CN115093895B - Device and method for preparing rapeseed oil with assistance of high-voltage alternating-current pulsed electric field - Google Patents
Device and method for preparing rapeseed oil with assistance of high-voltage alternating-current pulsed electric field Download PDFInfo
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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
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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
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Abstract
The application improves a device and a method for preparing rapeseed oil assisted by a high-voltage alternating-current pulse electric field, changes the permeability of plant seed cell membranes by using the high-voltage alternating-current pulse electric field, increases the oil yield, and simultaneously achieves the effects of enzyme deactivation and demulsification by using the high-voltage alternating-current pulse electric field. The immobilized enzyme prepared by the method can be recycled by a simple method, so that the enzyme can be reused, and meanwhile, the enzyme stability is improved.
Description
Technical Field
The application relates to the technical field of grease processing, in particular to a device and a method for preparing rapeseed oil with the assistance of a high-voltage alternating-current pulse electric field.
Background
Rapeseed oil has fragrant and mellow smell and rich nutrition. The absorption rate of the human body to the rapeseed oil is very high and can reach 99 percent. Has effects of tonifying deficiency, moisturizing intestine, removing liver fire, promoting gallbladder function, promoting brain development, resisting irritation of eyes to various strong light, preventing senile eye diseases, and infantile amblyopia. The high oleic rapeseed oil is rich in unsaturated fatty acids such as oleic acid, linoleic acid and the like and vitamin E, and can soften blood vessels and delay aging. Sterols are also higher in content than common vegetable oils such as soybean oil, and are of a wide variety, some sterols also have specific physiological functions. The phospholipids of rapeseed oil are beneficial to development of blood vessels, nerves and brain, and the cholesterol of the rapeseed oil is little or no. The canola oil has a very low saturated fatty acid content, an oleic acid content of over 60%, and reasonable levels of linoleic and linolenic acids, and is therefore known as the "healthiest edible vegetable oil". Compared with the plant sterol content of other edible vegetable oils, the rapeseed oil has lower cholesterol content, and the rapeseed sterol, campesterol and stigmasterol which are beneficial to the body health are the highest in the edible vegetable oils. The rapeseed polyphenol is an important secondary metabolite unique to rapeseeds, has biological activities of resisting tumor, reducing blood sugar, inhibiting bacteria, removing free radicals and the like, and is a potential important natural antioxidant.
At present, most of the rapeseed oil production processes in China adopt a shelled high-temperature pre-squeezing-leaching oil production process. The products are crude oil and rapeseed cake. Because of the high temperature pre-pressing, crude oil is mostly dark brown and needs to be refined, so the flavor and the nutrition components of the rapeseed oil can be lost to different degrees. While the leaching stage currently uses No. 6 solvent oil (n-hexane content of about 30%), extraction of rapeseed oil using hexane has recently become the focus of its safety and environmental impact as hexane is included in the harmful air pollutant group. At laboratory and pilot plant scale levels, aqueous enzymatic processes have been tried for extracting oil from many oilseeds/fruits. Compared with the prior art, the process is mild and safe since the organic solvent is completely avoided. Despite these advantages, the disadvantages of the aqueous enzymatic process are also apparent. First, enzyme preparation price is still higher in the present stage, production cost is increased, so that the aqueous enzymatic method is mostly remained in laboratory research and pilot-plant stages for many years, and industrial application is limited. In the process of extracting vegetable oil, the cell walls are hard, thick and complex in composition, and the synergistic effect of various enzymes is often required, so that the wall breaking effect of partial oil materials is poor, and the oil extraction rate is low. In addition, in the process of extracting grease by the aqueous enzymatic method, the residual oil rate in the formed emulsion layer and the residual slag layer is high, so that the oil extraction rate is low.
Disclosure of Invention
The application aims to overcome the defects in the prior art and provide a device and a method for preparing the aromatic rapeseed oil by high-voltage alternating-current pulse type electric field assisted catalysis, which have the advantages of low treatment temperature, capability of keeping the flavor of rapeseeds to the maximum extent and capability of keeping bioactive substances such as tocopherol, polyphenol, antioxidant, phytosterol and the like.
The permeability of plant seed cell membrane is changed by using an alternating current pulse electric field, and the oil yield is increased. Meanwhile, in the later extraction stage of the aqueous enzymatic method, the alternating current pulse electric field can effectively increase vibration and collision of liquid drops in the oil liquid, improve the coalescence efficiency of the liquid drops, and have a good demulsification effect. In the case of aqueous enzymatic extraction, however, the immobilized enzyme is used instead of the conventional enzyme in free form. Compared with the free form enzyme, the enzyme has good temperature and pH adaptability, and can be recycled by a simple method with less loss of enzyme activity. And the separation and purification of the product are easier.
