CN108325581B - Comprehensive utilization process of flaxseeds - Google Patents

Comprehensive utilization process of flaxseeds Download PDF

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CN108325581B
CN108325581B CN201810124841.1A CN201810124841A CN108325581B CN 108325581 B CN108325581 B CN 108325581B CN 201810124841 A CN201810124841 A CN 201810124841A CN 108325581 B CN108325581 B CN 108325581B
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flaxseed
flaxseeds
extracting
shells
drying
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CN108325581A (en
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兴丽
赵庆亮
曹有福
王梅
刘威
张小燕
李少萍
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Chinese Academy of Agricultural Mechanization Sciences
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02B—PREPARING GRAIN FOR MILLING; REFINING GRANULAR FRUIT TO COMMERCIAL PRODUCTS BY WORKING THE SURFACE
    • B02B1/00—Preparing grain for milling or like processes
    • B02B1/02—Dry treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02B—PREPARING GRAIN FOR MILLING; REFINING GRANULAR FRUIT TO COMMERCIAL PRODUCTS BY WORKING THE SURFACE
    • B02B1/00—Preparing grain for milling or like processes
    • B02B1/08—Conditioning grain with respect to temperature or water content
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02B—PREPARING GRAIN FOR MILLING; REFINING GRANULAR FRUIT TO COMMERCIAL PRODUCTS BY WORKING THE SURFACE
    • B02B3/00—Hulling; Husking; Decorticating; Polishing; Removing the awns; Degerming
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02B—PREPARING GRAIN FOR MILLING; REFINING GRANULAR FRUIT TO COMMERCIAL PRODUCTS BY WORKING THE SURFACE
    • B02B7/00—Auxiliary devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
    • B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
    • B07B9/00—Combinations of apparatus for screening or sifting or for separating solids from solids using gas currents; General arrangement of plant, e.g. flow sheets
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Peptides Or Proteins (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention belongs to the technical field of deep processing of agricultural products, and particularly relates to a comprehensive utilization process of flaxseeds. According to the comprehensive utilization process of flaxseeds, the flaxseeds are subjected to shelling treatment and shell-kernel separation treatment, and the collected flaxseed shells and flaxseed kernels are respectively subjected to effective component extraction, so that the quality and extraction rate of flaxseed gum and lignans in the flaxseed shells and the quality and extraction rate of flaxseed oil and flaxseed protein in the flaxseed kernels are further improved. The method can realize comprehensive and high-efficiency utilization of the flaxseeds, can drive the healthy and high-value development of the industry, can obtain active ingredients with higher economic value, and further realizes the development of flaxseed active substance functional products.

Description

Comprehensive utilization process of flaxseeds
Technical Field
The invention belongs to the technical field of deep processing of agricultural products, and particularly relates to a comprehensive utilization process of flaxseeds.
Background
Linum, the linum linnaceae, is one of the oldest crops, produced mainly in china, canada, argentina, india and the united states. The annual total yield of linseed oil worldwide is more than 200 million tons at present, and the 7 th bit of the world total oil yield is occupied. Flax is mainly produced in places such as Heilongjiang, Shanxi, Hebei, inner Mongolia, Xinjiang, Gansu, Ningxia and the like in China, and the planting area and the total yield of the flax in China are second to Canada and second in the world.
Flax is rich in various nutrients, such as protein, polysaccharide, unsaturated fatty acid, lignan, etc. In north america and europe, flaxseed is often used in various bakery products for direct consumption or is developed as edible grade flaxseed oil. But the utilization of the whole flaxseed product is relatively simple and the production cost is high. In the aspect of comprehensive utilization research of flaxseeds in China, the method mainly comprises the steps of squeezing of flaxseed oil and utilization of animal feed, functional products such as flaxseed protein powder, flaxseed gum and the like only reach the crude level, the added value is low, the flaxseeds are mostly used as food additives, and the potential value of the flaxseeds cannot be fully developed.
