CN115093895A - Device and method for preparing rapeseed oil by aid of high-voltage alternating-current pulse electric field - Google Patents
Device and method for preparing rapeseed oil by aid of high-voltage alternating-current pulse electric field Download PDFInfo
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Abstract
The invention provides a device and a method for preparing rapeseed oil with the assistance of a high-voltage alternating-current pulse electric field, which change the permeability of plant seed cell membranes by using the high-voltage alternating-current pulse electric field, increase the oil yield, achieve the effects of enzyme inactivation and emulsion breaking by using the high-voltage alternating-current pulse electric field, have the characteristics of simple process, low treatment temperature and the like, can reserve biological active substances such as tocopherol, polyphenol, antioxidant, phytosterol and the like in the rapeseed to the maximum extent, reduce the harm caused by high-temperature treatment, ensure the flavor of the rapeseed oil and improve the quality of the rapeseed oil. The immobilized enzyme prepared by the method can be recycled by a simple method, the enzyme can be reused, and the enzyme stability is improved.
Description
Technical Field
The invention relates to the technical field of grease processing, in particular to a device and a method for preparing rapeseed oil under the assistance of a high-voltage alternating-current pulse electric field.
Background
The rapeseed oil has fragrant smell and rich nutrition. The absorption rate of the rapeseed oil by human body is very high and can reach 99%. Has effects of tonifying deficiency, moistening intestine, removing liver fire, promoting gallbladder function, promoting brain development, resisting stimulation of various strong lights, and preventing senile ophthalmopathy 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 senility. The content of sterol is higher than that of common vegetable oil such as soybean oil, and the like, and the sterol has various varieties, and some sterols also have special physiological functions. The phospholipid of the rapeseed oil is beneficial to the development of blood vessels, nerves and brains, and the cholesterol of the rapeseed oil is little or almost free. The saturated fatty acid content of the low erucic acid rapeseed oil is very low, the oleic acid content is more than 60%, and the low erucic acid rapeseed oil has reasonable contents of linoleic acid and linolenic acid, so the low erucic acid rapeseed oil is called as 'healthiest edible vegetable oil'. Compared with the phytosterol content of other edible vegetable oil, the cholesterol content of the rapeseed oil is lower, and the contents of the brassicasterol, the campesterol and the stigmasterol which are beneficial to the health of a human body are the highest in the edible vegetable oil. The rapeseed polyphenol is an important secondary metabolite unique to rapeseeds, has biological activities of resisting tumors, reducing blood sugar, inhibiting bacteria, removing free radicals and the like, and is a potential important natural antioxidant.
At present, the oil preparation process of rapeseeds in China mostly adopts a high-temperature prepressing-leaching oil preparation process with shells. The product is crude oil and rapeseed cake. Due to high-temperature pre-pressing, the crude oil is mostly dark brown and needs to be refined, so the flavor and the nutrient components of the rapeseed oil are also lost to different degrees. In the leaching stage, the 6# solvent oil (the normal hexane content is about 30%) is mostly adopted at present, and along with the fact that the hexane is listed as a harmful air pollutant group, the extraction of the rapeseed oil by using the hexane is recently the focus of safety and environmental impact. At the laboratory and pilot industrial scale, aqueous enzymatic methods have been attempted for extracting oil from many oil seeds/fruits. Compared with the traditional technology, the process is mild and safe because organic solvents are completely avoided. Despite these advantages, the disadvantages of the aqueous enzymatic method are also evident. Firstly, the price of the enzyme preparation at the present stage is still higher, the production cost is increased, most of the aqueous enzymatic methods are stopped in the laboratory research and pilot plant test stages for many years, and the industrial application of the aqueous enzymatic methods is always limited. Secondly, in the process of extracting the vegetable oil, because cell walls are hard and thick and components are complex, the synergistic action of a plurality of enzymes is often needed, so that the wall breaking effect of part of oil is not good enough, and the oil extraction rate is low. In addition, in the process of extracting the oil by the aqueous enzymatic method, the residual oil rate in the formed emulsion layer and the residue layer is high, so that the oil extraction rate is low.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides a device and a method for preparing aromatic rapeseed oil by high-voltage alternating-current pulse type electric field assisted catalysis, which have the advantages of low treatment temperature, capability of retaining the flavor of the rapeseed oil to the maximum extent, and biological active substances such as tocopherol, polyphenol, antioxidant, phytosterol and the like.
