CN112457912A - Hazelnut oil reinforced supercritical CO2Extraction method - Google Patents
Hazelnut oil reinforced supercritical CO2Extraction method Download PDFInfo
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- CN112457912A CN112457912A CN202011224238.4A CN202011224238A CN112457912A CN 112457912 A CN112457912 A CN 112457912A CN 202011224238 A CN202011224238 A CN 202011224238A CN 112457912 A CN112457912 A CN 112457912A
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- hazelnut
- treatment
- supercritical
- pressure
- hazelnut kernel
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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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
Abstract
The invention discloses a hazelnut oil reinforced supercritical CO2The extraction method comprises the following steps: s1, shelling the hazelnut kernel, freezing and embrittling the hazelnut kernel for 1-3 hours at the temperature of-18 ℃, performing ultrasonic wall breaking treatment at the temperature of 30-40 ℃ to obtain hazelnut kernel powder, and drying the hazelnut kernel powder for later use; s2, mixing the dried hazelnut kernel powder with an entrainer, and performing instantaneous high-pressure treatment by an ultrahigh-pressure homogenizer, wherein the pressure is adjusted to be 100-200 MPa, the treatment is performed for 2-3 times in a circulating manner, the treatment flow rate is 5-8L/h, and the temperature is 20-30 ℃; s3, introducing the solution subjected to instantaneous high-pressure treatment into an extraction kettle, and performing supercritical CO2Extracting, and collecting the extract. The invention obviously improves the extraction rate of hazelnut oil by the mode of ultrasonic wall breaking treatment in cooperation with instantaneous high-pressure treatment, and the extraction rate can reach about 93.7 percent.
Description
Technical Field
The invention relates to the field of extraction of hazelnut oil, and particularly relates to hazelnut oil-reinforced supercritical CO2An extraction method.
Background
The hazelnut oil is a functional edible oil with great development prospect. At present, the existing extraction methods of hazelnut oil mainly comprise a squeezing method, an organic solvent leaching method, a supercritical CO2 extraction method and the like. The supercritical CO2 extraction method adopts carbon dioxide as a solvent, has the advantages of simple process, short production period, no solvent residue in the product, mild operation conditions, no damage to the activity of unsaturated fatty acid and protein and the like, and is suitable for industrial production.
Disclosure of Invention
The invention aims to provide hazelnut oil reinforced supercritical CO2The extraction method remarkably improves the extraction rate of hazelnut oil.
In order to achieve the purpose, the invention adopts the technical scheme that:
hazelnut oil reinforced supercritical CO2The extraction method comprises the following steps:
s1, shelling the hazelnut kernel, freezing and embrittling the hazelnut kernel for 1-3 hours at the temperature of-18 ℃, performing ultrasonic wall breaking treatment at the temperature of 30-40 ℃ to obtain hazelnut kernel powder, and drying the hazelnut kernel powder for later use;
s2, mixing the dried hazelnut kernel powder with an entrainer, and performing instantaneous high-pressure treatment by an ultrahigh-pressure homogenizer, wherein the pressure is adjusted to be 100-200 MPa, the treatment is performed for 2-3 times in a circulating manner, the treatment flow rate is 5-8L/h, and the temperature is 20-30 ℃;
s3, introducing the solution subjected to instantaneous high-pressure treatment into an extraction kettle, and performing supercritical CO2Extracting, and collecting the extract.
Further, in the step S1, the particle size of the hazelnut kernel powder is 40-60 meshes.
Further, in step S1, the conditions for breaking the wall by ultrasonic waves are as follows: the ultrasonic frequency is 20-25 KHZ, the time is 10-15 min, and the rotating speed is 20-50 rpm.
Further, in the step S2, the entrainer is 15% ethyl acetate, and the weight ratio of the entrainer to the hazelnut kernel powder is 3: 100.
Further, in the step S3, supercritical CO2The extraction temperature is 35-40 ℃, and the pressure is 20-25 MPa.
Further, in the step S3, CO2 The flow rate is 18-22L/h.
The invention has the following beneficial effects:
the extraction rate of the hazelnut oil is obviously improved by the mode of ultrasonic wall breaking treatment in cooperation with instantaneous high-pressure treatment, and can reach about 93.7%.