In recent years, as the bioactive components in flaxseed have been discovered and recognized by researchers, the flaxseed processing industry has been gradually developed. At present, two main approaches are available for improving the nutrient utilization rate of flaxseeds: firstly, linseed oil is mainly extracted, cake meal is recycled, the preparation process is mainly established on the traditional pressing method and leaching method, and the protein residue is obtained by viscosity removal and detoxification treatment and is directly used as ruminant feed, but the overall utilization rate is not high; the other way is to separate or respectively enrich the flaxseed gum, the flaxseed oil, the flaxseed protein and the flaxseed hull part contained in the flaxseed by different processes according to the distribution of each component in the flaxseed and the characteristics of the flaxseed structure, and then respectively recover and utilize the flaxseed gum, the flaxseed oil, the flaxseed protein and the flaxseed hull part by proper processes. The method gives consideration to the nutrition and the biological activity of different active ingredients, is more favorable for the digestion and the utilization of various nutrient components and the reasonable exertion of the efficacy, and becomes a basic idea for the comprehensive utilization of the flaxseeds at home and abroad. However, there is still no systematic study on the specific operation, the extraction process of each nutrient and the separation sequence of kernel and shell. The reason is that the problem of flaxseed dehulling is difficult to break through, and therefore, various bioactive components respectively existing in flaxseed hulls and kernels are difficult to extract, process and apply efficiently, the development of the flaxseed industry is limited, and the flaxseed in China has the problems of single processing mode, low processing level, low utilization rate of the active components and the like in the aspect of processing and utilization, and cannot be comprehensively processed and utilized.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to provide a comprehensive utilization process of flaxseeds, which effectively solves the problem of flaxseed dehulling and the problem of low comprehensive utilization rate of flax seeds in the prior art.
In order to solve the technical problems, the comprehensive utilization process of flaxseeds comprises the following steps:
(1) drying flaxseeds and dehulling the flaxseeds;
(2) carrying out shell-kernel separation treatment on the flaxseeds after shelling by adopting a mode of combining air separation and screening;
(3) respectively extracting the active ingredients of the collected linseed shells and linseed kernels.
In the step (1), the drying step is hot air drying until the moisture content of the flaxseeds is 3.0-5.0%; and the shelling step is to continuously shell by adopting a friction and collision combined mode.
In the step (2), the flaxseed shell and kernel separation treatment step is a combination of air separation and screening:
the air separation step is that the flaxseed shells are separated from the flaxseed shell mixture through a fan, and the separated flaxseed shells enter a collection device;
and in the screening step, the mixture of the flaxseed kernels, the flaxseeds and the residual flaxseed husks passes through a vibrating screen and is separated by the vibrating screen with the size suitable for the flaxseed kernels, the flaxseeds and the flaxseed husks.
In the winnowing step, the wind speed of the fan is controlled to be 5-20 m/s;
in the screening step, the rotating speed of the vibrating screen is controlled to be 200-400 r/min.
The vibrating screen comprises three screens with the screen mesh sizes of 5.0mm multiplied by 2.0mm, 4.0mm multiplied by 1.5mm and 3.0mm multiplied by 0.9mm respectively.
In the step (1), the method further comprises the step of classifying and screening the flaxseeds according to the sizes by using a screen with the screen hole size of (4.0-6.0) mm x (1.0-3.0) mm.
In the step (3), the active ingredient extraction step comprises a step of extracting flaxseed gum and lignans from flaxseed shells and a step of extracting linseed oil fatty acids and flax proteins from flaxseed kernels.
The steps for extracting the flaxseed gum and the lignans from the flax shells comprise:
extracting the collected flaxseed shells with water under vacuum condition at temperature below 100 deg.C under extraction pressure of 0.07-0.09MPa to obtain flaxseed gum solution, and vacuum drying to obtain flaxseed gum;
adding ethanol solution into the residue after extracting flaxseed gum, extracting at 40-50 deg.C, collecting the extractive solution, drying, adding cellulase, and performing enzymolysis to obtain lignan.