The alternating current pulse electric field is used for changing the permeability of plant seed cell membranes and increasing the oil yield. Meanwhile, in the later stage of aqueous enzymatic extraction, the alternating-current pulse electric field can effectively increase the vibration and collision of liquid drops in oil, improve the coalescence efficiency of the liquid drops and have a better demulsification effect. In aqueous enzymatic extraction, immobilized enzymes are used instead of the conventional free form enzymes. Compared with free enzyme, the enzyme has good temperature and pH adaptability, and can be recycled by a simple method with little loss of enzyme activity. And the separation and purification from the product are easy.
The invention aims to provide a device for preparing aromatic rapeseed oil by using high-voltage alternating current pulse type electric field auxiliary extraction, which comprises a main body (1); the main part (1) is provided with a servo motor (2), a feed inlet (3), a steel plate (4), a mixing rod (5), a rotating baffle (6), a screening hole (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 port (20).
In one embodiment of the invention, 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 inside the first layer, the second layer and the fourth layer of the main body (1); main part (1) internally mounted has servo motor (2), and the lower extreme of servo motor (2) is connected with mixing rod (5), second floor and third layer are inside to be equipped with heating piece (11), second floor and third layer inner wall are equipped with pH detector (9) and temperature-detecting appearance (10), both sides all set up screening hole (7) about the rotating baffle between every layer of main part (1), main part (1) first layer screening hole lower extreme is provided with hang plate (8), main part (1) second, three-layer screening hole lower extreme set up surperficial magnetic enzyme accumulator (12), be convenient for take out with the form of slider, main part (1) is provided with filter tank (13), install in the bottom with the form of slider equally, filter tank (13) bottom has the filter screen.
In one embodiment of the invention, the main body (1) further comprises an alkali adding pipeline (17) and an enzyme adding pipeline (18).
In one embodiment of the invention, 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 invention, the inside of the body (1) is coated with an internal insulating material.
In one embodiment of the invention, 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).
In one embodiment of the invention, the screening holes (7) are uniformly distributed along two sides of the rotating baffle (6), the rotating baffle (6) is electrically connected with a controller (15), and the controller (15) controls the rotating baffle (6) to rotate.
In one embodiment of the present invention, the heating blocks (11) are circularly and symmetrically distributed inside the main body (1), and the controller (15) is electrically connected to the heating blocks (11).
In one embodiment of the invention, the magnetic enzyme recovery groove (12) is distributed at the lower end of the screening hole (7), the magnetic enzyme recovery groove (12) is provided with a magnet, and a sliding structure is formed between the magnetic enzyme recovery groove (12) and the main body (1).
In one embodiment of the invention, the filter tanks (13) are distributed at the bottom of the main body (1), the filter screen is arranged at the bottom layer, and a sliding structure is formed between the filter tanks (13) and the main body (1).
In one embodiment of the invention, the discharge port (20) is located on the side of the reservoir (14) and is connected with a pump to discharge the liquid in the reservoir (14) out of the main body (1).
The second purpose of this document is to provide a method for preparing aromatic rapeseed oil with the aid of high-voltage alternating-current pulse electric field, which comprises the following steps:
firstly, screening, cleaning, drying and crushing the rapeseed raw material;
secondly, performing pulse electric field pretreatment on the crushed rapeseeds;
thirdly, adding water for mixing, and carrying out secondary pulse electric field treatment on the mixture;
adding immobilized cellulase, and separating and removing the immobilized enzyme after the enzymatic hydrolysis is finished;
adding immobilized alkaline endoprotease, and separating and removing the immobilized enzyme after the enzymatic hydrolysis is finished;
sixthly, performing third pulse electric field treatment on the obtained mixture;
and seventhly, centrifugally separating to obtain an upper layer, thus obtaining the rapeseed oil.