The first aim of the application is to provide a device for preparing the aromatic rapeseed oil by utilizing high-voltage alternating current pulse type electric field auxiliary extraction, which comprises a main body (1); the main body (1) is provided with a servo motor (2), a feed inlet (3), a steel plate (4), a mixing rod (5), a rotary baffle plate (6), screening holes (7), an inclined plate (8), a pH detector (9), a temperature detector (10), a heating block (11), a magnetic enzyme recovery tank (12), a filter tank (13), a liquid storage tank (14), a controller (15), an acid adding pipeline (16), a water inlet pipe (19) and a discharge outlet (20).
In one embodiment of the application, the main body (1) comprises a first layer, a second layer, a third layer and a fourth layer from top to bottom, a rotary baffle is arranged between the layers, and steel plates (4) are symmetrically arranged in the first layer, the second layer and the fourth layer of the main body (1); the utility model discloses a filter device, including main part (1), rotatory baffle, main part (1), inclined plate (8), main part (1), rotatory baffle, filtering tank (13) and filter screen, main part (1) internally mounted has servo motor (2), and the lower extreme of servo motor (2) is connected with hybrid pole (5), inside heating block (11) of being equipped with of second floor and third layer, pH detector (9) and temperature detector (10) are equipped with to second floor and third layer inner wall, all set up screening hole (7) in the rotatory baffle left and right sides between every layer of main part (1), main part (1) first layer screening hole lower extreme is provided with inclined plate (8), main part (1) second, three-layer screening hole lower extreme sets up surface magnetism's enzyme recovery groove (12) to the form of slider is convenient for take out, and main part (1) is provided with filter tank (13), installs in the bottom with the form of slider equally.
In one embodiment of the application, the main body (1) further comprises an alkali adding pipeline (17) and an enzyme adding pipeline (18).
In one embodiment of the application, the main body (1) and the servo motor (2) are fixedly connected, and the mixing rods (5) are uniformly distributed along the vertical center line of the servo motor.
In one embodiment of the application, the interior of the body (1) is coated with an internal insulating material.
In one embodiment of the application, the steel plates (4) are symmetrically distributed on the insulating material in the main body, and the front surface of the main body is provided with a controller (15), and the controller (15) is electrically connected with the steel plates (4).
In one embodiment of the application, the screening holes (7) are uniformly distributed along two sides of the rotating baffle plate (6), the rotating baffle plate (6) is electrically connected with the controller (15), and the controller (15) controls the rotating baffle plate (6) to rotate.
In one embodiment of the application, the heating blocks (11) are annularly and symmetrically distributed inside the main body (1), and the connection mode between the controller (15) and the heating blocks (11) is electric connection.
In one embodiment of the application, the magnetic enzyme recovery grooves (12) are distributed at the lower end of the screening hole (7), the magnetic enzyme recovery grooves (12) are provided with magnets, and a sliding structure is formed between the magnetic enzyme recovery grooves (12) and the main body (1).
In one embodiment of the application, the filter tanks (13) are distributed at the bottom of the main body (1), the bottom layer is provided with a filter screen, and a sliding structure is formed between the filter tanks (13) and the main body (1).
In one embodiment of the application, the discharge port (20) is positioned at the side of the liquid storage tank (14) and is connected with a pump, so that the liquid in the liquid storage tank (14) is discharged out of the main body (1).
The second object of the present application is to provide a method for preparing aromatic rapeseed oil with assistance of a high-voltage ac pulsed electric field by using the above device, comprising the following steps:
(1) screening, cleaning, sun drying and pulverizing semen Brassicae campestris raw materials;
(2) carrying out pulse electric field pretreatment on crushed rapeseeds;
(3) adding water for mixing, and carrying out a second pulse electric field treatment on the mixture;
(4) adding immobilized cellulase, and separating to remove immobilized enzyme after enzyme hydrolysis is finished;
(5) adding immobilized alkaline endoprotease, separating and removing immobilized enzyme after enzyme hydrolysis is finished;
(6) performing a third pulsed electric field treatment on the obtained mixture;
(7) centrifuging to obtain upper layer to obtain rapeseed oil.
