANOLIN), FATTY OILS AND WAXES, INCLUDING EXTRACTION FROM WASTE MATERIALS; ESSENTIAL OILS; PERFUMES
    • C11B3/00Refining fats or fatty oils
    • C11B3/16Refining fats or fatty oils by mechanical means

Abstract

The invention discloses a method for extracting grease by ultrasonic-vapor-liquid coexisting state ethanol fluid. The method comprises the steps of drying and crushing nuts at low temperature in vacuum, adding sodium chloride into a system by taking ethanol as a solvent, and realizing oil extraction of nut raw materials by combining an ultrasonic technology; the method ensures that the ethanol is always in a vapor-liquid mixed state in the extraction process by accurately controlling the heating temperature, the feed liquid temperature and the pressure of a reaction system in the extraction process, greatly improves the solubility of the ethanol to the grease, and thus obtains higher extraction efficiency and extraction yield; compared with other traditional squeezing methods, solvent extraction methods and extraction methods, the method has the advantages of lower extraction temperature, less side reaction, high extraction yield, high oil quality, no toxicity, no solvent residue, low production cost and the like.

Description

Method for extracting grease by ultrasonic-vapor-liquid coexisting state ethanol fluid

Technical Field

The invention relates to a method for extracting grease, in particular to a method for extracting grease by ultrasonic-vapor-liquid coexisting state ethanol fluid, belonging to the technical field of organic matter extraction.

Background

The nuts are rich in protein, oil, mineral substances and vitamins, and are food with excellent effects of growing and developing human bodies, strengthening physique and preventing diseases, the fat content of the nuts can reach over 58.8 percent, and the nuts can be directly used in the fields of food, daily chemicals and the like by extracting the oil from the nuts.

The extraction method of nut oil is commonly compression, solvent extraction, subcritical extraction, supercritical extraction and other methods. In the existing extraction method, in order to obtain higher oil yield, gasoline, normal hexane, isopropanol, liquefied gas, methane and the like are used as extraction solvents, and if the extraction solvents are not completely removed, the extraction solvents can remain in oil products, influence the quality of the oil products and bring potential harm; some extraction methods, such as supercritical extraction, require expensive extraction equipment, which increases costs, burdens enterprises, and embarrassment in technical transformation.

Disclosure of Invention

In view of the above-mentioned shortcomings of the prior art, the present invention provides a method for extracting oil from an ultrasonic-vapor-liquid co-existing ethanol fluid.

The technical scheme of the invention is as follows: a method for extracting grease by ultrasonic-vapor-liquid coexisting state ethanol fluid comprises the following steps:

(1) pretreatment of raw materials: removing impurities from nut, and vacuum drying at low temperature until water content is lower than 12%;

(2) crushing raw materials: freezing the dried nutlet to-10 to-20 ℃, and crushing the nutlet to the particle size of 100-300 mu m by using an airflow type superfine crusher, wherein the crushing temperature is controlled to be lower than 90 ℃;

(3) ultrasonic-assisted extraction: mixing the crushed nutlet and ethanol according to the feed-liquid ratio of 1:1-1:15, adding sodium chloride, placing in an ultrasonic reaction kettle, heating the mixed feed liquid in the reaction kettle, and performing ultrasonic-assisted extraction;

wherein a hot water jacketed reaction kettle is adopted in the reaction kettle, and a condenser is arranged at the top of the reaction kettle; the mixed material liquid in the reaction kettle is heated by hot water in the jacket, and the temperature of the hot water in the jacket is controlled by the following gradient steps: firstly, controlling the temperature of hot water to be 90-100 ℃, reducing the temperature of the hot water to be 80-95 ℃ when the temperature of mixed material liquid reaches 70 +/-2 ℃, and controlling the temperature of the mixed material liquid to be 75-90 ℃ by adjusting the entering amount of the hot water;

the ultrasonic-assisted extraction is carried out, the pressure of a reaction system in a reaction kettle is 0.1MPa, the ultrasonic power is 500W-1000W, and the extraction time is 30-120 min;

(4) solid-liquid separation of extract liquid: when the extraction is finished, the heating is stopped, and no condensed liquid drops in a condenser at the top of the reaction kettle, the material liquid is separated, and the method comprises the following specific steps: filtering the extractive solution with 50 μm high pressure filter membrane or passing through tubular centrifuge, performing solid-liquid separation at rotation speed of 18000r/min, cooling the separated liquid to 25-40 deg.C, standing for layering, collecting crude oil layer, decolorizing, and deodorizing to obtain the final product.