In one embodiment of the invention, when the rapeseed oil is prepared by using the device, a user firstly inserts the enzyme recovery tank (12) and the filter tank (13) into the main body (1), then pours the crushed rapeseed into the main body (1) along the feed inlet (3), and simultaneously, the user turns on the servo motor (2), and the servo motor (2) is matched with the mixing rod (5) to uniformly mix the materials, and then a high-voltage alternating-current pulse type electric field is formed between the steel plates (4) on the first layer of the main body (1) through the command of the controller (15), so that the plant cell walls are damaged to release more grease;
then, a rotary baffle (6) is arranged to open an exposure screening hole (7), materials slide into a second layer of the main body (1) along an inclined plate (8), a controller (15) commands a water inlet pipeline (19) to be opened, a high-voltage alternating current pulse type electric field is formed between second layer steel plates (4) of the main body (1), the temperature and the pH of the material liquid are monitored by a pH detector (9) and a temperature detector (10), the controller opens a set acid adding pipeline (16) and a set alkali adding pipeline (17) to adjust the pH, and commands a heating block (12) to start to adjust the temperature, and then immobilized cellulase is released through a set enzyme adding pipeline (18) to be treated;
after the treatment is finished, a rotary baffle (6) is arranged to open an exposure screening hole (7), materials slide into the third layer of the main body (1) along the inclined surface of an enzyme recovery tank (12), wherein immobilized cellulase is attached to the recovery tank due to the magnetism on the surface of the recovery tank (12), the temperature and the pH of the feed liquid are monitored by a pH detector (9) and a temperature detector (10), a controller opens an acid addition pipeline (16) and an alkali addition pipeline (17) to adjust the pH, a heating block (12) is commanded to start to adjust the temperature, and then immobilized alkaline endoprotease is released through the enzyme addition pipeline to carry out treatment;
after the treatment is finished, the arranged rotary baffle (6) opens the exposure screening hole (7), the material slides 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) on the fourth layer of the main body (1) through the command of the controller (15) to achieve the demulsification effect;
after the demulsification treatment is finished, the rotary baffle (6) is arranged to open the exposure filter tank (13), the feed liquid flows out along the discharge hole (20) through the liquid storage tank (14) under the action of the main body (1) outer pump, the solid matters 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, the solid matter residues and the enzymes can be conveniently treated, and the whole process for preparing the rapeseed oil by using the device is finished.
In one embodiment of the invention, in the second step, the plasma membrane permeability of rapeseed cells is increased by electrical stimulation by using a high-voltage alternating current pulse type electric field, the plant cell structure is damaged, and the way of dissolving out intracellular substances is increased.
In one embodiment of the invention, in the second step, 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 invention, in the step III, a pulse electric field is used for replacing the traditional high-temperature enzyme deactivation process, so that the loss of partial flavor and nutrient substances is avoided.
In one embodiment of the present invention, in the step (c), the ratio of the oil material to the water is 1: 3-5 (w/v, g/mL).
In one embodiment of the invention, in the third step, the electric field strength is 65-75 kV/cm, the pulse frequency is 750-850 Hz, and the duty ratio is 0.5-0.6.
In one embodiment of the invention, in the step (iv), the immobilized cellulase used is immobilized by ferroferric oxide nanoparticles containing a carrier.
In one embodiment of the invention, in the step IV, the temperature of the enzymatic hydrolysis is 40-45 ℃, the pH value is 7.5-8.0, and the stirring is carried out for 1-2 hours.
In one embodiment of the present invention, in the fifth step, the immobilized alkaline endoprotease is immobilized by carrier-containing ferroferric oxide nanoparticles.
In an embodiment of the present invention, in the fifth step, the temperature of the enzymatic hydrolysis is 60 to 65 ℃, the pH is 8.5 to 9.0, and the mixture is stirred for 4 to 4.5 hours.
In one embodiment of the invention, in the step (sixthly), 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 invention, in the step (sixty), the preferred electric field strength is 40kV/cm, the pulse frequency is 600Hz, and the duty ratio is 0.7.
In one embodiment of the present invention, in the step (c), the centrifugation speed is 4500-6000 r/min, and the centrifugation is performed at room temperature for 10-20 min.
Has the advantages that:
the rapeseed oil is extracted by adopting an aqueous enzymatic method, and the cellular structure of oil material tissue and the ultramicro structure of lipopolysaccharide and lipoprotein are degraded by adopting biological enzyme, so that the fluidity of oil in the oil material tissue is increased, the oil is dissociated from the oil material, phenols and other substances are further promoted to enter the oil, and some proteins and phenols are prevented from being oxidized due to the protection of a water phase and an emulsion layer in the extraction process, so that the oxidation stability, shelf life, nutrition, flavor, sense and other properties of the oil are further improved.