The ethanol is 50-70% of ethanol by mass concentration, and the concentration of the cellulase is 0.02-0.04 mu g/L
The steps for extracting the linseed oil fatty acid and the flax protein in the linseed kernels comprise the following steps:
adding petroleum ether into the collected linseed kernels as an extraction solvent, and extracting at 30-60 ℃ under an ultrasonic condition to obtain linseed oil fatty acid;
the power of the ultrasonic extraction step is 120-;
mixing the residue after extracting oleum Lini fatty acid with water, extracting at 50-80 deg.C, performing solid-liquid separation, collecting precipitate, drying, mixing with water, adjusting pH to alkaline, performing solid-liquid separation, collecting supernatant, adjusting pH to neutral, concentrating, and spray drying to obtain flax protein;
in the water extraction step, the liquid-material ratio is controlled to be 20-50mL/g, the vibration extraction is carried out for 70-100min at the temperature of 50-80 ℃, the centrifugation is carried out for 15-20min at 4000r/min of 2500-.
The comprehensive utilization process of the flaxseeds also comprises the step of identifying the components contained in the extracted flaxseed oil by infrared spectroscopy.
According to the comprehensive utilization process of flaxseeds, the flaxseeds are subjected to shelling treatment and shell-kernel separation treatment, and the flaxseeds are respectively collected to extract the effective components, so that the extraction rate of flaxseed shell flaxseed gum and lignan and the extraction rate of flaxseed oil and flaxseed protein are further improved. The method can realize comprehensive and high-efficiency utilization of the flaxseeds, can drive the healthy and high-value development of the industry, can obtain active ingredients with higher economic value, and further realizes the development of flaxseed active substance functional products.
Detailed Description
Example 1
The comprehensive utilization process of flaxseeds in this embodiment includes the following steps:
(1) shelling
Screening the purchased flaxseeds without impurities and dust sequentially by using sieves with the sizes (length multiplied by width) of 5.0mm multiplied by 2.0mm, 4.0mm multiplied by 1.5mm and 3.0mm multiplied by 0.9mm respectively to obtain three types of flaxseeds with different sizes, wherein the flaxseeds with the sizes of about 5.2mm multiplied by 2.3mm are selected for testing in the embodiment;
determining the initial water content of the selected semen Lini to be 7.8% by existing method, placing the semen Lini in a drying oven, and drying at 120 deg.C for 25min to obtain semen Lini with water content of 4.3%;
the obtained dried flaxseeds are placed in dehulling equipment for dehulling treatment, the dehulling equipment adopts a flaxseed dehulling and separating device disclosed in Chinese patent CN203530272U, the dehulling mode adopted by the device is a friction and collision combined mode for continuous dehulling, the friction force is realized by a grinding wheel, the shearing force is realized by a gear, and the rotating speed range is 1800-2500 r/min; the device is used for dehulling 200g of dried flaxseeds with the moisture content of 4.3 percent, the revolution speed of dehulling equipment is adjusted to 2200r/min, dehulling is continuously carried out for 4 times, and the dehulling rate is measured to reach 92 percent and the breakage rate is measured to be 3.2 percent.
(2) Separation of shell and kernel
Separating the husked mixture containing flaxseeds (without husking), flaxseed hulls and flaxseed kernels by air separation and screening;
firstly, separating by adopting a winnowing mode, namely, providing power by using a fan, controlling the wind speed of the fan to be 10m/s, separating the flaxseed shells from the flaxseed shells, and feeding the separated shells into a collecting device for later use;
separating the residual mixture (including flaxseed, flaxseed kernel and residual flaxseed hull) by adopting a screening mode, wherein the screen is divided into three layers, the screen mesh sizes (length multiplied by width) of the screen are respectively 5.0mm multiplied by 2.0mm, 4.0mm multiplied by 1.5mm and 3.0mm multiplied by 0.9mm, the rotation speed of the screen is controlled to be 260r/min, so that the flaxseed kernel, the flaxseed kernel and the residual flaxseed hull contained in the flaxseed kernel are effectively separated, and the three separated materials respectively enter corresponding collecting devices;
the separation rate of the flaxseed hull from the flaxseed kernel and flaxseed, and the separation rate of the flaxseed kernel from flaxseed were calculated according to the following formula:
T1＝Wshell/WGeneral assembly×100％(1)
T2＝WNut food/W(Total-shell)×100％(2)
T1: the separation rate of flaxseed hull from flaxseed kernel and flaxseed,%;
T2: separation rate of flaxseed kernel from flaxseed,%;
the calculated separation rate of the flaxseed hull from the flaxseed kernel and the flaxseed is 87.2%, and the separation rate of the flaxseed kernel from the flaxseed is 91.5%.