Preferably, the vacuum low-temperature drying conditions are as follows: the drying temperature is 50-60 ℃, and the drying time is 10-15 h.

Preferably, the volume concentration of the ethanol is 80-100%.

Preferably, the addition amount of the sodium chloride is 1-5% of the addition amount of the ethanol.

Preferably, in the ultrasonic-assisted extraction process in the step (3), when the temperature in the reaction kettle reaches the azeotropic point of the system, the ethanol starts to evaporate, the vaporous ethanol starts to condense under the action of a condensing device at the top of the reaction kettle and flows back into the kettle, and the water inflow of cold water of the condenser is controlled to be 1-3 Kg/min.

Through years of research, the method has the advantages that when the ethanol is heated to 60-80 ℃, and the ethanol is in a vapor-liquid coexisting state, the fat in the nuts is very strong in solubility in the temperature range, therefore, the method uses the ethanol as an extraction solvent, adopts the treatment conditions of the method, firstly pretreats the nut raw materials, combines an ultrasonic technology, and accurately controls the conditions of heating temperature, extraction temperature (mixture temperature), reaction system pressure and the like, so that the ethanol is always in the vapor-liquid mixed state in the extraction process, and higher grease yield and better grease quality can be obtained. The method is particularly suitable for oil extraction of one or more nut raw materials in oil nuts such as cashew nuts, macadamia nuts, oil-tea camellia seed nuts and the like.

Compared with the prior art, the invention has the following beneficial technical effects:

(1) the nut raw material is dried in vacuum at low temperature, cooled to an embrittlement point, and crushed into particles with smaller particle size under the action of a jet mill, so that the temperature of the material in the mill can be protected to be lower than 100 ℃, the oxidation of the raw material oil and the loss of other nutritional ingredients are reduced, and the edible quality of the oil is improved;

(2) ultrasonic-assisted extraction is adopted, mixing of an extracting agent and an extract is promoted by ultrasonic waves, dissolution of grease is promoted, extraction time is shortened, and extraction efficiency is improved;

(3) the sodium chloride powder is added, so that the azeotropic point of an ethanol-water-sodium chloride mixed system is increased, the solubility of ethanol to grease is increased, the ethanol is changed from a liquid state to a vapor-liquid coexisting state, the boiling point of the vapor-liquid coexisting state is increased, and the solubility of ethanol to grease is greatly improved;

(4) compared with other traditional squeezing methods, the extraction temperature is lower, the reactions such as oxidation and the like of the kernel oil are reduced, the oil quality is improved, and meanwhile, the extraction rate of the oil is higher; by adopting the method for extracting the nut grease, the yield of the crude oil can reach 60-85 percent;

(5) compared with other traditional solvent (gasoline, normal hexane and isopropanol) extraction methods and subcritical extraction methods (liquefied gas, methane and the like), ethanol is used as a solvent, is an edible and nontoxic raw material, has no toxic and harmful solvent residues, and improves the quality of oil;

(6) compared with the supercritical extraction method, the method has the advantages of low equipment investment cost and low cost in the extraction process, and further reduces the production cost of enterprises.

Detailed Description

The present invention is further illustrated in detail by the following examples, which are provided only for illustrating the present invention and are not intended to limit the scope of the present invention.

Example 1 the invention was carried out using the following steps:

(1) pretreatment of raw materials: removing impurities from macadimia nut kernels, and drying in vacuum at low temperature until the water content is lower than 12%; the adopted vacuum low-temperature drying conditions are as follows: the drying temperature is 50-60 ℃, and the drying time is 12 h;

(2) crushing raw materials: freezing the dried nutlet to-10 deg.C, and pulverizing the nutlet to 200 μm with an air-flow type micronizer at a temperature below 90 deg.C;

(3) ultrasonic-assisted extraction: mixing the crushed nutlet and 90% ethanol according to a feed-liquid ratio of 1:10, adding 2.5% of sodium chloride powder, placing the mixture in an ultrasonic reaction kettle, heating the mixed feed liquid in the reaction kettle, and performing ultrasonic-assisted extraction;

wherein a hot water jacketed reaction kettle is adopted in the reaction kettle, and a condenser is arranged at the top of the reaction kettle; the mixed material liquid in the reaction kettle is heated by hot water in the jacket, and the temperature of the hot water in the jacket is controlled by the following gradient steps: firstly, controlling the temperature of hot water to be 90-100 ℃, reducing the temperature of the hot water to be 80-95 ℃ when the temperature of mixed material liquid reaches 70 +/-2 ℃, and controlling the temperature of the mixed material liquid to be 75-90 ℃ by adjusting the entering amount of the hot water;

an ultrasonic-assisted extraction process is carried out, wherein the pressure of a reaction system in a reaction kettle is controlled to be 0.1MPa, the ultrasonic power is controlled to be 800W, and the extraction time is 90 min;

in the ultrasonic-assisted extraction process in the step (3), when the temperature in the reaction kettle reaches the azeotropic point of the system, ethanol begins to evaporate, vaporous ethanol begins to condense under the action of a condensing device at the top of the reaction kettle and flows back into the reaction kettle, and the water inflow of cold water of a condenser is controlled to be 1-3 kg/min;