The method disclosed by the invention applies the high-voltage alternating-current pulse type electric field treatment technology for three times, performs the high-voltage alternating-current pulse type electric field treatment on the oil seeds for the first time, replaces the traditional steaming and frying process, is mild in condition, generates high-voltage current through discharging, destroys plant cells, changes the permeability of the plant cells, enables substances in the cells to effectively flow out, promotes the release of volatile components, improves the flavor of oil gas, and improves the oil extraction rate and the oil flavor of a subsequent pressing process. And performing high-voltage alternating-current pulse type electric field treatment on the mixed system of the oil material and the water for the second time to enable the mixed system to be dispersed more uniformly in the water, and simultaneously utilizing the action of an instantaneous pulse electric field on microbial cells to enable cell membranes to form pores, enhance permeability, expand the cells, finally break the cells to inactivate the microbes and passivate enzymes contained in the system. Compared with the traditional high-temperature enzyme deactivation, the high-voltage alternating-current pulse type electric field is cold treatment, can sterilize and deactivate the enzyme while preserving the inherent components of the rapeseeds, and saves energy consumption. The third pulsed electric field treatment has the functions of sterilization and enzyme deactivation, can effectively increase the vibration and collision of liquid drops in the oil, improve the coalescence efficiency of the liquid drops, play a role in demulsification, and simultaneously can adjust parameters such as electric field intensity, pulse frequency and space-to-space ratio according to the working condition of the oil so as to obtain the optimal demulsification effect.
The enzyme adopted by the invention is a self-made immobilized enzyme, the cellulase and the alkaline endoprotease are immobilized by the ferroferric oxide nano-particles containing the carrier, and the enzyme has magnetism and is convenient to recover, so that the enzyme can be repeatedly utilized, the production cost is reduced, and the production efficiency is improved.
The device of the invention can uniformly mix the rapeseeds by the mutual matching of the arranged servo motor and the mixing rod, and the arranged rotating baffle and the filtering holes are mutually matched to control the treatment time and the flow rate.
Through the enzyme accumulator and the filter tank that set up sliding construction, improve the recovery efficiency of enzyme, utilize the filter tank to detach the solid matter, reduce centrifugal operation's the degree of difficulty and avoid impurity to influence the purity of follow-up oil, the sliding construction that sets up moreover can conveniently wash and change it.
Drawings
FIG. 1 Process flow diagram of the process of the invention
FIG. 2 emulsion breaking ratio under electric field treatment of different strengths
FIG. 3 emulsion breaking rate under electric field treatment of different pulse frequencies
FIG. 4 emulsion breaking rate under electric field treatment of different duty ratios
FIG. 5 is a schematic view of the structure of the device of the present invention
FIG. 6 is an external view of the device of the present invention
FIG. 7 is a schematic cross-sectional view of the device of the present invention
In the figure: (1) a main body; (2) a servo motor; (3) a feed inlet; (4) a steel plate; (5) a mixing rod; (6) rotating the baffle; (7) a screening well; (8) an inclined plate; (9) a pH detector; (10) a temperature detector; (11) a heating block; (12) a magnetic enzyme recovery tank; (13) a filter tank; (14) a liquid storage tank; (15) a controller; (16) an acid addition conduit; (17) an alkali addition conduit; (18) an enzyme addition conduit; (19) a water inlet pipe; (20) and (4) discharging a material outlet.