In one embodiment of the application, when the device is used for preparing rapeseed oil, a user firstly inserts an enzyme recovery tank (12) and a filter tank (13) into a main body (1), then pours crushed rapeseed into the main body (1) along a feed port (3), meanwhile, the user turns on a servo motor (2), the servo motor (2) is matched with a mixing rod (5) to enable materials to be mixed evenly, and then a high-voltage alternating current pulse type electric field is formed between steel plates (4) of a first layer of the main body (1) by a command of a controller (15), so that plant cell walls are damaged and more grease is released;
the rotary baffle plate (6) arranged at the end opens the exposing screening hole (7), the material slides into the second layer of the main body (1) along the inclined plate (8), the water inlet pipeline (19) is commanded to be opened through the controller (15), meanwhile, a high-voltage alternating current pulse type electric field is formed between the second layer of the steel plates (4) of the main body (1), the temperature and the pH of the material liquid are monitored through the pH detector (9) and the temperature detector (10) arranged at the end, the controller opens the acid adding pipeline (16) and the alkali adding pipeline (17) arranged at the end to adjust the pH, the heating block (12) is commanded to be started to adjust the temperature, and then the immobilized cellulase is released through the enzyme adding pipeline (18) arranged at the end to process;
after the treatment is finished, the arranged rotary baffle (6) opens the exposure screening hole (7), the material slides into the third layer of the main body (1) along the inclined surface of the enzyme recovery tank (12), wherein immobilized cellulase is attached to the recovery tank due to magnetism on the surface of the recovery tank (12), the temperature and pH of the material liquid are monitored through the arranged pH detector (9) and the temperature detector (10), the controller opens the arranged acid adding pipeline (16) and the alkali adding pipeline (17) to adjust the pH, meanwhile, the heating block (12) is instructed to start to adjust the temperature, and then the immobilized alkaline endoprotease is released through the arranged enzyme adding pipeline to carry out the treatment;
after the treatment is finished, the arranged rotary baffle (6) opens the exposed screening holes (7), and materials slide into the fourth layer of the main body (1) along the inclined surface of the recovery tank (12), wherein the immobilized alkaline endoprotease is attached to the recovery tank due to the magnetism on the surface of the recovery tank (12), and a high-voltage alternating current pulse type electric field is formed between the steel plates (4) of the fourth layer of the main body (1) through the command of the controller (15) to play a role in demulsification;
after demulsification treatment is completed, the rotary baffle (6) is arranged to open the exposed filter tank (13), under the action of the main body (1) external pump, feed liquid flows out along the discharge port (20) through the liquid storage tank (14), solids are attached to the filter tank (13), after the use is completed, the device is closed, the enzyme recovery tank (12) and the filter tank (13) are pulled open, so that solid residues and enzymes can be conveniently treated, and the whole process of preparing rapeseed oil by using the device is completed.
In one embodiment of the present application, in the step (2), the high-voltage ac pulsed electric field is used to increase the permeability of the cytoplasmic membrane of rapeseed by electric stimulation, destroy the plant cell structure and increase the dissolution path of intracellular substances.
In one embodiment of the present application, in the step (2), the electric field strength is 25-35 kV/cm, the material retention time is 180-200 s, the pulse frequency is 750-850 Hz, and the duty ratio is 0.5-0.6.
In one embodiment of the present application, in the step (3), a pulsed electric field is used instead of the conventional high temperature enzyme deactivation process, avoiding loss of part of flavor and nutrients.
In one embodiment of the present application, in the step (3), the ratio of oil to water is 1:3 to 5 (w/v, g/mL).
In one embodiment of the present application, in the step (3), the electric field strength is 65 to 75kV/cm, the pulse frequency is 750 to 850Hz, and the duty ratio is 0.5 to 0.6.
In one embodiment of the present application, the immobilized cellulase used in the step (4) is immobilized with carrier-containing ferroferric oxide nanoparticles.
In one embodiment of the present application, in the step (4), the temperature of the enzymatic hydrolysis is 40 to 45 ℃, the pH is 7.5 to 8.0, and the stirring is performed for 1 to 2 hours.
In one embodiment of the present application, in the step (5), the immobilized alkaline endoprotease is immobilized with carrier-containing ferroferric oxide nanoparticles.
In one embodiment of the present application, in the step (5), the temperature of the enzymatic hydrolysis is 60 to 65 ℃, the pH is 8.5 to 9.0, and the stirring is performed for 4 to 4.5 hours.
In one embodiment of the present application, in the step (6), a pulse electric field is used for demulsification treatment, wherein the electric field strength is 35-40 kV/cm, the pulse frequency is 550-600 Hz, and the duty ratio is 0.6-0.7
In one embodiment of the present application, in the step (6), the preferable electric field strength is 40kV/cm, the pulse frequency is 600Hz, and the duty ratio is 0.7.
In one embodiment of the present application, in the step (7), the centrifugal speed is 4500-6000 r/min, and the centrifugal speed is 10-20 min at room temperature.
The beneficial effects are that:
the application adopts the aqueous enzymatic method to extract the rapeseed oil, adopts biological enzymes to degrade the cell structure of the oil tissue and the ultrastructure of lipopolysaccharide and lipoprotein, thereby increasing the fluidity of the oil in the oil tissue, enabling the oil to be free from the oil, further promoting phenols and other substances to enter the oil, and further improving the oxidation stability, shelf life, nutrition, flavor, sense organ and other performances of the oil because of the protection of the water phase and the emulsion layer in the extraction process.