(4) solid-liquid separation of extract liquid: when the extraction is finished, the heating is stopped, and no condensed liquid drops in a condenser at the top of the reaction kettle, the material liquid is separated, and the method comprises the following specific steps: filtering the extractive solution with 50 μm high pressure filter membrane or passing through tubular centrifuge, performing solid-liquid separation at rotation speed of 18000r/min, cooling the separated liquid to 25-40 deg.C, standing for layering, collecting oil layer to obtain crude oil, decolorizing and deodorizing the crude oil to obtain finished oil with extraction rate of 75.24%.

Example 2 the invention was carried out using the following steps:

(1) pretreatment of raw materials: removing impurities from macadimia nut kernels, and drying in vacuum at low temperature until the water content is lower than 12%; the adopted vacuum low-temperature drying conditions are as follows: the drying temperature is 50-60 ℃, and the drying time is 15 h;

(2) crushing raw materials: freezing the dried nutlet to-20 deg.C, and pulverizing the nutlet to 300 μm with an air-flow type micronizer at a temperature below 90 deg.C;

(3) ultrasonic-assisted extraction: mixing the crushed nutlet and 80 vol% ethanol according to a material-liquid ratio of 1:15, adding 5 vol% sodium chloride powder, placing in an ultrasonic reaction kettle, heating the mixed material liquid in the reaction kettle, and performing ultrasonic-assisted extraction;

wherein a hot water jacketed reaction kettle is adopted in the reaction kettle, and a condenser is arranged at the top of the reaction kettle; the mixed material liquid in the reaction kettle is heated by hot water in the jacket, and the temperature of the hot water in the jacket is controlled by the following gradient steps: firstly, controlling the temperature of hot water to be 90-100 ℃, reducing the temperature of the hot water to be 80-95 ℃ when the temperature of mixed material liquid reaches 70 +/-2 ℃, and controlling the temperature of the mixed material liquid to be 75-90 ℃ by adjusting the entering amount of the hot water;

an ultrasonic-assisted extraction process is carried out, wherein the pressure of a reaction system in a reaction kettle is controlled to be 0.1MPa, the ultrasonic power is 1000W, and the extraction time is 120 min;

in the ultrasonic-assisted extraction process in the step (3), when the temperature in the reaction kettle reaches the azeotropic point of the system, ethanol begins to evaporate, vaporous ethanol begins to condense under the action of a condensing device at the top of the reaction kettle and flows back into the reaction kettle, and the water inflow of cold water of a condenser is controlled to be 1-3 kg/min;

(4) solid-liquid separation of extract liquid: when the extraction is finished, the heating is stopped, and no condensed liquid drops in a condenser at the top of the reaction kettle, the material liquid is separated, and the method comprises the following specific steps: filtering the extractive solution with 50 μm high pressure filter membrane or passing through tubular centrifuge, performing solid-liquid separation at rotation speed of 18000r/min, cooling the separated liquid to 25-40 deg.C, standing for layering, collecting oil layer to obtain crude oil, decolorizing and deodorizing the crude oil to obtain oil product with extraction rate of 82.4%.

Example 3 the invention was carried out using the following steps:

(1) pretreatment of raw materials: removing impurities from cashew nut, and vacuum drying at low temperature until the water content is lower than 12%; the adopted vacuum low-temperature drying conditions are as follows: the drying temperature is 50-60 ℃, and the drying time is 15 h;

(2) crushing raw materials: freezing the dried nutlet to-15 deg.C, and pulverizing the nutlet to 100 μm with an air-flow type micronizer at a temperature below 90 deg.C;