Detailed Description
In order that the objects and advantages of the invention will be more clearly understood, the invention is further described in detail below with reference to examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
Hazelnut oil reinforced supercritical CO2The extraction method comprises the following steps:
s1, shelling the hazelnut kernel, freezing and embrittling the hazelnut kernel for 1 hour at the temperature of-18 ℃, performing ultrasonic wall breaking treatment at the temperature of 40 ℃ to obtain hazelnut kernel powder, sieving the hazelnut kernel powder with a 40-mesh sieve, and drying the hazelnut kernel powder for later use;
s2, mixing the dried hazelnut kernel powder with an entrainer, and performing instantaneous high-pressure treatment by an ultrahigh-pressure homogenizer, wherein the pressure is adjusted to be 100 MPa, the circulation treatment is performed for 3 times, the treatment flow rate is 5L/h, and the temperature is 30 ℃; wherein the entrainer is 15% ethyl acetate, and the weight ratio of the entrainer to the hazelnut kernel powder is 3: 100;
s3, introducing the solution subjected to instantaneous high-pressure treatment into an extraction kettle, and performing supercritical CO2Extracting, and collecting the extract.
In this embodiment, the conditions for breaking the wall by ultrasonic waves are as follows: the ultrasonic frequency is 20 KHZ, the time is 15min, and the rotating speed is 35 rpm.
In this example, supercritical CO2The extraction temperature is 35 ℃, the pressure is 20MPa, and CO is2 The flow rate was 20L/h.
Example 2
Hazelnut oil reinforced supercritical CO2The extraction method comprises the following steps:
s1, shelling the hazelnut kernel, freezing and embrittling the hazelnut kernel for 3 hours at the temperature of-18 ℃, performing ultrasonic wall breaking treatment at the temperature of 30 ℃ to obtain hazelnut kernel powder, sieving the hazelnut kernel powder with a 60-mesh sieve, and drying the hazelnut kernel powder for later use;
s2, mixing the dried hazelnut kernel powder with an entrainer, and performing instantaneous high-pressure treatment by an ultrahigh-pressure homogenizer, wherein the pressure is adjusted to 200 MPa, the circulation treatment is performed for 2 times, the treatment flow rate is 8L/h, and the temperature is 20 ℃; wherein the entrainer is 15% ethyl acetate, and the weight ratio of the entrainer to the hazelnut kernel powder is 3: 100;
s3, introducing the solution subjected to instantaneous high-pressure treatment into an extraction kettle, and performing supercritical CO2Extracting, and collecting the extract.
In this embodiment, the conditions for breaking the wall by ultrasonic waves are as follows: the ultrasonic frequency is 25 KHZ, the time is 10min, and the rotating speed is 50 rpm.
In this example, supercritical CO2The extraction temperature is 40 ℃, the pressure is 25MPa, and CO is added2 The flow rate was 18L/h.
Example 3
Hazelnut oil reinforced supercritical CO2The extraction method comprises the following steps:
s1, shelling the hazelnut kernel, freezing and embrittling the hazelnut kernel for 2 hours at the temperature of-18 ℃, performing ultrasonic wall breaking treatment at the temperature of 35 ℃ to obtain hazelnut kernel powder, sieving the hazelnut kernel powder with a 50-mesh sieve, and drying the hazelnut kernel powder for later use;
s2, mixing the dried hazelnut kernel powder with an entrainer, and performing instantaneous high-pressure treatment by an ultrahigh-pressure homogenizer, wherein the pressure is adjusted to be 150 MPa, the circulation treatment is performed for 2 times, the treatment flow rate is 6L/h, and the temperature is 25 ℃; wherein the entrainer is 15% ethyl acetate, and the weight ratio of the entrainer to the hazelnut kernel powder is 3: 100;
s3, introducing the solution subjected to instantaneous high-pressure treatment into an extraction kettle, and performing supercritical CO2Extracting, and collecting the extract.
In this embodiment, the conditions for breaking the wall by ultrasonic waves are as follows: the ultrasonic frequency is 22 KHZ, the time is 12min, and the rotating speed is 35 rpm.