The method of the application uses the high-voltage alternating current pulse type electric field treatment technology for three times, carries out the high-voltage alternating current pulse type electric field treatment on the oilseeds for the first time, replaces the traditional steaming and frying technology, has mild conditions, generates high-voltage current through discharge, damages plant cells, changes the permeability of the plant cells, enables substances in the cells to effectively flow out, promotes the release of volatile components, and improves the oil gas flavor so as to improve the oil extraction rate and the oil flavor of the subsequent squeezing technology. The second time carries out high-voltage alternating current pulse type electric field treatment on the mixed system of oil and water to ensure that the mixed system is more uniformly dispersed in the water, and simultaneously, the instant pulse type electric field is utilized to act on microbial cells, so that the cell membranes form pores, the permeability is enhanced, the cells expand, and finally, the mixed system breaks down to inactivate microorganisms, and meanwhile, enzymes contained in the system are passivated. Compared with the traditional high-temperature enzyme deactivation, the high-voltage alternating-current pulse type electric field is cold treatment, can preserve the inherent components of rapeseeds, and meanwhile, can sterilize and deactivate enzymes, thereby saving energy consumption. Besides sterilization and enzyme deactivation, the third pulsed electric field treatment can effectively increase vibration and collision of liquid drops in oil, improve coalescence efficiency of the liquid drops, play a role in demulsification, and simultaneously can adjust parameters such as electric field intensity, pulse frequency, duty ratio and the like according to oil working conditions so as to obtain an optimal demulsification effect.
The enzyme adopted by the application is self-made immobilized enzyme, and the cellulase and the alkaline endoprotease are immobilized by the ferroferric oxide nano-particles containing the carrier, so that the enzyme is convenient to recover due to magnetism, the recycling of the enzyme can be realized, the production cost is reduced, and the production efficiency is improved.
The device provided by the application can enable rapeseeds to be uniformly mixed through the mutual matching of the arranged servo motor and the mixing rod, and the arranged rotary baffle and the filter holes are mutually matched to control the treatment duration and the flow velocity.
Through setting up sliding construction's enzyme recovery tank and filter vat, improve enzyme's recovery efficiency, utilize the filter vat to detach the solid matter, reduce the degree of difficulty of centrifugal operation and avoid impurity to influence the purity of follow-up oil, the sliding construction who sets up moreover can conveniently wash it and change.
Drawings
FIG. 1 is a process flow diagram of the method of the present application
FIG. 2 demulsification Rate under electric field treatments of different intensities
FIG. 3 demulsification Rate under electric field treatment at different pulse frequencies
FIG. 4 demulsification Rate under electric field treatment with different duty cycles
FIG. 5 is a schematic view of the structure of the device of the present application
FIG. 6 is an external view of the device of the present application
FIG. 7 is a schematic cross-sectional view of the device of the present application
In the figure: (1) a body; (2) a servo motor; (3) a feed inlet; (4) a steel sheet; (5) a mixing rod; (6) rotating the baffle; (7) screening the wells; (8) inclined plates; (9) a pH detector; (10) a temperature detector; (11) a heating block; (12) a magnetic enzyme recovery tank; (13) a filtration tank; (14) a reservoir; (15) a controller; (16) an acid addition line; (17) a base addition line; (18) an enzyme addition line; (19) a water inlet pipe; (20) a discharge port.
Detailed Description
The color measurement of the rapeseed oil refers to GB/T22460-2008 for measuring the color of animal and plant grease Luowei; acid value determination is referred to GB/T5530-2005, determination of acid value and acidity of animal and vegetable fats & oils; measurement of peroxide value is referred to GB/T5538-2005 "measurement of peroxide value of oil and fat"; moisture and volatile content are referred to GB/T5528-2008. Measurement of oxidation stability reference NY/T2001-2011, "measurement of oxidation stability of rapeseed oil accelerated oxidation test"; determination of polyphenol content reference LS/T6119-2017, spectrophotometry for determining polyphenol in vegetable oil for grain and oil detection; the demulsification rate measurement method comprises the following steps: 5g of rapeseed emulsion is weighed by a 50mL beaker, and is taken out after being treated by a high-voltage alternating current pulse type electric field with certain electric field strength, electric field frequency and duty ratio. Centrifuging at 4500r/min at room temperature for 10min to obtain free oil, water phase mixture and residue, and calculating demulsification rate according to formula (1). The oil yield is calculated according to the following formula (2):
the principles and features of the present application are described below with examples given for the purpose of illustration only and are not intended to limit the scope of the application.
Example 1: device for preparing aromatic rapeseed oil by high-voltage alternating-current pulse type electric field assisted catalytic extraction
The utility model provides a device of high-voltage alternating current pulse type electric field auxiliary catalytic extraction preparation aromatic rapeseed oil, main part (1) is provided with servo motor (2), feed inlet (3), steel sheet (4), hybrid rod (5), rotating barrier (6), screening hole (7), hang plate (8), pH detector (9), temperature detector (10), heating block (11), magnetic enzyme recovery tank (12), filter tank (13), reservoir (14), controller (15), acid addition pipeline (16), inlet tube (19) and discharge gate (20).
