CN112010921B - Two-stage foam flotation method for concentrating and separating protein in perilla cake - Google Patents
Two-stage foam flotation method for concentrating and separating protein in perilla cake Download PDFInfo
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Abstract
The invention provides a method for concentrating and separating protein in perilla cake by a two-stage froth flotation method, which comprises the following steps: firstly, preparing a perilla cake leaching liquor; secondly, the first-stage foam flotation utilizes a foam flotation tower provided with an hourglass-shaped component to strengthen foam drainage and improve the enrichment ratio of the perilla protein, and the obtained concentrated solution can be directly used as a raw material for producing the perilla protein powder; and step three, the second-stage froth flotation takes the residual liquid of the first stage as a feed liquid, so that the recovery effect of the perilla protein is further improved. The method has the advantages of greenization of the process, low energy consumption, low investment, simple steps and the like, effectively solves the problem of concentration and separation of the perilla protein, and has good economic and social benefits.
Description
Technical Field
The invention relates to the field of recovery and concentration of waste protein in a chemical separation process, in particular to a method for concentrating and separating protein in perilla cake by a two-stage froth flotation method.
Background
Perilla frutescens L is one of the plants for both food and medicine issued by the national ministry of health, and plays an important role in the large health industry and functional agricultural construction. The by-product of perilla seed oil extraction and degreasing, namely perilla cake, has high protein content (28-45%), the composition mode of essential amino acid meets the standards specified by FAO (food and agriculture organization of the United nations) and WHO (world health organization), and the by-product is not like rapeseed meal and cottonseed meal protein containing toxic components such as glucosinolate, gossypol and the like, is a high-quality plant protein resource, and can be widely applied to the fields of food, biology, medicine and the like. At present, because of the shortage of concentration and separation means, perilla cake protein (hereinafter referred to as perilla protein) is mainly used as animal feed or crop fertilizer and is very limited in high-value utilization.
At present, the representative methods for separating perilla protein from perilla cake meal are as follows: the peridium protein is extracted, recovered and purified by adopting an ultrafiltration membrane technology (application number: CN 200910147929.6); ② Lijianhua et al (application number: CN201310301136.1) develop a supercritical extraction process for separating perilla protein; ③ Wei-Guojiang et al (application number: CN201610825294.0) through alkali-dissolving, acid-precipitating, removing impurities, deodorizing, and spray-drying. However, the membrane is easy to block due to high solution viscosity in the process of separating the perilla protein by the ultrafiltration membrane; the supercritical extraction method needs high-pressure equipment, the investment is large, and the industrialization difficulty is high; the alkali-soluble acid precipitation method not only can cause protein denaturation, but also consumes a large amount of acid and water, and increases the purification difficulty. More importantly, although the above patents achieve high-efficiency separation of perillain, none of them have performed concentration treatment on perillain. In fact, the enrichment degree of the perilla protein is an important index for determining whether the perilla protein can be effectively purified and then be produced, so that the development of an efficient, green and low-cost concentration method is very important for separating the protein in the perilla cake.
The froth flotation has the obvious engineering advantages of simple equipment, no pollution, low energy consumption and the like, is a main means in the field of recovery and concentration of surface active substances, and is successfully used for separating whey protein (application number: CN201810454523.1) in whey wastewater and concentrating and preparing soybean protein (application numbers: CN201010173810.9 and CN201310531012.2) in soybean protein wastewater, however, the froth flotation is not used for recovery and enrichment of perilla protein at present.
Disclosure of Invention
The invention aims to provide a two-stage foam flotation method for concentrating and separating protein from perilla cake pulp, aiming at the defects of the current perilla protein separation and concentration technology. The method adopts a flotation tower with better foam drainage effect to replace a flotation tank, and takes the flotation tower provided with internal components as a first-stage foam flotation device to strengthen foam drainage and reduce the volume of defoaming solution, thereby enriching perilla protein to a high degree and simplifying the subsequent purification steps; and then, a flotation tower which is not added and constructed is used as a second-stage froth flotation device, so that the recovery rate of the perilla protein is further improved. The invention overcomes the defects of poor concentration effect, high equipment cost, complex process, easy environmental pollution and the like of other protein separation technologies. In particular, the method comprises the following steps of,
the invention provides a two-stage froth flotation method for concentrating and separating protein in perilla cake, which comprises the following steps:
preparing a perilla cake leaching liquor;
performing intermittent froth flotation, preferably two-stage froth flotation, on the obtained perilla cake leaching liquor,
performing primary foam flotation by taking the perilla cake leaching liquor as a primary feeding liquid, collecting foam and defoaming to obtain a primary defoaming liquid, namely a perilla protein concentrated solution, performing secondary foam flotation by taking residual liquid of the primary foam flotation as a secondary feeding liquid, collecting foam and defoaming to obtain a secondary defoaming liquid;
the apparent air speed of the first-stage froth flotation is 0.3-0.7 mm/s, preferably 0.4-0.6mm/s, and the aeration is stopped when the froth cannot flow out; the operation time of the first-stage froth flotation is preferably 0.8-2 h, and further preferably 1.3-2 h.