Detailed Description
The color and luster of the rapeseed oil is determined by reference to GB/T22460-; the acid value determination refers to GB/T5530 and 2005 animal and vegetable oil acid value and acidity determination; the determination of the peroxide value refers to GB/T5538-; the water content and the volatile matter content are referred to GB/T5528-2008. The oxidation stability is measured by reference to NY/T2001-2011 accelerated oxidation test for measuring the oxidation stability of rapeseed oil; the measurement of polyphenol content refers to LS/T6119 and 2017 spectrophotometry for measuring polyphenol in vegetable oil by grain and oil; the demulsification rate measuring method comprises the following steps: 5g of rapeseed emulsion is weighed by a 50mL beaker, treated by a high-voltage alternating current pulse type electric field with certain electric field intensity, electric field frequency and duty ratio and then taken out. Centrifuging at 4500r/min at room temperature for 10min to obtain free oil, water phase mixed solution and residue, and demulsifying rate is calculated according to the following formula (1). The oil yield was calculated by the following formula (2):
the principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
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 strong fragrant rapeseed oil of high pressure alternating current pulse type electric field assisted catalytic extraction preparation, main part (1) is provided with servo motor (2), feed inlet (3), steel sheet (4), mixing rod (5), rotating baffle (6), screening hole (7), hang plate (8), pH detector (9), temperature detector (10), heating block (11), magnetism enzyme accumulator (12), filter-tank (13), reservoir (14), controller (15), sour interpolation 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 inside the first layer, the second layer and the fourth layer of the main body (1); main part (1) internally mounted has servo motor (2), and the lower extreme of servo motor (2) is connected with mixing rod (5), second floor and third layer are inside to be equipped with heating piece (11), second floor and third layer inner wall are equipped with pH detector (9) and temperature-detecting appearance (10), both sides all set up screening hole (7) about the rotating baffle between every layer of main part (1), main part (1) first layer screening hole lower extreme is provided with hang plate (8), main part (1) second, three-layer screening hole lower extreme set up surperficial magnetic enzyme accumulator (12), be convenient for take out with the form of slider, main part (1) is provided with filter tank (13), install in the bottom with the form of slider equally, filter tank (13) bottom has the filter screen.
The main body (1) also comprises an alkali adding pipeline (17) and an enzyme adding pipeline (18).
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.
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).
Screening hole (7) are along rotating barriers (6) both sides evenly distributed, rotating barriers (6) and controller (15) electric connection, controller (15) control rotating barriers (6) are rotatory.
The heating blocks (11) are annularly and symmetrically distributed inside the main body (1), and the controller (15) is electrically connected with the heating blocks (11).
The magnetic enzyme recovery groove (12) is distributed at the lower end of the screening hole (7), the magnetic enzyme recovery groove (12) is provided with a magnet, and a sliding structure is formed between the magnetic enzyme recovery groove (12) and the main body (1).
The filter tank (13) is distributed at the bottom of the main body (1), a filter screen is arranged at the bottom layer, and a sliding structure is formed between the filter tank (13) and the main body (1).
The discharge port (20) is positioned on the side surface of the liquid storage tank (14) and is connected with the pump to discharge the liquid in the liquid storage tank (14) out of the main body (1).
The working principle is as follows: for the rapeseed oil preparation device, before use, a user firstly inserts the enzyme recovery tank (12) and the filter tank (13) into the main body (1), then pours the crushed rapeseed into the main body (1) along the feed inlet (3), meanwhile, the user turns on the servo motor (2), the servo motor (2) is matched with the mixing rod (5) to enable the materials to be uniformly mixed, and then a high-voltage alternating-current pulse type electric field is formed between the steel plates (4) on the first layer of the main body (1) through a command of the controller (15) to damage plant cell walls and release more grease. And then, a rotary baffle (6) is arranged to open and expose a screening hole (7), materials slide into the second layer of the main body (1) along an inclined plate (8), a water inlet pipeline (19) is commanded to be opened through a controller (15), a high-voltage alternating-current pulse type electric field is formed between the steel plates (4) of the second layer of the main body (1), the temperature and the pH of the feed liquid are monitored through a pH detector (9) and a temperature detector (10), the controller opens a set acid adding pipeline (16) and a set alkali adding pipeline (17) to adjust the pH, a heating block (12) is commanded to start to adjust the temperature, and then enzyme A is released through a set enzyme adding pipeline (18). After a period of treatment, a rotary baffle (6) is arranged to open and expose a screening hole (7), materials slide into the third layer of the main body (1) along the inclined surface of an enzyme recovery tank (12), wherein an enzyme A is attached to the recovery tank due to magnetism on the surface of the recovery tank (12), the temperature and the pH of the feed liquid are monitored by a pH detector (9) and a temperature detector (10), a controller opens an acid addition pipeline (16) and an alkali addition pipeline (17) to adjust the pH, a heating block (12) is commanded to start to adjust the temperature, and then an enzyme B is released through the enzyme addition pipeline. After the treatment for a period of time, the rotary baffle (6) is arranged to open and expose the screening hole (7), the material slides into the fourth layer of the main body (1) along the inclined surface of the recovery tank (12), wherein the enzyme B 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) on the fourth layer of the main body (1) through the command of the controller (15) to achieve the demulsification effect. After a period of time is processed, the rotary baffle (6) is arranged to open the exposed filter tank (13), the feed liquid flows out along the discharge hole (20) through the liquid storage tank (14) under the action of the main body (1) outer pump, the solid matters are attached to the filter tank (13), after the use, the device is closed, the enzyme recovery tank (12) and the filter tank (13) are pulled open, the solid matter residues and the enzymes can be conveniently processed, and the use process of the whole oil production device is completed.