The main body (1) comprises a first layer, a second layer, a third layer and a fourth layer from top to bottom, a rotary baffle is arranged between the layers, and steel plates (4) are symmetrically arranged in the first layer, the second layer and the fourth layer of the main body (1); the utility model discloses a filter device, including main part (1), rotatory baffle, main part (1), inclined plate (8), main part (1), rotatory baffle, filtering tank (13) and filter screen, main part (1) internally mounted has servo motor (2), and the lower extreme of servo motor (2) is connected with hybrid pole (5), inside heating block (11) of being equipped with of second floor and third layer, pH detector (9) and temperature detector (10) are equipped with to second floor and third layer inner wall, all set up screening hole (7) in the rotatory baffle left and right sides between every layer of main part (1), main part (1) first layer screening hole lower extreme is provided with inclined plate (8), main part (1) second, three-layer screening hole lower extreme sets up surface magnetism's enzyme recovery groove (12) to the form of slider is convenient for take out, and main part (1) is provided with filter tank (13), installs in the bottom with the form of slider equally.
The main body (1) also comprises an alkali adding pipeline (17) and an enzyme adding pipeline (18).
The main body (1) is fixedly connected with the servo motor (2), and the mixing rods (5) are uniformly distributed along the vertical central line of the servo motor.
The inside of the main body (1) is coated with an internal insulating material.
The steel plates (4) are symmetrically distributed on the insulating material in the main body, the controller (15) is arranged on the front surface of the main body, and the controller (15) is electrically connected with the steel plates (4).
The screening holes (7) are uniformly distributed along two sides of the rotary baffle plate (6), the rotary baffle plate (6) is electrically connected with the controller (15), and the controller (15) controls the rotary baffle plate (6) to rotate.
The heating blocks (11) are annularly and symmetrically distributed inside the main body (1), and the connection mode between the controller (15) and the heating blocks (11) is electric connection.
The magnetic enzyme recovery grooves (12) are distributed at the lower ends of the screening holes (7), the magnetic enzyme recovery grooves (12) are provided with magnets, and a sliding structure is formed between the magnetic enzyme recovery grooves (12) and the main body (1).
The filter tanks (13) are distributed at the bottom of the main body (1), the bottom layer is provided with a filter screen, and a sliding structure is formed between the filter tanks (13) and the main body (1).
The discharge hole (20) is positioned at the side surface of the liquid storage tank (14) and is connected with a pump, so that the liquid in the liquid storage tank (14) is discharged out of the main body (1).
Working principle: before using the rapeseed oil preparation device, a user firstly inserts an enzyme recovery tank (12) and a filter tank (13) into a main body (1), then pours crushed rapeseeds into the main body (1) along a feed inlet (3), meanwhile, the user turns on a servo motor (2), the servo motor (2) is matched with a mixing rod (5), materials can be evenly mixed, and then a high-voltage alternating current pulse type electric field is formed between steel plates (4) of a first layer of the main body (1) through a command of a controller (15), so that the plant cell walls are damaged, and more grease is released. The rotary baffle (6) that sets up later opens and exposes screening hole (7), and the material slides into main part (1) second floor along inclined plate (8), and inlet channel (19) are opened through controller (15) order, make simultaneously between main part (1) second floor steel sheet (4) form high-pressure alternating current pulse electric field, monitor the temperature and the pH of feed liquid through pH detector (9) and temperature detector (10) that set up, the controller is opened acid and is added pipeline (16) and alkali and add pipeline (17) that set up and adjust pH, simultaneously order heating piece (12) to open regulating temperature, then release enzyme A through enzyme that sets up adding pipeline (18). After a period of treatment, the rotary baffle (6) is arranged to open the exposure screening hole (7), the material slides into the third layer of the main body (1) along the inclined surface of the enzyme recovery tank (12), wherein enzyme A is attached to the recovery tank due to magnetism on the surface of the recovery tank (12), the temperature and pH of the feed liquid are monitored through the pH detector (9) and the temperature detector (10), the pH is regulated by opening the acid adding pipeline (16) and the alkali adding pipeline (17) which are arranged by the controller, the heating block (12) is commanded to be started to regulate the temperature, and then enzyme B is released through the arranged enzyme adding pipeline. After a period of treatment, the rotary baffle (6) is arranged to open the exposed screening holes (7), and materials slide into the fourth layer of the main body (1) along the inclined surface of the recovery tank (12), wherein enzyme B is attached to the recovery tank due to magnetism on the surface of the recovery tank (12), and a high-voltage alternating current pulse type electric field is formed between the steel plates (4) of the fourth layer of the main body (1) through a command of the controller (15) to achieve a demulsification effect. After a period of treatment, the rotary baffle (6) is arranged to open and expose the filter tank (13), under the action of the main body (1) external pump, feed liquid flows out along the discharge port (20) through the liquid storage tank (14), solids are attached to the filter tank (13), after the use is finished, the device is closed, the enzyme recovery tank (12) and the filter tank (13) are pulled open, and the treatment of solid residues and enzymes can be conveniently carried out, so that the use process of the whole oil production device is completed.