(3) Extraction of active ingredients
Taking the flaxseed shells collected in the step (2) to extract flaxseed gum and lignans, wherein the flaxseed gum is extracted by a water extraction method, and the lignans are extracted by an enzymatic hydrolysis method, and the method specifically comprises the following steps:
placing the collected flaxseed shells in a vacuum device, wherein the temperature of the vacuum device can be continuously adjusted, and the real-time monitoring of the temperature can be carried out, adding a proper amount of water into the flaxseed shells under the vacuum environment, mixing, extracting at the temperature of 80 ℃, the pressure of 0.09Mpa and the rotating speed of 70r/min, centrifuging, collecting supernatant to obtain flaxseed gum solution, collecting the flaxseed gum solution, and carrying out spray drying to obtain a finished product flaxseed gum;
collecting the centrifuged solid part, namely the residue after the flaxseed gum extraction, adding 30mL of 60% ethanol solution into 3g of the flaxseed hull residue, uniformly mixing, extracting in a water bath at 40 ℃ for 50min, collecting the extracting solution, centrifuging at the rotating speed of 3500r/min, collecting the supernatant, rotatably evaporating to dryness, adding 50mL of a cellulase (purchased from sigma company) preparation with the concentration of 0.04 mug/L into the dried product, carrying out enzymolysis at 35 ℃ for 30min, and then inactivating the enzyme at 100 ℃ to obtain the extracted lignan component;
extracting linseed oil fatty acid and flax protein from the linseed kernels collected in the step (2), wherein the linseed oil fatty acid is extracted by adopting an ultrasonic alcohol extraction method, and the protein is extracted by adopting a water extraction method, and the method specifically comprises the following steps:
adding petroleum ether (60-90 ℃) into the collected linseed kernels as an extraction solvent, wherein the liquid-material ratio of the linseed kernels to the petroleum ether is 15mL/g, extracting the linseed kernels under an ultrasonic condition, controlling the power of an ultrasonic step to be 180Mpa, controlling the temperature to be 68 ℃, and extracting for 35min, and collecting an obtained grease part, namely a linseed oil mixture; performing component analysis on the collected oil by adopting an infrared spectroscopy according to a conventional technology, and identifying the components of the obtained oil to comprise linolenic acid, linoleic acid, oleic acid, palmitic acid and stearic acid;
taking 10mL of the flax oil mixture, dissolving the mixture in a 500mL volumetric flask by using n-hexane, sucking 200mL of the solution into a beaker, and adding 2mol/L NaOH-CH3Saponifying OH solution 100mL, oscillating for 10min, treating in 50 deg.C water bath for 5min, and cooling to room temperature; to the saponified sample was added 2mol/L HCl-CH3200mL of OH solution, oscillating for 10min, performing methyl esterification treatment in water bath at 50 ℃ for 5min,adding urea into anhydrous methanol, heating and refluxing until the urea is completely dissolved, adding the obtained mixed fatty acid, carrying out reflux treatment in a water bath for 40min, cooling, then transferring into a refrigerator with the temperature of-15 ℃ for freezing for 8-20h, taking out, rapidly filtering under reduced pressure, collecting filtrate, carrying out reduced pressure distillation to remove the methanol, then adding a proper amount of water for layering, collecting an oil layer, washing with water until no urea exists, transferring the oil layer into a beaker, adding anhydrous sodium sulfate for dehydration, and carrying out suction filtration to obtain α -linolenic acid;
extracting flax protein from the residue after extraction of the flax oil fatty acid by a water extraction method, taking 200g of the flax kernel residue after extraction of the flax oil fatty acid, adding 6L of water, uniformly mixing, oscillating for 80min at 60 ℃, centrifuging for 20min at the rotating speed of 3000r/min, carrying out vacuum drying on the obtained precipitate for 5h, adding water into the dried substance according to the liquid-material ratio of 10mL/g, uniformly mixing, adjusting the pH value of the mixed solution to 10.0 by NaOH, centrifuging, taking the supernatant, adding hydrochloric acid to adjust the pH value of the supernatant to 7.0, and carrying out spray drying after rotary evaporation to obtain the flax kernel protein isolate.