The apparent air speed of the second-stage froth flotation is 0.7-1.1 mm/s, preferably 0.7-1.0 mm/s, and the aeration is stopped when the froth cannot flow out. The operation time of the second-stage froth flotation is preferably 2.0-3.0 h, and more preferably 2.1-2.6 h.
Preferably, the second stage defoaming solution can be used as the first stage feeding solution alone or together with the perilla cake leaching solution.
Preferably, the preparation of the perilla cake leaching liquor comprises the steps of adding water into perilla cake according to a material-liquid ratio of 1: 0.6-1: 1(g/L), adjusting the pH value to 8.5-9.5, stirring, centrifuging, and taking supernatant to adjust the pH value to 6.5-7.5.
Preferably, the stirring is carried out at the temperature of 30-40 ℃ and the rotating speed of 300-500 r/min for 0.6-1 h.
Preferably, the centrifugation is performed for 5min at 5000 r/min.
Preferably, the first-stage froth flotation is performed in a hollow cylindrical first-stage froth flotation tower, the height-diameter ratio of the first-stage froth flotation tower is 25-35: 1, an hourglass-shaped member is installed in the first-stage froth flotation tower and is formed by butt joint of two identical hollow bottomless circular truncated cones, the edge of the bottom surface is in seamless connection with the inner wall of the first-stage froth flotation tower, the diameter of the top surface of the circular truncated cone is smaller than that of the bottom surface, the diameter of the bottom surface is equal to that of the first-stage froth flotation tower, the vertical height of the hourglass-shaped member is 1/4 of the height of a froth phase, and the junction of the two circular truncated cones is located in the middle of the froth phase. Preferably, the diameter of the top surface of the circular truncated cone is 1/2 of the diameter of the bottom surface.
In one embodiment of the invention, the diameter of the first stage froth flotation tower is 40-60 mm, and the height of the first stage froth flotation tower is 1.2-1.6 m.
Preferably, the second-stage froth flotation is carried out in a hollow cylindrical second-stage froth flotation tower, and the height-diameter ratio of the second-stage froth flotation tower is 10-20: 1.
Further preferably, the diameter of the second-stage froth flotation tower is 60-80 mm, the height is 0.8-1.2 m, and more preferably 0.9-1.1 m.
Preferably, the height of the froth layer of the first-stage froth flotation is 3/5-4/5 of the height of the first-stage froth flotation tower.
In one embodiment of the invention, the height of the froth layer of the first stage froth flotation is 0.8-1.2 m.
Preferably, the height of the froth layer of the second-stage froth flotation is 2/5-3/5 of the height of the second-stage froth flotation tower.
In one embodiment of the invention, the froth layer height of the second stage froth flotation is 0.4-0.7 m.
Preferably, the perilla cake meal is perilla cake meal powder which is obtained by deoiling dried perilla seeds and then crushing.
Preferably, the purple perilla is planted in a village test field in the Shanghai Taiyuan lawn area of Shanxi province, and is dried in a 50 ℃ ventilation drying oven for 72 hours for standby after seeds are collected.
Preferably, the defoaming can be performed by any defoaming method known to those skilled in the art without affecting the quality of the product. Such as mechanical defoaming.
In one embodiment of the present invention, the two-stage froth flotation process comprises the steps of:
removing impurities from dried perilla seeds, squeezing at low temperature, deoiling, crushing, sieving with a 80-mesh sieve to obtain perilla cake meal powder, adding water into the perilla cake meal powder according to a material-liquid ratio of 1: 0.6-1: 1(g/L), adjusting the pH value to 8.5-9.5 by using a sodium hydroxide solution, stirring for 0.6-1 h at 30-40 ℃ and 300-500 r/min, cooling to room temperature, centrifuging for 5min at 5000r/min, taking supernatant, adjusting the pH value to 6.5-7.5 by using a hydrochloric acid solution to obtain a perilla cake meal leaching liquor;
injecting the perilla cake leaching liquor serving as a first-stage feeding liquid into a first-stage foam flotation tower, performing first-stage foam flotation at room temperature, collecting and defoaming foam flowing out of the top of the tower, stopping ventilation when the foam cannot flow out of the top of the flotation tower, and defoaming the foam collected from the top of the tower to obtain a first-stage defoaming liquid, wherein the apparent air speed is 0.3-0.7 mm/s, preferably 0.4-0.6mm/s, and the height of a foam layer is 3/5-4/5 of the height of the first-stage foam flotation tower; preferably, the operation time of the first-stage froth flotation is 0.8-2 h, preferably 1.3-2 h.