Example 2: preparation of immobilized enzyme
Dissolving sodium alginate in distilled water to obtain 2.0% (w/v, g/mL) sodium alginate solution, adding 1.6% (w/v, g/mL) Fe 3 O 4 The nanoparticles were stirred for 30min. The mixture was heated to 80℃and stirred under nitrogen for 1h. The ferrofluid was further sonicated for 20min and centrifuged to remove small amounts of large agglomerates (1000 Xg, 10 min) for purification. Adding 10mL of alkaline endoprotease (30000U) or cellulase (30000U) solution into 100mL of magnetic fluid, mixing uniformly, injecting ferrofluid into 10wt% CaCl by a syringe 2 In the aqueous solution, magnetic microspheres are prepared. After the magnetic microspheres are soaked for 1 hour, washing with distilled water to remove free Ca adhered to the surface 2+ Then crosslinked with 0.5% glutaraldehyde for 1.5 hours and washed with distilled water. Finally, the microspheres were incubated at 4 ℃ overnight to harden them. Drying at 35 ℃ for 12 hours to obtain the immobilized enzyme.
Example 3
(1) Screening, and cleaning to remove impurities such as weed seeds, cereal seeds, seed hulls and the like in the rapeseed raw materials; cleaning, namely cleaning the screened rapeseeds with clear water, washing off dust on the surfaces of the rapeseeds, draining, and airing moisture in sunlight; crushing, and crushing the dried rapeseeds by a grinder.
(2) First high-voltage alternating current pulse type electric field treatment: the crushed rapeseeds are subjected to high-voltage alternating current pulse type electric field pretreatment, the strength of the voltage pulse electric field is 25kV/cm, the material retention time is 180s, the pulse frequency is 850Hz, and the duty ratio is 0.5.
(3) And (3) secondary high-voltage alternating current pulse type electric field treatment: 5 grams of treated rapeseed was mixed with distilled water at a mass ratio of 1:3 (w/v, g/mL). The mixture was subjected to a high voltage alternating current pulsed electric field with a pulse frequency of 850Hz and a duty cycle of 0.5 at a voltage pulsed electric field strength of 75 kV/cm.
(4) First enzyme treatment: heating to 40 ℃, adjusting the pH to 8.0, adding immobilized cellulase, and stirring at 40 ℃ for 1 hour. And (3) separating the immobilized cellulase with magnetism.
(5) Second enzyme treatment: the temperature was reduced to 60℃and the pH was adjusted to 9.0, and the immobilized alkaline endoprotease was added, mixed and stirred for 4 hours. After the completion of the enzymatic hydrolysis, the immobilized alkaline endoprotease having magnetism is isolated.
(6) Third high voltage pulse treatment: the mixture after the immobilized enzyme is separated is treated by a high-voltage alternating current pulse type electric field, the intensity of the voltage pulse type electric field is 40kV/cm, the pulse frequency is 600Hz, and the duty ratio is 0.7.
(7) And (5) centrifuging. Centrifuging the obtained suspension at room temperature at 4500r/min for 10min, and collecting upper layer oil to obtain rapeseed oil.
Example 4: high-voltage alternating-current pulse type electric field demulsification condition (electric field strength) optimization
(1) - (5) steps (1) to (5) as in example 3;
(6) Third high voltage pulse treatment: carrying out high-voltage alternating current pulse type electric field treatment on the mixture after the immobilized enzyme is separated, wherein the high-voltage pulse electric field intensity is 15, 20, 25, 30, 35, 40, 45, 50, 55 and 60kV/cm, the pulse frequency is 600Hz, and the duty ratio is 0.7;
(7) Centrifuging the obtained suspension at room temperature at a rotating speed of 4500r/min for 10min to obtain free oil, water phase mixed solution and residue, and calculating demulsification rate.
Example 5: high-voltage alternating-current pulse type electric field demulsification condition (electric field frequency) optimization
(1) - (5) steps (1) to (5) as in example 3;
(6) Third high voltage pulse treatment: carrying out high-voltage alternating current pulse type electric field treatment on the mixture after the immobilized enzyme is separated, wherein the high-voltage alternating current pulse type electric field strength is 40kV/cm, and the pulse frequencies are 300, 350, 400, 450, 500, 550, 600, 650, 700 and 750Hz, and the duty ratio is 0.7;
(7) Centrifuging the obtained suspension at room temperature at a rotating speed of 4500r/min for 10min to obtain free oil, water phase mixed solution and residue, and calculating demulsification rate.
Example 6: high-voltage alternating-current pulse type electric field demulsification (duty cycle) optimization
(1) - (5) steps (1) to (5) as in example 3;
(6) Third high voltage pulse treatment: performing high-voltage alternating current pulse type electric field treatment on the mixture from which the immobilized enzyme is separated, wherein the high-voltage alternating current pulse type electric field strength is 40kV/cm, the pulse frequency is 600Hz, and the duty ratios are 0.1, 0.3, 0.5, 0.7, 0.8 and 0.9;
(7) Centrifuging the obtained suspension at room temperature at a rotating speed of 4500r/min for 10min to obtain free oil, water phase mixed solution and residue, and calculating demulsification rate.