Example 2
The comprehensive utilization process of flaxseeds in this embodiment includes the following steps:
(1) shelling
Screening the purchased flaxseeds without impurities and dust sequentially by using sieves with the sizes (length multiplied by width) of 5.0mm multiplied by 2.0mm, 4.0mm multiplied by 1.5mm and 3.0mm multiplied by 0.9mm respectively to obtain three types of flaxseeds with different sizes, wherein the flaxseeds with the sizes of about 5.2mm multiplied by 2.3mm are selected for testing in the embodiment;
measuring the initial water content of the selected flaxseeds to be 7.8% by using a method in the prior art, placing the flaxseeds in a drying oven, and drying the flaxseeds at 120 ℃ for 30min to obtain flaxseeds with the water content of 4.1%;
the obtained dried flaxseeds are placed in dehulling equipment for dehulling treatment, the dehulling equipment adopts a flaxseed dehulling and separating device disclosed in Chinese patent CN203530272U, the dehulling mode adopted by the device is a friction and collision combined mode for continuous dehulling, the friction force is realized by a grinding wheel, the shearing force is realized by a gear, and the rotating speed range is 1800-2500 r/min; the device is used for dehulling 200g of dried flaxseeds with the moisture content of 4.3 percent, the revolution speed of dehulling equipment is adjusted to 2200r/min, dehulling is continuously carried out for 4 times, and the dehulling rate is measured to reach 92 percent and the breakage rate is measured to be 3.2 percent.
(2) Separation of shell and kernel
Separating the husked mixture containing flaxseeds (without husking), flaxseed hulls and flaxseed kernels by air separation and screening;
firstly, separating by adopting a winnowing mode, namely, providing power by using a fan, controlling the wind speed of the fan to be 5m/s, separating the flaxseed shells from the flaxseed shells, and feeding the separated shells into a collecting device for later use;
separating the residual mixture (including flaxseed, flaxseed kernel and residual flaxseed hull) by adopting a screening mode, wherein the screen is divided into three layers, the screen mesh sizes (length multiplied by width) of the screen are respectively 5.0mm multiplied by 2.0mm, 4.0mm multiplied by 1.5mm and 3.0mm multiplied by 0.9mm, the rotation speed of the screen is controlled to be 260r/min, so that the flaxseed kernel, the flaxseed kernel and the residual flaxseed hull contained in the flaxseed kernel are effectively separated, and the three separated materials respectively enter corresponding collecting devices;
the calculated separation rate of the flaxseed hull from the flaxseed kernel and the flaxseed is 86.4%, and the separation rate of the flaxseed kernel from the flaxseed is 90.7%.
(3) Extraction of active ingredients
Taking the flaxseed shells collected in the step (2) to extract flaxseed gum and lignans, wherein the flaxseed gum is extracted by a water extraction method, and the lignans are extracted by an enzymatic hydrolysis method, and the method specifically comprises the following steps:
placing the collected flaxseed shells in a vacuum device, wherein the temperature of the vacuum device can be continuously adjusted, and the vacuum device can be used for monitoring the temperature in real time, adding a proper amount of water into the flaxseed shells to mix under the vacuum environment, controlling the temperature to be 70 ℃, the pressure to be 0.08Mpa and the rotating speed to be 60r/min for extraction, centrifuging and collecting supernatant liquid to obtain flaxseed gum solution, collecting the flaxseed gum solution, and performing spray drying to obtain a finished product flaxseed gum;
collecting the centrifuged solid part, namely the residue after the flaxseed gum extraction, adding 30mL of 50% ethanol solution into 3g of the flaxseed hull residue, uniformly mixing, extracting in a 50 ℃ water bath for 50min, collecting the extracting solution, centrifuging at the rotating speed of 3500r/min, collecting the supernatant, carrying out rotary evaporation to dryness, adding the dried product into 50mL of a 0.02 mu g/L cellulase (purchased from sigma company) preparation, carrying out enzymolysis at 35 ℃ for 30min, and then inactivating the enzyme at 100 ℃ to obtain an extracted lignan component;