Example 2: preparation of immobilized enzymes
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 30 min. The mixture was heated to 80 ℃ and stirred under nitrogen atmosphere for 1 h. The ferrofluid was further ultrasonically dispersed for 20min and purified by centrifugation to remove a few large agglomerates (1000 Xg, 10 min). Adding 10mL of alkaline endoprotease (30000U) or cellulase (30000U) solution into 100mL of magnetic fluid, mixing well, and injecting the ferrofluid into 10 wt% CaCl by using an injector 2 In aqueous solution, preparing magnetic microspheres. Soaking the magnetic microspheres for 1h, washing with distilled water, and removing the adhesiveFree Ca on the surface 2+ Then crosslinked with 0.5% glutaraldehyde for 1.5h, and washed with distilled water. Finally, the microspheres were allowed to harden by incubating overnight at 4 ℃. Drying at 35 deg.C for 12h to obtain immobilized enzyme.
Example 3
Firstly, screening, cleaning and removing impurities such as weed seeds, cereal seeds, seed shells and the like in the rapeseed raw material; cleaning, namely cleaning the screened rapeseed with clear water, washing off dust on the surface of the rapeseed, draining, and drying in the sun; crushing, and grinding the dried rapeseeds by a grinder.
The first high-voltage alternating current pulse type electric field treatment: the crushed rapeseeds are pretreated by a high-voltage alternating-current pulse electric field, the intensity of the voltage pulse electric field is 25kV/cm, the retention time of materials is 180s, the pulse frequency is 850Hz, and the duty ratio is 0.5.
Third, the second high voltage alternating current pulse type electric field treatment: 5g of the treated rapeseed was mixed with distilled water at a mass ratio of 1:3(w/v, g/mL). The mixture is treated by a high-voltage alternating-current pulse type electric field, the intensity of the voltage pulse electric field is 75kV/cm, the pulse frequency is 850Hz, and the duty ratio is 0.5.
Fourthly, first enzyme treatment: heating to 40 deg.C, adjusting pH to 8.0, adding immobilized cellulase, and stirring at 40 deg.C for 1 hr. Separating the immobilized cellulase with magnetism.
And fifthly, second enzyme treatment: the temperature is reduced to 60 ℃, the pH value is adjusted to 9.0, the immobilized alkaline endoprotease is added, and the mixture is mixed and stirred for 4 hours. After the enzymatic hydrolysis is finished, the immobilized alkaline endoprotease with magnetism is separated.
Sixthly, high-voltage pulse treatment for the third time: and (3) carrying out high-voltage alternating-current pulse type electric field treatment on the mixture after the immobilized enzyme is separated, wherein the voltage pulse electric field strength is 40kV/cm, the pulse frequency is 600Hz, and the duty ratio is 0.7.
And (c) centrifuging. Centrifuging the obtained suspension at 4500r/min for 10min at room temperature, and collecting the upper layer oil to obtain rapeseed oil.