Injecting residual liquid discharged from the bottom of the first-stage foam flotation tower into a second-stage foam flotation tower, performing second-stage foam flotation at room temperature, wherein the apparent air speed is 0.7-1.1 mm/s, preferably 0.7-1.0 mm/s, the height of a foam layer is 2/5-3/5 the height of the second-stage foam flotation tower, collecting and defoaming foam flowing out of the top of the tower, stopping ventilation when the foam cannot flow out of the top of the second-stage foam flotation tower, defoaming the foam collected from the top of the tower to obtain liquid serving as second-stage defoaming liquid, and combining the second-stage defoaming liquid and perilla cake leaching liquor to serve as first-stage feeding liquid. Preferably, the operation time of the second-stage froth flotation is 2.0-3.0 h, and further preferably 2.1-2.6 h.
Preferably, the volume of the first defoaming solution is 6.0-10.0% of the volume of the first-stage feeding solution (perilla cake leaching liquor), and the concentration of perilla protein is 3.0-6.5 g/L.
Preferably, the volume of the second defoaming solution is 12.0-22.0% of the volume of the perilla cake leaching liquor, and the concentration of the perilla protein is 260-660 mg/L, which is close to the concentration of the perilla protein in the perilla cake leaching liquor.
Preferably, the concentration of the perilla protein in the residual liquid after the first-stage froth flotation is 90-280 mg/L.
Preferably, the concentration of the perilla protein in the residual liquid after the second-stage froth flotation is 70-170 mg/L.
Preferably, the concentration of the perilla protein in the perilla cake leaching liquor is 250-650 mg/L.
In another embodiment of the invention, a two-stage froth flotation process for concentrating and separating proteins from perilla seed meal comprises the following steps:
first, preparation of perilla cake leaching liquor
Removing impurities from dried perilla seeds, squeezing at low temperature to remove oil, mashing, crushing by a high-speed crusher, and sieving by a 80-mesh sieve to obtain perilla cake meal powder. Weighing a certain amount of perilla cake meal (5-10 g), adding distilled water according to a feed-liquid ratio of 1: 0.6-1: 1(g/L), adding 0.05-0.08% of sodium hydroxide solution to adjust the pH value of the mixed solution to 8.5-9.5, stirring for 0.6-1 h at 30-40 ℃ and 300-500 r/min (rotating speed), cooling to room temperature, centrifuging for 5min at 5000r/min, taking supernatant, placing in an adjusting tank, and adjusting the pH value to 6.5-7.5 (adding 0.04-0.06% of hydrochloric acid solution), thus obtaining the perilla cake leaching liquor.
Second, first stage froth flotation process
Injecting the perilla cake leaching liquor in the regulating reservoir as a first-stage feeding liquid into a first-stage foam flotation tower, performing first-stage foam flotation at room temperature, wherein the apparent gas velocity is 0.3-0.7 mm/s, preferably 0.4-0.6mm/s, the height of a foam layer is 3/5-4/5 of the height of the first-stage foam flotation tower, collecting and defoaming the foam flowing out of the top of the tower, and stopping ventilation when the foam cannot flow out of the top of the flotation tower. Defoaming the foam collected from the tower top to obtain a first-stage defoaming liquid, wherein the volume of the first-stage defoaming liquid is 6.0-10.0% of the volume of the first-stage feeding liquid, and the concentration of the perilla protein is 3.0-6.5 g/L; the defoaming solution is a perilla protein concentrated solution obtained by separation and is directly used as a raw material for producing perilla protein powder. The concentration of the perilla protein in the residual liquid (residual liquid) discharged from the bottom of the flotation tower is 90-280 mg/L, and the liquid enters a discharged liquid storage pool to be used as a feeding liquid for secondary foam flotation. Preferably, the operation time of the first-stage froth flotation is 0.8-2 h, and further preferably 1.3-2 h.
Third, second stage froth flotation process
And injecting the first-stage residual liquid in the discharged liquid storage pool into a second-stage foam flotation tower, performing second-stage foam flotation at room temperature, collecting and defoaming the foam flowing out of the tower top, and stopping ventilation when the foam cannot flow out of the top end of the flotation tower, wherein the apparent air speed is 0.7-1.1 mm/s, preferably 0.7-1.0 mm/s, and the height of a foam layer is 2/5-3/5 the height of the second-stage foam flotation tower. Defoaming the foam collected from the tower top to obtain a second-stage defoaming liquid, wherein the volume of the second-stage defoaming liquid is 12.0-22.0% of the volume of the second-stage feeding liquid, and the concentration of the perilla protein is 260-660 mg/L; the concentration of the liquid perilla protein is close to that of the perilla cake leaching liquor, and the liquid perilla protein can return to the regulating tank and be used as the first-stage feeding liquid of the next production cycle together with the newly injected perilla cake leaching liquor. The concentration of perilla protein in residual liquid (raffinate) discharged from the bottom of the flotation tower is 70-170 mg/L, and the perilla protein can be used as a raw material for extracting perilla flavone, rosmarinic acid, polysaccharide and other active ingredients. Preferably, the operation time of the second-stage froth flotation is 2.0-3.0 h, and further preferably 2.1-2.6 h.