In this example, supercritical CO2The extraction temperature is 37 ℃, the pressure is 22MPa, and CO is added2 The flow rate was 20L/h.
Comparative example 1
Mixing the dried semen Coryli Heterophyllae powder with entrainer, directly introducing into extraction kettle, and performing supercritical CO extraction2The extraction was carried out, and the extract was collected, and the rest of the procedure was the same as in example 1.
Comparative example 2
The hazelnut kernel was directly pulverized to 60 mesh after shelling, and dried, and the rest was the same as example 2.
Comparative example 3
The procedure of example 3 was followed except that the hazelnut kernel was dehulled, directly pulverized to 60 mesh, dried, mixed with entrainer, and then directly introduced into the extraction vessel for supercritical CO2 extraction and the extract was collected.
The extraction rate of the hazelnut oil of the examples 1 to 3 and the comparative examples 1 to 3 is tested, and the physical and chemical indexes of the hazelnut oil obtained in the examples 1 to 3 are simultaneously determined, wherein: the acid value refers to GB 5009.229-2016 (determination of acid value in food safety national standard food); the fatty acid was measured according to GB 5009.168-2016 (national food safety Standard) for fatty acid measurement.
And (3) detection results: example 1: the extraction rate of hazelnut oil reached 93.1%, the acid value (KOH) was 0.53mg/g, no significant change in fatty acid composition occurred, and no trans-fatty acid was detected.
Example 2: the extraction rate of hazelnut oil reached 93.3%, the acid value (KOH) was 0.51mg/g, no significant change in fatty acid composition occurred, and no trans-fatty acid was detected.
Example 3: the extraction rate of hazelnut oil reached 93.7%, the acid value (KOH) was 0.55mg/g, no significant change in fatty acid composition occurred, and no trans-fatty acid was detected.
Comparative example 1: the extraction rate of hazelnut oil reaches 90.7 percent.
Comparative example 2: the extraction rate of hazelnut oil reaches 91.2 percent.
Comparative example 3: the extraction rate of hazelnut oil reaches 88.3 percent.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be construed as the protection scope of the present invention.
Claims (6)
1. Hazelnut oil reinforced supercritical CO2The extraction method is characterized by comprising the following steps:
s1, shelling the hazelnut kernel, freezing and embrittling the hazelnut kernel for 1-3 hours at the temperature of-18 ℃, performing ultrasonic wall breaking treatment at the temperature of 30-40 ℃ to obtain hazelnut kernel powder, and drying the hazelnut kernel powder for later use;
s2, mixing the dried hazelnut kernel powder with an entrainer, and performing instantaneous high-pressure treatment by an ultrahigh-pressure homogenizer, wherein the pressure is adjusted to be 100-200 MPa, the treatment is performed for 2-3 times in a circulating manner, the treatment flow rate is 5-8L/h, and the temperature is 20-30 ℃;
s3, introducing the solution subjected to instantaneous high-pressure treatment into an extraction kettle, and performing supercritical CO2Extracting, and collecting the extract.
2. The hazelnut oil-enhanced supercritical CO of claim 12The extraction method is characterized in that in the step S1, the particle size of the hazelnut kernel powder is 40-60 meshes.
3. The hazelnut oil-enhanced supercritical CO of claim 12The extraction method is characterized in that in the step S1, the conditions of ultrasonic wall breaking are as follows: the ultrasonic frequency is 20-25 KHZ, the time is 10-15 min, and the rotating speed is 20-50 rpm.
4. The hazelnut oil-enhanced supercritical CO of claim 12The extraction method is characterized in that in the step S2, the entrainer is 15% ethyl acetate, and the weight ratio of the entrainer to the hazelnut kernel powder is 3: 100.
5. The hazelnut oil-enhanced supercritical CO of claim 12The extraction method is characterized in that in the step S3, supercritical CO is adopted2The extraction temperature is 35-40 ℃, and the pressure is 20-25 MPa.
6. The hazelnut oil-enhanced supercritical CO of claim 12The extraction method is characterized in that in the step S3, CO2 The flow rate is 18-22L/h.
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