Comparative example 1: traditional aqueous enzymatic process
Screening: cleaning and removing a small amount of weed seeds, cereal seeds, seed husks and the like.
Cleaning: and cleaning the screened rapeseeds with clear water, washing off dust on the surfaces of the rapeseeds, draining, and airing moisture in sunlight.
Crushing: and crushing the aired rapeseeds by a grinder.
Adding water and mixing: 5g of treated rapeseed was mixed with distilled water in a mass ratio of 1:3 (w/v, g/mL) and boiled for 4min.
First enzyme treatment: heating to 50deg.C, adjusting pH to 6.0, stirring at 50deg.C for 1 hr.
Second enzyme treatment: the temperature was raised to 60℃and the pH was adjusted to 9.0, and the immobilized alkaline endoprotease was added, mixed and stirred for 4 hours. Heating to 90 ℃ and keeping for 10min.
And (3) centrifuging: centrifuging the obtained suspension at room temperature at 4500r/min for 10min, and collecting upper layer oil to obtain rapeseed oil.
Comparative example 2: using immobilized enzymes (without treatment by high-voltage AC pulsed electric fields)
Screening: cleaning and removing a small amount of weed seeds, cereal seeds, seed husks and the like.
Cleaning: and cleaning the screened rapeseeds with clear water, washing off dust on the surfaces of the rapeseeds, draining, and airing moisture in sunlight.
Crushing: and crushing the aired rapeseeds by a grinder.
Adding water and mixing: 5g of treated rapeseed was mixed with distilled water in a mass ratio of 1:3 (w/v, g/mL) and boiled for 4min.
First enzyme treatment: heating to 40 ℃, adjusting the pH to 8.0, adding immobilized cellulase, and stirring at 40 ℃ for 1 hour. And (3) separating the immobilized cellulase with magnetism.
Second enzyme treatment: the temperature was reduced to 60℃and the pH was adjusted to 9.0, and the immobilized alkaline endoprotease was added, mixed and stirred for 4 hours. After the completion of the enzymatic hydrolysis, the immobilized alkaline endoprotease having magnetism is separated again. Heating to 90 ℃ and keeping for 10min.
And (3) centrifuging: centrifuging the obtained suspension at room temperature at 4500r/min for 10min, and collecting upper layer oil to obtain rapeseed oil.
Table 1 shows the extraction yield, color, acid value, peroxide value, moisture machine volatile components, and oxidation completion time of the rapeseed oil prepared in example 6 and comparative examples 1 to 2.
Table 2 shows the trace components of rapeseed oil prepared in example 6 and comparative examples 1-2.
TABLE 1 extraction yield, color, acid value, peroxide value, moisture machine volatile component, oxidation completion time of rapeseed oil prepared in example 6 and comparative examples 1-2
TABLE 2 micro-ingredients of rapeseed oil prepared in example 6 and comparative examples 1-2
As shown in the table, the rapeseed oil prepared by the high-pressure pulse assisted low-temperature catalytic extraction has the oil yield reaching 84.21%, and has higher extraction rate compared with the rapeseed oil prepared by the non-traditional aqueous enzymatic method. The content of tocopherol is 900.40mg/kg, the content of plant polyphenol is 162.21mg/kg, the content of phytosterol is 6752.36mg/kg, the content of beta-carotene is 6.89mg/kg, which is higher than that of rapeseed oil which is not treated by a high-voltage alternating-current pulsed electric field, the oxidation induction time of the rapeseed oil prepared by the method is relatively longer and reaches 7-8 hours, the result is consistent with the content of trace components such as plant polyphenol, beta-carotene and the like in grease, and the trace components enable the rapeseed oil prepared by the method to have stronger oxidation stability, which means that the shelf life of the product is longer. The possible reasons are: the application uses the pulse electric field to change the permeability of the plant seed cell membrane, increases the oil yield, achieves the purposes of enzyme deactivation, demulsification and the like in a physical mode, has milder conditions compared with the common aqueous enzymatic method, and can furthest reserve the biological active substances such as tocopherol, polyphenol, antioxidant, phytosterol and the like in the rapeseeds. And meanwhile, the immobilized enzyme is used for enzymolysis, and the immobilized enzyme can be recycled by a simple method.
The foregoing has shown and described the basic principles, principal features and advantages of the application. The present application is not limited to the above-described embodiments, and the description in the above-described embodiments and the description is merely illustrative of the principles of the present application, and various changes and modifications may be made therein without departing from the spirit and scope of the application, which is defined in the appended claims. The scope of the application is defined by the appended claims and equivalents thereof.