extracting linseed oil fatty acid and flax protein from the linseed kernels collected in the step (2), wherein the linseed oil fatty acid is extracted by adopting an ultrasonic alcohol extraction method, and the protein is extracted by adopting a water extraction method, and the method specifically comprises the following steps:
adding petroleum ether (60-90 ℃) into the collected linseed kernels as an extraction solvent, wherein the liquid-material ratio of the linseed kernels to the petroleum ether is 5mL/g, extracting the linseed kernels under an ultrasonic condition, controlling the power of an ultrasonic step to be 200Mpa, the temperature to be 48 ℃, and the extraction time to be 35min, and collecting an obtained grease part, namely a linseed oil mixture; analyzing and identifying the components of the collected oil by infrared spectroscopy according to a conventional technology, and separating and extracting the components contained in the oil by referring to a conventional method in the prior art and the method in the example 1;
extracting flax protein from the residue after extraction of the flax oil fatty acid by a water extraction method, taking 200g of the flax kernel residue after extraction of the flax oil fatty acid, adding 4L of water, uniformly mixing, oscillating for 80min at 70 ℃, centrifuging for 20min at a rotation speed of 3500r/min, carrying out vacuum drying on the obtained precipitate for 6h, adding water into the dried substance according to a liquid-material ratio of 5mL/g, uniformly mixing, adjusting the pH value of the mixed solution to 10.0 by NaOH, centrifuging, taking the supernatant, adding hydrochloric acid to adjust the pH value of the supernatant to 7.0, and carrying out spray drying after rotary evaporation to obtain the flax kernel protein isolate.
Example 3
The comprehensive utilization process of flaxseeds in this embodiment includes the following steps:
(1) shelling
Screening the purchased flaxseeds without impurities and dust sequentially by using sieves with the sizes (length multiplied by width) of 5.0mm multiplied by 2.0mm, 4.0mm multiplied by 1.5mm and 3.0mm multiplied by 0.9mm respectively to obtain three types of flaxseeds with different sizes, wherein the flaxseeds with the sizes of about 5.2mm multiplied by 2.3mm are selected for testing in the embodiment;
determining the initial water content of the selected semen Lini to be 7.8% by existing method, placing the semen Lini in a drying oven, and drying at 120 deg.C for 25min to obtain semen Lini with water content of 4.3%;
the obtained dried flaxseeds are placed in dehulling equipment for dehulling treatment, the dehulling equipment adopts a flaxseed dehulling and separating device disclosed in Chinese patent CN203530272U, the dehulling mode adopted by the device is a friction and collision combined mode for continuous dehulling, the friction force is realized by a grinding wheel, the shearing force is realized by a gear, and the rotating speed range is 1800-2500 r/min; the device is used for dehulling 200g of dried flaxseeds with the moisture content of 4.3 percent, the revolution speed of dehulling equipment is adjusted to 2200r/min, dehulling is continuously carried out for 4 times, and the dehulling rate is measured to reach 92 percent and the breakage rate is measured to be 3.2 percent.
(2) Separation of shell and kernel
Separating the husked mixture containing flaxseeds (without husking), flaxseed hulls and flaxseed kernels by air separation and screening;
firstly, separating by adopting a winnowing mode, namely, providing power by using a fan, controlling the wind speed of the fan to be 20m/s, separating the flaxseed shells from the flaxseed shells, and feeding the separated shells into a collecting device for later use;
separating the residual mixture (including flaxseed, flaxseed kernel and residual flaxseed hull) by adopting a screening mode, wherein the screen is divided into three layers, the screen mesh sizes (length multiplied by width) of the screen are respectively 5.0mm multiplied by 2.0mm, 4.0mm multiplied by 1.5mm and 3.0mm multiplied by 0.9mm, the rotation speed of the screen is controlled to be 260r/min, so that the flaxseed kernel, the flaxseed kernel and the residual flaxseed hull contained in the flaxseed kernel are effectively separated, and the three separated materials respectively enter corresponding collecting devices;
the calculated separation rate of the flaxseed hull from the flaxseed kernel and the flaxseed is 88.7%, and the separation rate of the flaxseed kernel from the flaxseed is 92.3%.