Example 4: high-voltage alternating-current pulse type electric field demulsification condition (electric field intensity) optimization
(1) - (5) Steps (1) to (5) of example 3;
(6) and (3) high-voltage pulse treatment for the third time: performing high-voltage alternating-current pulse type electric field treatment on the mixture after the immobilized enzyme is separated, wherein the intensity of the high-voltage pulse electric field 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 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) of example 3;
(6) and (3) high-voltage pulse treatment for the third time: performing high-voltage alternating current pulse type electric field treatment on the mixture after the immobilized enzyme is separated, wherein the electric field intensity of the high-voltage alternating current pulse type electric field is 40kV/cm, the pulse frequency is 300, 350, 400, 450, 500, 550, 600, 650, 700 and 750Hz, and the duty ratio is 0.7;
(7) centrifuging the obtained suspension at 4500r/min for 10min to obtain free oil, water phase mixed solution and residue, and calculating demulsification rate.
Example 6: high voltage ac pulse type electric field demulsification and demulsification (duty ratio) optimization
(1) - (5) Steps (1) to (5) of example 3;
(6) and (3) high-voltage pulse treatment for the third time: carrying out high-voltage alternating-current pulse type electric field treatment on the mixture after the immobilized enzyme is separated, wherein the electric field intensity of the high-voltage alternating-current pulse type electric field 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 4500r/min for 10min to obtain free oil, water phase mixed solution and residue, and calculating demulsification rate.
Comparative example 1: traditional aqueous enzymatic method
Screening: cleaning to remove a small amount of weed seeds, cereal seeds, seed shells and the like.
Cleaning: cleaning the screened rapeseed with clear water, washing off dust on the surface of the rapeseed, draining, and drying in the sun.
Crushing: the air-dried rapeseed was pulverized by a grinder.
Adding water and mixing: 5g of the treated rapeseed was mixed with distilled water at a mass ratio of 1:3(w/v, g/mL) and boiled for 4 min.
First enzyme treatment: heating to 50 deg.C, adjusting pH to 6.0, adding cellulase, and stirring at 50 deg.C for 1 hr.
And (3) second enzyme treatment: the temperature was raised to 60 ℃ and the pH was adjusted to 9.0, immobilized alkaline endoprotease was added, mixed and stirred for 4 hours. The temperature is raised to 90 ℃ and kept for 10 min.
Centrifuging: centrifuging the obtained suspension at 4500r/min for 10min, and collecting the upper layer oil to obtain oleum Rapae.
Comparative example 2: using immobilized enzymes (without treatment by high voltage AC pulse type electric field)
Screening: cleaning to remove a small amount of weed seeds, cereal seeds, seed shells and the like.
Cleaning: cleaning the screened rapeseed with clear water, washing off dust on the surface of the rapeseed, draining, and drying in the sun.
Crushing: the air-dried rapeseed was pulverized by a grinder.
Adding water and mixing: 5g of the treated rapeseed was mixed with distilled water at a mass ratio of 1:3(w/v, g/mL) and boiled for 4 min.
First enzyme treatment: heating to 40 deg.C, adjusting pH to 8.0, adding immobilized cellulase, and stirring at 40 deg.C for 1 hr. Separating the immobilized cellulase with magnetism.
And (3) second enzyme treatment: the temperature is reduced to 60 ℃, the pH is adjusted to 9.0, the immobilized alkaline endoprotease is added, and the mixture is mixed and stirred for 4 hours. After the enzymatic hydrolysis is finished, the magnetic immobilized alkaline endoprotease is separated again. The temperature is raised to 90 ℃ and kept for 10 min.
Centrifuging: centrifuging the obtained suspension at 4500r/min for 10min, and collecting the upper layer oil to obtain oleum Rapae.
Table 1 shows the extraction yield, color, acid value, peroxide number, moisture content, and oxidation completion time of rapeseed oil prepared in example 6 and comparative examples 1-2.
Table 2 shows the minor constituents of rapeseed oil obtained in example 6 and comparative examples 1-2.