Through two-stage froth flotation, the recovery rate of the perilla protein is 78.0-88.0%, and the enrichment ratio is 7.0-12.0. Wherein, the calculation formulas of the recovery rate and the enrichment ratio are as follows:
the purple perilla is planted in a Shanlan village test field in a sharp lawn area of Taiyuan city of Shanxi province, and is dried for 72 hours in a 50 ℃ ventilation drying oven for later use after seeds are collected.
The concentration of the perilla protein in the perilla cake leaching liquor is 250-650 mg/L.
In a second aspect of the invention, there is provided a perillain concentrate obtained by the two-stage froth flotation method.
The third aspect of the invention provides an application of the perilla protein concentrated solution obtained by the two-stage froth flotation method in preparing perilla protein powder.
In a third aspect of the invention, there is provided a use of the raffinate from the second stage of froth flotation in the two-stage froth flotation process described above as a raw material for the extraction of perilla frutescens flavone, rosmarinic acid, polysaccharides and other active ingredients.
The invention provides a froth flotation tower for concentrating and separating protein in perilla seed meal, which is hollow cylindrical and has the height-diameter ratio of 25-35: 1, an hourglass-shaped member is installed in the froth flotation tower and is formed by butting the top edges of two identical hollow bottomless circular truncated cones, the bottom edge is in seamless connection with the inner wall of the froth flotation tower, the diameter of the top surface of the circular truncated cone is smaller than that of the bottom surface, the diameter of the bottom surface is equal to that of the froth flotation tower, the vertical height of the hourglass-shaped member is 1/4 of the height of a froth phase, and the junction of the two circular truncated cones is positioned in the middle of the froth phase.
Preferably, the diameter of the top surface of the circular truncated cone is 1/2 of the diameter of the bottom surface.
In one embodiment of the invention, the diameter of the froth flotation tower for concentrating and separating the protein in the perilla seed meal is 40-60 mm, and the height of the froth flotation tower is 1.2-1.6 m.
Preferably, the hourglass-shaped member is made of a plastic sheet with the thickness of 1 mm.
The term "operating time" as used herein means the time from the start of aeration to the froth flotation cell to the termination of aeration, i.e. the time at which aeration is stopped when froth cannot flow from the top of the cell.
The invention has the beneficial effects that:
1. the invention develops a novel two-stage froth flotation technology and applies the novel two-stage froth flotation technology to the concentration and separation of protein in perilla cake meal. According to the surface adsorption principle, the flotation technology does not need to additionally add a flotation auxiliary agent in the process of separating the natural surfactant of the perilla protein, and has the advantages of low investment, low energy consumption, no pollution, simple steps and the like, thereby greatly reducing the difficulty and the cost of concentration and separation of the perilla protein.
2. The addition of the hourglass-shaped component in the first-stage foam flotation can enable rising foam to undergo shrinkage and expansion, reduce liquid holdup, enhance liquid drainage, realize high enrichment of perillaprotein (the concentration of the perillaprotein in the first-stage defoaming liquid is 3.0-6.5 g/L), and the obtained perillaprotein concentrated solution can be directly used as a production raw material of perillaprotein powder.
3. The perilla protein which is not concentrated in the first-stage residual liquid is recovered by the second-stage foam flotation, and the perilla protein is returned to the regulating tank for secondary separation, so that the recovery rate of the perilla protein is improved as much as possible; the second-stage residual liquid can be used as raw materials for extracting perilla flavone, rosmarinic acid, polysaccharide and other active ingredients for preparation treatment, so that the economic benefit is further improved.
4. Through the two-stage foam flotation process, on the basis of ensuring the high-efficiency recovery of the perilla protein (78-88%), the hourglass-shaped component is adopted to effectively improve the enrichment ratio of the perilla protein (7.0-12.0), so that the subsequent purification of the perilla protein is facilitated, and the production process of the perilla protein can be obviously promoted.
Drawings
Embodiments of the invention are described in detail below with reference to the attached drawing figures, wherein:
FIG. 1: a process flow chart for concentrating and separating protein in perilla cake by a two-stage froth flotation method.