(3) ultrasonic-assisted extraction: mixing the crushed nutlet and 85 vol% ethanol according to a material-liquid ratio of 1:1, adding sodium chloride powder with the addition of 1 vol% of ethanol, placing the mixture in an ultrasonic reaction kettle, heating the mixed material liquid in the reaction kettle, and performing ultrasonic-assisted extraction;

wherein a hot water jacketed reaction kettle is adopted in the reaction kettle, and a condenser is arranged at the top of the reaction kettle; the mixed material liquid in the reaction kettle is heated by hot water in the jacket, and the temperature of the hot water in the jacket is controlled by the following gradient steps: firstly, controlling the temperature of hot water to be 90-100 ℃, reducing the temperature of the hot water to be 80-95 ℃ when the temperature of mixed material liquid reaches 70 +/-2 ℃, and controlling the temperature of the mixed material liquid to be 75-90 ℃ by adjusting the entering amount of the hot water;

an ultrasonic-assisted extraction process is carried out, wherein the pressure of a reaction system in a reaction kettle is controlled to be 0.1MPa, the ultrasonic power is controlled to be 500W, and the extraction time is controlled to be 30 min;

in the ultrasonic-assisted extraction process in the step (3), when the temperature in the reaction kettle reaches the azeotropic point of the system, ethanol begins to evaporate, vaporous ethanol begins to condense under the action of a condensing device at the top of the reaction kettle and flows back into the reaction kettle, and the water inflow of cold water of a condenser is controlled to be 1-3 kg/min;

(4) solid-liquid separation of extract liquid: when the extraction is finished, the heating is stopped, and no condensed liquid drops in a condenser at the top of the reaction kettle, the material liquid is separated, and the method comprises the following specific steps: filtering the extractive solution with 50 μm high pressure filter membrane or passing through tubular centrifuge, performing solid-liquid separation at rotation speed of 18000r/min, cooling the separated liquid to 25-40 deg.C, standing for layering, collecting oil layer to obtain crude oil, decolorizing and deodorizing the crude oil to obtain oil product with extraction yield of 70.02%.

Claims (2)

1. A method for extracting grease by ultrasonic-vapor-liquid coexisting state ethanol fluid is characterized by comprising the following steps of: the method comprises the following steps:
(1) pretreatment of raw materials: removing impurities from nut, and vacuum drying at low temperature until water content is lower than 12%;
(2) crushing raw materials: freezing the dried nutlet to-10 to-20 ℃, and crushing the nutlet to the particle size of 100-300 mu m by using an airflow type superfine crusher, wherein the crushing temperature is controlled to be lower than 90 ℃;
(3) ultrasonic-assisted extraction: mixing the crushed nutlet and ethanol according to the feed-liquid ratio of 1:1-1:15, adding sodium chloride, placing in an ultrasonic reaction kettle, heating the mixed feed liquid in the reaction kettle, and performing ultrasonic-assisted extraction;
wherein a hot water jacketed reaction kettle is adopted in the reaction kettle, and a condenser is arranged at the top of the reaction kettle; the mixed material liquid in the reaction kettle is heated by hot water in the jacket, and the temperature of the hot water in the jacket is controlled by the following gradient steps: firstly, controlling the temperature of hot water to be 90-100 ℃, adjusting the temperature of the hot water to be 80-95 ℃ when the temperature of the mixed material liquid reaches 70 +/-2 ℃, and controlling the temperature of the mixed material liquid to be 75-90 ℃ by adjusting the entering amount of the hot water;
the ultrasonic-assisted extraction is carried out, the pressure of a reaction system in a reaction kettle is 0.1MPa, the ultrasonic power is 500W-1000W, and the extraction time is 30-120 min;
(4) solid-liquid separation of extract liquid: when the extraction is finished, the heating is stopped, and no condensed liquid drops in a condenser at the top of the reaction kettle, the material liquid is separated, and the method comprises the following specific steps: filtering the extractive solution with 50 μm high pressure filter membrane or passing through tubular centrifuge, performing solid-liquid separation at rotation speed of 18000r/min, cooling the separated liquid to 25-40 deg.C, standing for layering, collecting oil layer to obtain crude oil, decolorizing and deodorizing the crude oil to obtain oil product;
in the ultrasonic-assisted extraction process in the step (3), when the temperature in the reaction kettle reaches the azeotropic point of the system, the ethanol begins to evaporate, the vaporous ethanol begins to condense under the action of a condensing device at the top of the reaction kettle and flows back into the reaction kettle, and the water inflow of cold water of a condenser is controlled to be 1-3 Kg/min;
the vacuum low-temperature drying conditions are as follows: drying at 50-60 deg.C for 10-15 h;
the volume concentration of the ethanol is 80-90%.
2. The method of claim 1, wherein: the addition amount of the sodium chloride is 1-5% of the addition amount of the ethanol.
CN201710816528.XA 2017-09-12 2017-09-12 Method for extracting grease by ultrasonic-vapor-liquid coexisting state ethanol fluid CN107446693B (en)

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