TABLE 1 extraction yield, color, acid value, peroxide number, moisture content, volatile content, oxidation completion time of rapeseed oil prepared in example 6 and comparative examples 1-2
Table 2 minor constituents of rapeseed oil obtained in example 6 and comparative examples 1-2
From the above table, the rapeseed oil prepared by the high-voltage pulse assisted low-temperature catalytic extraction method has an oil yield of 84.21%, and has a higher extraction rate compared with that of rapeseed oil prepared by a conventional aqueous enzymatic method. The content of the tocopherol is 900.40mg/kg, the content of the plant polyphenol is 162.21mg/kg, the content of the phytosterol is 6752.36mg/kg, and the content of the beta-carotene is 6.89mg/kg, which are higher than those of rapeseed oil which is not treated by a high-voltage alternating current pulse type 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 the plant polyphenol, the beta-carotene and the like in oil, 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 rapeseed oil is longer. The possible reasons are: the invention utilizes the pulse electric field to change the permeability of the plant seed cell membrane, increases the oil yield, achieves the purposes of enzyme inactivation, emulsion breaking and the like in a physical mode, has milder conditions compared with the common aqueous enzymatic method, and can furthest retain the biological active substances such as tocopherol, polyphenol, antioxidant, phytosterol and the like in the rapeseed. Meanwhile, the enzymolysis is carried out by using immobilized enzyme, and the enzyme can be recycled by a simple method.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. The present invention is not limited to the above-described embodiments, and the above-described embodiments and the description in the specification are only illustrative of the principle of the present invention, and various changes and modifications may be made to the present invention without departing from the spirit and scope of the present invention, and these changes and modifications fall within the scope of the claimed invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A device for preparing aromatic rapeseed oil by using a 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 feeding hole (3), a steel plate (4), a mixing rod (5), a rotary baffle (6), a screening hole (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 discharging hole (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 inside the first layer, the second layer and the fourth layer of the main body (1); the automatic cleaning device is characterized in that a servo motor (2) is installed inside the main body (1), the lower end of the servo motor (2) is connected with a mixing rod (5), heating blocks (11) are installed inside the second layer and the third layer, a pH detector (9) and a temperature detector (10) are installed 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 every two layers of the main body (1), an inclined plate (8) is arranged at the lower end of a first layer of screening hole of the main body (1), a surface magnetic enzyme recovery tank (12) is arranged at the lower end of the second layer of screening hole and the lower end of the third layer of the main body (1) and is convenient to take out in a sliding block mode, the main body (1) is provided with a filter tank (13) which is also installed at the bottom in a sliding block mode, and a filter screen is arranged at the bottom of the filter tank (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 servo motor (2) is a fixed connection and the mixing rods (5) are evenly distributed along the vertical centre line of the servo motor.
3. Device according to claim 1, characterized in that the body (1) is internally 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 inside 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).
5. The device according to claim 1, wherein the screening holes (7) are evenly distributed along two sides of the rotating baffle (6), the rotating baffle (6) is electrically connected with a controller (15), and the controller (15) controls the rotating baffle (6) to rotate.
6. The device according to claim 1, wherein the heating blocks (11) are circularly and symmetrically distributed in the main body (1), and the controller (15) is electrically connected with the heating blocks (11).
7. The device according to claim 1, wherein the magnetic enzyme recovery groove (12) is distributed at the lower end of the screening hole (7), the magnetic enzyme recovery groove (12) is provided with a magnet, and a sliding structure is formed between the magnetic enzyme recovery groove (12) and the main body (1).
8. The device according to claim 1, characterized in that the filter tank (13) is distributed at the bottom of the main body (1), a filter screen is arranged at the bottom layer, and a sliding structure is formed between the filter tank (13) and the main body (1).
9. A device according to claim 1, wherein the outlet (20) is located on the side of the reservoir (14) and connected to a pump for displacing liquid from the reservoir (14) out of the body (1).
10. A method for preparing rapeseed oil by using a high-voltage alternating-current pulse electric field to assist low temperature is characterized by comprising the following steps:
firstly, screening, cleaning, drying and crushing the rapeseed raw material;
secondly, performing pulsed electric field pretreatment on the crushed rapeseed;
thirdly, adding water for mixing, and carrying out secondary pulse electric field treatment on the mixture;
fourthly, adding immobilized cellulase, and separating and removing the immobilized cellulase after the enzymatic hydrolysis is finished;
adding immobilized alkaline endoprotease, and separating and removing the immobilized alkaline endoprotease after the enzymatic hydrolysis is finished;
sixthly, performing third pulsed electric field treatment on the obtained mixture;
seventhly, centrifugally separating and taking the upper layer to obtain the rapeseed oil;
(vii) the steps (c) to (c) are performed in the apparatus of claims 1 to 9;
and sixthly, performing demulsification treatment by using a pulse electric field, wherein the electric field intensity 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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