FIG. 2: the first stage froth flotation tower structure is schematic. Wherein: 1 is a froth flotation column, 2 is an hourglass-shaped member, and 3 is the interface of a liquid phase and a froth phase. The part above 3 is foam phase, and is added into the hourglass-shaped member, and the part below 3 is liquid phase.
FIG. 3: schematic view of an hourglass-shaped member. Wherein: the foam flotation tower column is 1, the hourglass-shaped component is 2, and the junction of the hollow round platform components of the upper part and the lower part is the middle position of a foam phase.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1: first stage froth flotation tower
A froth flotation tower (as shown in figures 2 and 3) for concentrating and separating protein in perilla frutescens cake comprises a hollow cylindrical froth flotation tower column 1, the diameter of the hollow cylindrical froth flotation tower column 1 is 50mm, the height of the hollow cylindrical froth flotation tower column is 1.3m, an hourglass-shaped member 2 is installed in the froth flotation tower column 1, the hourglass-shaped member 2 is formed by butt joint of two identical hollow bottomless circular truncated cones, the top surface edge of the hollow cylindrical hollow circular truncated cones is in seamless connection with the inner wall of a froth flotation tower column 11, the top surface diameter of the circular truncated cones is 1/2 of the bottom surface diameter, the bottom surface diameter is 50mm, the vertical height of the hourglass-shaped member 2 is 225mm, and the junction of the two circular truncated cones is located in the middle of a foam phase.
The hourglass-shaped component is made of a plastic sheet with the thickness of 1mm, the sheet is made into a hollow circular table through a conventional thermoplastic process, and then the two parts are spliced to form the component shown in the figures 2 and 3.
Example 2: first stage froth flotation tower
A froth flotation tower (as shown in figures 2 and 3) for concentrating and separating protein in perilla frutescens cake comprises a hollow cylindrical froth flotation tower column 1, the diameter of the hollow cylindrical froth flotation tower column 1 is 50mm, the height of the hollow cylindrical froth flotation tower column is 1.3m, an hourglass-shaped member 2 is installed in the froth flotation tower column 1, the hourglass-shaped member 2 is formed by butt joint of two identical hollow bottomless circular truncated cones, the top surface edge of the hollow cylindrical hollow circular truncated cones is in seamless connection with the inner wall of a froth flotation tower column 11, the top surface diameter of the circular truncated cones is 1/2 of the bottom surface diameter, the bottom surface diameter is 50mm, the vertical height of the hourglass-shaped member 2 is 200mm, and the junction of the two circular truncated cones is located in the middle of a foam phase.
The hourglass-shaped component is made of a plastic sheet with the thickness of 1mm, the sheet is made into a hollow circular table through a conventional thermoplastic process, and then the two parts are spliced to form the component shown in the figures 2 and 3.
Example 3: first stage froth flotation tower
A froth flotation tower (as shown in figures 2 and 3) for concentrating and separating protein in perilla frutescens cake comprises a hollow cylindrical froth flotation tower column 1, the diameter of the hollow cylindrical froth flotation tower column 1 is 50mm, the height of the hollow cylindrical froth flotation tower column is 1.3m, an hourglass-shaped member 2 is installed in the froth flotation tower column 1, the hourglass-shaped member 2 is formed by butt joint of two identical hollow bottomless circular truncated cones, the top surface edge of the hollow cylindrical hollow circular truncated cones is in seamless connection with the inner wall of a froth flotation tower column 11, the top surface diameter of the circular truncated cones is 1/2 of the bottom surface diameter, the bottom surface diameter is 50mm, the vertical height of the hourglass-shaped member 2 is 250mm, and the junction of the two circular truncated cones is located in the middle of a foam phase.
The hourglass-shaped component is made of a plastic sheet with the thickness of 1mm, the sheet is made into a hollow circular table through a conventional thermoplastic process, and then the two parts are spliced to form the component shown in the figures 2 and 3.
Example 4: first stage froth flotation tower
A froth flotation tower (as shown in figures 2 and 3) for concentrating and separating protein in perilla frutescens cake comprises a hollow cylindrical froth flotation tower column 1, the diameter of the hollow cylindrical froth flotation tower column 1 is 50mm, the height of the hollow cylindrical froth flotation tower column is 1.5m, an hourglass-shaped member 2 is installed in the froth flotation tower column 1, the hourglass-shaped member 2 is formed by butt joint of two identical hollow bottomless circular truncated cones, the top surface edge of the hollow cylindrical hollow circular truncated cones is in seamless connection with the inner wall of a froth flotation tower column 11, the top surface diameter of the circular truncated cones is 1/2 of the bottom surface diameter, the bottom surface diameter is 50mm, the vertical height of the hourglass-shaped member 2 is 275mm, and the junction of the two circular truncated cones is located in the middle of a foam phase.