(3) Extraction of active ingredients
Taking the flaxseed shells collected in the step (2) to extract flaxseed gum and lignans, wherein the flaxseed gum is extracted by a water extraction method, and the lignans are extracted by an enzymatic hydrolysis method, and the method specifically comprises the following steps:
placing the collected flaxseed shells in a vacuum device, wherein the temperature of the vacuum device can be continuously adjusted, and the real-time monitoring of the temperature can be carried out, adding a proper amount of water into the flaxseed shells under the vacuum environment, mixing, extracting at the temperature of 60 ℃, the pressure of 0.07Mpa and the rotating speed of 50r/min, centrifuging, collecting supernatant to obtain flaxseed gum solution, collecting the flaxseed gum solution, and carrying out spray drying to obtain a finished product flaxseed gum;
collecting the centrifuged solid part, namely the residue after the flaxseed gum extraction, adding 30mL of 70% ethanol solution into 3g of the flaxseed hull residue, uniformly mixing, extracting in a water bath at 40 ℃ for 50min, collecting the extracting solution, centrifuging at the rotating speed of 3500r/min, collecting the supernatant, carrying out rotary evaporation to dryness, adding the dried product into 50mL of a cellulase (purchased from sigma company) preparation with the concentration of 0.03 mu g/L, carrying out enzymolysis at 35 ℃ for 30min, and then carrying out enzyme inactivation at 100 ℃ to obtain an extracted lignan component;
extracting linseed oil fatty acid and flax protein from the linseed kernels collected in the step (2), wherein the linseed oil fatty acid is extracted by adopting an ultrasonic alcohol extraction method, and the protein is extracted by adopting a water extraction method, and the method specifically comprises the following steps:
adding petroleum ether (60-90 ℃) into the collected linseed kernels as an extraction solvent, wherein the liquid-material ratio of the linseed kernels to the petroleum ether is 25mL/g, extracting the linseed kernels under an ultrasonic condition, controlling the power of an ultrasonic step to be 120Mpa, the temperature to be 30 ℃, and the extraction time to be 20min, and collecting an obtained grease part, namely a linseed oil mixture; analyzing and identifying the components of the collected oil by infrared spectroscopy according to a conventional technology, and separating and extracting the components contained in the oil by referring to a conventional method in the prior art and the method in the example 1;
extracting flax protein from the residue after extraction of the linseed oil fatty acid by a water extraction method, adding 10L of water into 200g of the linseed kernel residue after extraction of the linseed oil fatty acid, uniformly mixing, oscillating for 80min at 50 ℃, centrifuging for 20min at the rotating speed of 2500r/min, carrying out vacuum drying on the obtained precipitate for 4-6h, adding water into the dried substance according to the liquid-material ratio of 20mL/g, uniformly mixing, adjusting the pH value of the mixed solution to 10.0 by NaOH, centrifuging, taking the supernatant, adding hydrochloric acid to adjust the pH value of the supernatant to 7.0, and carrying out spray drying after rotary evaporation to obtain the linseed oil protein isolate.
Comparative example 1
The process for the comprehensive utilization of flaxseed in this comparative example is the same as that of example 1, except that the step of separating the hulls from the kernels in step (2) is not included, and the active ingredient is extracted directly from the mixture comprising flaxseed, hulls from flaxseed and kernels.
Examples of effects
In the above embodiments of the invention, because the flaxseed shells and the flaxseed kernels are separated, in the process of extracting the effective components, the flaxseed shells can be used for extracting the flaxseed gum and the lignans, and the whole extraction process is not influenced by other components, so that the obtained flaxseed gum and the lignans have higher quality and purity.
In the scheme of the comparative example, in the whole extraction process, the components of the extracted fat and protein are influenced by the flaxseed gum, so that the quality and the purity of the flaxseed gum are influenced; the extraction of the flaxseed gum and the lignan is influenced by fat leaching, and the quality is reduced; especially for oil, a degumming step is needed to be added, the cost is increased, the quality of the oil is reduced, and the comprehensive utilization efficiency and the product quality of the flaxseeds are seriously influenced.
Through detection, compared with a comparative example, the yield of the flaxseed gum and the lignan in each embodiment of the invention is respectively improved by about 30-50% and 20-40%; similarly, because only the linseed kernels are adopted to directly extract the grease and the flax protein, the extraction rate of the grease and the protein is higher, the obtained product is not influenced by other components, the quality and the purity are higher, and compared with a comparative example, the grease and protein yield in each embodiment of the invention can be correspondingly improved, and the improvement rate is about 30-50%.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.