Claims (10)
1. The device for preparing the aromatic rapeseed oil with the assistance of the high-voltage alternating-current pulse type electric field is characterized by comprising a main body (1); the main body (1) is provided with a servo motor (2), a feed inlet (3), a steel plate (4), a mixing rod (5), a rotary baffle plate (6), screening holes (7), an inclined plate (8), a pH detector (9), a temperature detector (10), a heating block (11), a magnetic enzyme recovery tank (12), a filter tank (13), a liquid storage tank (14), a controller (15), an acid adding pipeline (16), a water inlet pipe (19) and a discharge outlet (20);
the main body (1) comprises a first layer, a second layer, a third layer and a fourth layer from top to bottom, a rotary baffle is arranged between the layers, and steel plates (4) are symmetrically arranged in the first layer, the second layer and the fourth layer of the main body (1); the novel multifunctional filter is characterized in that a servo motor (2) is arranged in the main body (1), the lower end of the servo motor (2) is connected with a mixing rod (5), a heating block (11) is arranged in the second layer and the third layer, a pH detector (9) and a temperature detector (10) are arranged on the inner walls of the second layer and the third layer, screening holes (7) are formed in the left side and the right side of a rotary baffle between each layer of the main body (1), an inclined plate (8) is arranged at the lower end of the screening hole of the first layer of the main body (1), a surface magnetic enzyme recovery groove (12) is formed at the lower ends of the screening holes of the second layer and the third layer of the main body (1), the main body (1) is conveniently taken out in the form of a sliding block, a filter groove (13) is arranged at the bottom in the form of the sliding block, and a filter screen is arranged at the bottom of the filter groove (13);
the main body (1) further comprises an alkali adding pipeline (17) and an enzyme adding pipeline (18).
2. The device according to claim 1, characterized in that the connection between the body (1) and the servomotor (2) is a fixed connection, and the mixing bars (5) are evenly distributed along the vertical center line of the servomotor.
3. The device according to claim 1, characterized in that the inside of the body (1) is coated with an internal insulating material.
4. The device according to claim 1, wherein the steel plates (4) are symmetrically distributed on the insulating material in the main body, and the front surface of the main body is provided with a controller (15), and the connection mode between the controller (15) and the steel plates (4) is electric connection.
5. The device according to claim 1, wherein the screening holes (7) are uniformly distributed along two sides of the rotating baffle plate (6), the rotating baffle plate (6) is electrically connected with a controller (15), and the controller (15) controls the rotating baffle plate (6) to rotate.
6. The device according to claim 1, wherein the heating blocks (11) are distributed inside the main body (1) in a ring-shaped symmetrical manner, and the connection mode between the controller (15) and the heating blocks (11) is an electrical connection.
7. The device according to claim 1, wherein the magnetic enzyme recovery grooves (12) are distributed at the lower end of the screening hole (7), the magnetic enzyme recovery grooves (12) are provided with magnets, and a sliding structure is formed between the magnetic enzyme recovery grooves (12) and the main body (1).
8. The device according to claim 1, wherein the filter tanks (13) are distributed at the bottom of the main body (1), the bottom layer is provided with a filter screen, and a sliding structure is formed between the filter tanks (13) and the main body (1).
9. The device according to claim 1, characterized in that the outlet opening (20) is located at the side of the reservoir (14) and connected to a pump for discharging the liquid in the reservoir (14) out of the body (1).
10. The method for preparing the rapeseed oil at low temperature assisted by the high-voltage alternating-current pulsed electric field is characterized by comprising the following steps of:
(1) screening, cleaning, sun drying and pulverizing semen Brassicae campestris raw materials;
(2) carrying out pulse electric field pretreatment on crushed rapeseeds;
(3) adding water for mixing, and carrying out a second pulse electric field treatment on the mixture;
(4) adding immobilized cellulase, and separating and removing the immobilized cellulase after enzyme hydrolysis is finished;
(5) adding immobilized alkaline endoprotease, separating and removing the immobilized alkaline endoprotease after enzyme hydrolysis is finished;
(6) performing a third pulsed electric field treatment on the obtained mixture;
(7) centrifuging to obtain upper layer to obtain rapeseed oil;
the steps (2) - (7) are carried out in the device according to any one of claims 1-9;
in the step (6), demulsification treatment is performed by using a pulsed electric field, wherein the electric field strength is 35-40 kV/cm, the pulse frequency is 550-600 Hz, and the duty ratio is 0.6-0.7.
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| CN202210778915.XA CN115093895B (en) | 2022-06-30 | 2022-06-30 | Device and method for preparing rapeseed oil with assistance of high-voltage alternating-current pulsed electric field |
| PCT/CN2022/135462 WO2024001031A1 (en) | 2022-06-30 | 2022-11-30 | Device and method for preparing rapeseed oil with assistance of high-voltage alternating-current pulse electric field |
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| CN115491394B (en) * | 2022-10-24 | 2024-03-19 | 利诚检测认证集团股份有限公司 | Sample detection pretreatment method for enzymatic hydrolysis liquid grease |
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