The hourglass-shaped component is made of a plastic sheet with the thickness of 1mm, the sheet is made into a hollow circular table through a conventional thermoplastic process, and then the two parts are spliced to form the component shown in the figures 2 and 3.
Example 5: first stage froth flotation tower
A froth flotation tower (as shown in figures 2 and 3) for concentrating and separating protein in perilla frutescens cake comprises a hollow cylindrical froth flotation tower column 1, the diameter of the hollow cylindrical froth flotation tower column 1 is 60mm, the height of the hollow cylindrical froth flotation tower column is 1.5m, an hourglass-shaped member 2 is installed in the froth flotation tower column 1, the hourglass-shaped member 2 is formed by butt joint of two identical hollow bottomless circular truncated cones, the top surface edge of the hollow cylindrical hollow circular truncated cones is in seamless connection with the inner wall of a froth flotation tower column 11, the top surface diameter of the circular truncated cones is 1/2 of the bottom surface diameter, the bottom surface diameter is 60mm, the vertical height of the hourglass-shaped member 2 is 300mm, and the junction of the two circular truncated cones is located in the middle of a foam phase.
The hourglass-shaped component is made of a plastic sheet with the thickness of 1mm, the sheet is made into a hollow circular table through a conventional thermoplastic process, and then the two parts are spliced to form the component shown in the figures 2 and 3.
The technological process of concentrating and separating perilla protein by a two-stage froth flotation method is shown in figure 1: the first step is as follows: the perilla seeds are degreased, crushed and leached by weak base to obtain perilla cake leaching liquor, and the leaching liquor is injected into an adjusting tank to adjust the pH value of the perilla cake leaching liquor to be used as a feeding liquid for first-stage foam flotation. The second step is that: an hourglass-shaped component is arranged in the first-stage foam flotation tower, so that foam drainage is enhanced, the volume of defoaming liquid is reduced, and perilla protein is effectively enriched; the first-stage defoaming solution is a perilla protein concentrated solution and can be directly used as a raw material for producing perilla protein powder. The third step: the second-stage froth flotation takes the residual liquid of the first stage as a feed liquid, so that the recovery effect of the perilla protein is further improved; returning the second-stage defoaming solution to the regulating tank, and concentrating and separating the perilla protein again; the second stage raffinate can be used as raw material for extracting perilla flavone, rosmarinic acid, polysaccharide and other active ingredients. Therefore, the two-stage froth flotation method solves the concentration problem of separating the protein in the perilla seed meal at present, and simultaneously realizes the high-efficiency enrichment and recovery of the perilla protein.
Example 6: preparation of concentrated perilla protein solution
First, preparation of perilla cake leaching liquor
Removing impurities from dried perilla seeds, squeezing at low temperature to remove oil, mashing, crushing by a high-speed crusher, and sieving by a 80-mesh sieve to obtain perilla cake meal powder. Weighing 5g of perilla cake meal powder, adding distilled water according to a feed-liquid ratio of 1:0.8(g/L), adjusting the pH value of the mixed solution to 9.0, stirring at 30 ℃ and 300r/min (rotating speed) for 0.6h, cooling to room temperature, centrifuging at 5000r/min for 5min, taking supernatant, placing in an adjusting tank, and adjusting the pH value to 7.3 to obtain perilla cake meal leaching liquor, wherein the concentration of perilla protein is 391.9 mg/L.
The concentration of perilla protein was measured according to the measurement method given in "process for extracting perilla cake protein by response surface-optimized foam method" published in 44 volumes, page 574 to page 579 of proceedings of university of agriculture 4, Anhui, 2017 by researchers such as Wu banker (the same examples below).
Second, first stage froth flotation
The perilla cake leaching solution in the equalizing basin was injected into the first stage froth flotation tower (first stage froth flotation tower in example 1). And performing first-stage foam flotation at room temperature, wherein the apparent gas velocity is 0.6mm/s, the height of a foam layer is 0.9m, collecting and defoaming foam flowing out of the top of the flotation tower, stopping ventilation when the foam cannot flow out of the top of the flotation tower, and operating for 1.5 h. The liquid obtained by defoaming the foam collected from the tower top is a first-stage defoaming solution, namely a perilla protein concentrated solution, the volume of the perilla protein concentrated solution is 6.1% of the volume of a perilla cake leaching liquor, the concentration of the perilla protein is 4.1g/L, and the perilla protein concentrated solution is directly used as a raw material for producing perilla protein powder; the concentration of the perillain in the raffinate discharged from the bottom of the flotation tower is 156.7mg/L, and the liquid enters a discharged liquid storage pool to be used as a feed liquid for secondary froth flotation.