Claims (6)

1. The comprehensive utilization process of flaxseeds is characterized by comprising the following steps of:
(1) drying flaxseeds and dehulling the flaxseeds;
(2) carrying out shell-kernel separation treatment on the flaxseeds after shelling by adopting a mode of combining air separation and screening;
(3) respectively extracting the collected flaxseed shells to obtain flaxseed gum and lignans, and extracting the collected flaxseed kernel to obtain flaxseed oil fatty acid and flaxseed protein;
the steps for extracting the flaxseed gum and the lignans from the flax shells comprise:
extracting the collected flaxseed shells with water under vacuum condition at temperature below 100 deg.C under extraction pressure of 0.07-0.09MPa to obtain flaxseed gum solution, and vacuum drying to obtain flaxseed gum;
adding ethanol solution into the residue after extracting flaxseed gum, extracting at 40-50 deg.C, collecting the extractive solution, drying, adding cellulase, and performing enzymolysis to obtain lignan;
the steps for extracting the linseed oil fatty acid and the flax protein in the linseed kernels comprise the following steps:
adding petroleum ether into the collected linseed kernels as an extraction solvent, and extracting at 30-60 ℃ under an ultrasonic condition to obtain a linseed oil fatty acid mixture;
identifying the components contained in the extract by infrared spectroscopy, and extracting α -linolenic acid contained in the extract, which comprises the following steps:
dissolving the flax oil fatty acid mixture with n-hexane, and adding 2mol/L NaOH-CH3Saponifying OH solution, oscillating, treating in water bath at 50 deg.C, and cooling to room temperature; to the saponified sample was added 2mol/L HCl-CH3Adding urea into anhydrous methanol, heating and refluxing until the urea is completely dissolved, adding the obtained mixed fatty acid, carrying out water bath reflux treatment, cooling, freezing in a refrigerator at the temperature of-15 ℃ for 8-20h, taking out, rapidly filtering under reduced pressure, collecting filtrate, distilling under reduced pressure to remove the methanol, adding a proper amount of water for layering, collecting an oil layer, washing with water until no urea exists, transferring the oil layer into a beaker, adding anhydrous sodium sulfate for dehydration, and carrying out suction filtration to obtain α -linolenic acid;
mixing the residue after extracting oleum Lini fatty acid with water, extracting at 50-80 deg.C, performing solid-liquid separation, collecting precipitate, drying, mixing with water, adjusting pH to alkaline, performing solid-liquid separation, collecting supernatant, adjusting pH to neutral, concentrating, and spray drying to obtain flax protein.
2. The process for the comprehensive utilization of flaxseeds according to claim 1, wherein in step (1), the drying step is hot air drying and drying until the moisture content of flaxseeds is 3.0% -5.0%; and the shelling step is to continuously shell by adopting a friction and collision combined mode.
3. The process of claim 2, wherein in step (2), the step of separating the hull and kernel of flaxseeds is a combination of air separation and screening:
the air separation step is that the flaxseed shells are separated from the flaxseed shell mixture through a fan, and the separated flaxseed shells enter a collection device;
and in the screening step, the mixture of the flaxseed kernels, the flaxseeds and the residual flaxseed husks passes through a vibrating screen and is separated by the vibrating screen with the size suitable for the flaxseed kernels, the flaxseeds and the flaxseed husks.
4. The process of claim 3, wherein the flax seeds are processed by the following steps:
in the winnowing step, the wind speed of the fan is controlled to be 5-20 m/s;
in the screening step, the rotating speed of the vibrating screen is controlled to be 200-400 r/min.
5. The process of claim 4, wherein the flax seeds are selected from the group consisting of: the vibrating screen comprises three screens with the screen mesh sizes of 5.0mm multiplied by 2.0mm, 4.0mm multiplied by 1.5mm and 3.0mm multiplied by 0.9mm respectively.
6. The process for the recycling of flax seeds of any one of claims 1-5, wherein said step (1) further comprises the step of classifying and screening said flax seeds according to size by using a screen with a screen mesh size of (4.0-6.0) mm x (1.0-3.0) mm.
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