Third, second stage froth flotation
And injecting the first-stage residual liquid in the discharge liquid storage pool into a second-stage foam flotation tower, wherein the diameter of the second-stage foam flotation tower is 60mm, the height of the second-stage foam flotation tower is 0.9m, and no hourglass-shaped member is added in the second-stage foam flotation tower. And performing secondary froth flotation at room temperature, wherein the apparent gas velocity is 0.8mm/s, the height of a froth layer is 0.4m, collecting and defoaming the froth flowing out of the top of the flotation tower, stopping aeration when the froth cannot flow out of the top of the flotation tower, and operating for 2.2 h. The liquid obtained after defoaming the foam collected from the tower top is a second stage defoaming liquid, the volume of the second stage defoaming liquid is 21.3% of the volume of the second stage feeding liquid, and the concentration of the perilla protein is 388.5 mg/L; the liquid is close to the concentration of the leaching liquor of the perilla cake pulp and can be returned to the regulating tank to be used as the first-stage feeding liquid of the next production period. The concentration of perilla protein in the residual liquid discharged from the bottom of the flotation tower is 91.2mg/L, and the residual liquid can be used as a raw material for extracting perilla flavone, rosmarinic acid, polysaccharide and other active ingredients.
Through a two-stage foam flotation process, the recovery rate of the perilla protein is 82.6%, and the enrichment ratio is 10.5; when the first-stage foam flotation adopts a foam flotation tower without an hourglass-shaped component and other conditions are consistent to perform experiments, the enrichment ratio of the perilla protein is only 5.1.
Example 7: preparation of concentrated perilla protein solution
First, preparation of perilla cake leaching liquor
Removing impurities from dried perilla seeds, squeezing at low temperature to remove oil, mashing, crushing by a high-speed crusher, and sieving by a 80-mesh sieve to obtain perilla cake meal powder. Weighing 6g of perilla cake meal powder, adding distilled water according to a feed-liquid ratio of 1:0.6(g/L), adjusting the pH value of the mixed solution to 9.5, stirring at 30 ℃ and 400r/min (rotating speed) for 0.8h, cooling to room temperature, centrifuging at 5000r/min for 5min, taking supernatant, placing in an adjusting tank, and adjusting the pH value to 7.0 to obtain perilla cake meal leaching liquor, wherein the concentration of perilla protein is 616.8 mg/L.
Second, first stage froth flotation
The perilla cake leaching solution in the equalizing basin was injected into the first stage froth flotation tower (first stage froth flotation tower in example 2). And performing first-stage foam flotation at room temperature, wherein the apparent gas velocity is 0.4mm/s, the height of a foam layer is 0.8m, collecting and defoaming foam flowing out of the top of the flotation tower, stopping ventilation when the foam cannot flow out of the top of the flotation tower, and operating for 2.0 h. The liquid obtained by defoaming the foam collected from the tower top is a first-stage defoaming solution, namely a perilla protein concentrated solution, the volume of the perilla protein concentrated solution is 9.2% of the volume of a perilla cake leaching liquor, the concentration of the perilla protein is 4.8g/L, and the perilla protein concentrated solution is directly used as a raw material for producing perilla protein powder; the concentration of the perilla protein in the residual liquid discharged from the bottom of the flotation tower is 222.3mg/L, and the liquid enters a discharged liquid storage pool to be used as a feed liquid for secondary foam flotation.
Third, second stage froth flotation
And injecting the first-stage residual liquid in the discharge liquid storage pool into a second-stage foam flotation tower, wherein the diameter of the flotation tower is 60mm, the height of the flotation tower is 1.0m, and no hourglass-shaped component is added in the flotation tower. And performing secondary froth flotation at room temperature, wherein the apparent gas velocity is 0.7mm/s, the height of a froth layer is 0.5m, collecting and defoaming the froth flowing out of the top of the flotation tower, stopping aeration when the froth cannot flow out of the top of the flotation tower, and operating for 2.6 h. The liquid obtained after defoaming the foam collected from the tower top is a second stage defoaming liquid, the volume of the second stage defoaming liquid is 14.7% of the volume of the second stage feeding liquid, and the concentration of the perilla protein is 620.1 mg/L; the liquid is close to the concentration of the leaching liquor of the perilla cake pulp and can be returned to the regulating tank to be used as the first-stage feeding liquid of the next production period. The concentration of perilla protein in the residual liquid discharged from the bottom of the flotation tower is 136.8mg/L, and the residual liquid can be used as a raw material for extracting perilla flavone, rosmarinic acid, polysaccharide and other active ingredients.
Through the two-stage froth flotation process, the recovery rate of the perilla protein is 84.1 percent, and the enrichment ratio is 7.8; when the first-stage foam flotation adopts a foam flotation tower without an hourglass-shaped component and other conditions are consistent to perform experiments, the enrichment ratio of the perilla protein is only 3.8.
Example 8: preparation of concentrated perilla protein solution
First, preparation of perilla cake leaching liquor
Removing impurities from dried perilla seeds, squeezing at low temperature to remove oil, mashing, crushing by a high-speed crusher, and sieving by a 80-mesh sieve to obtain perilla cake meal powder. Weighing 8g of perilla cake meal powder, adding distilled water according to a feed-liquid ratio of 1:0.6(g/L), adjusting the pH value of the mixed solution to 9.5, stirring at 35 ℃ and 400r/min (rotating speed) for 1.0h, cooling to room temperature, centrifuging at 5000r/min for 5min, taking supernatant, placing in an adjusting tank, and adjusting the pH value to 7.2 to obtain perilla cake meal leaching liquor, wherein the concentration of perilla protein is 636.8 mg/L.
Second, first stage froth flotation
The perilla cake leaching solution in the equalizing basin was injected into the first stage froth flotation tower (first stage froth flotation tower in example 3). And performing first-stage foam flotation at room temperature, wherein the apparent gas velocity is 0.5mm/s, the height of a foam layer is 1.0m, collecting and defoaming foam flowing out of the top of the flotation tower, stopping ventilation when the foam cannot flow out of the top of the flotation tower, and operating for 1.8 h. The liquid obtained by defoaming the foam collected from the tower top is a first-stage defoaming solution, namely a perilla protein concentrated solution, the volume of the perilla protein concentrated solution is 6.8% of the volume of a perilla cake leaching liquor, the concentration of the perilla protein is 5.6g/L, and the perilla protein concentrated solution is directly used as a raw material for producing perilla protein powder; the concentration of the perillain in the raffinate discharged from the bottom of the flotation tower is 265.6mg/L, and the liquid enters a discharged liquid storage pool to be used as a feed liquid for secondary foam flotation.
Third, second stage froth flotation
And injecting the first-stage residual liquid in the discharge liquid storage pool into a second-stage foam flotation tower, wherein the diameter of the flotation tower is 60mm, the height of the flotation tower is 1.0m, and no hourglass-shaped component is added in the flotation tower. And performing secondary froth flotation at room temperature, wherein the apparent gas velocity is 0.8mm/s, the height of a froth layer is 0.5m, collecting and defoaming the froth flowing out of the top of the flotation tower, stopping aeration when the froth cannot flow out of the top of the flotation tower, and operating for 2.4 h. The liquid obtained after defoaming the foam collected from the tower top is a second stage defoaming liquid, the volume of the second stage defoaming liquid is 21.6% of the volume of the second stage feeding liquid, and the concentration of the perilla protein is 608.9 mg/L; the liquid is close to the concentration of the leaching liquor of the perilla cake pulp and can be returned to the regulating tank to be used as the first-stage feeding liquid of the next production period. The concentration of perilla protein in the residual liquid discharged from the bottom of the flotation tower is 162.4mg/L, and the residual liquid can be used as a raw material for extracting perilla flavone, rosmarinic acid, polysaccharide and other active ingredients.
Through a two-stage foam flotation process, the recovery rate of the perilla protein is 81.1 percent, and the enrichment ratio is 8.9; when the first-stage foam flotation adopts a foam flotation tower without an hourglass-shaped component and other conditions are consistent to perform experiments, the enrichment ratio of the perilla protein is only 4.2.
Example 9: preparation of concentrated perilla protein solution
First, preparation of perilla cake leaching liquor
Removing impurities from dried perilla seeds, squeezing at low temperature to remove oil, mashing, crushing by a high-speed crusher, and sieving by a 80-mesh sieve to obtain perilla cake meal powder. Weighing 7g of perilla cake meal powder, adding distilled water according to a feed-liquid ratio of 1:1(g/L), adjusting the pH value of the mixed solution to 8.5, stirring at 40 ℃ and 400r/min (rotating speed) for 0.8h, cooling to room temperature, centrifuging at 5000r/min for 5min, taking supernatant, placing in an adjusting tank, and adjusting the pH value to 6.8 to obtain perilla cake meal leaching liquor, wherein the concentration of perilla protein is 288.6 mg/L.
Second, first stage froth flotation
The perilla cake leaching solution in the equalizing basin was injected into the first stage froth flotation tower (first stage froth flotation tower in example 4). And performing first-stage foam flotation at room temperature, wherein the apparent gas velocity is 0.6mm/s, the height of a foam layer is 1.1m, collecting and defoaming foam flowing out of the top of the flotation tower, stopping ventilation when the foam cannot flow out of the top of the flotation tower, and operating for 1.3 h. The liquid obtained by defoaming the foam collected from the tower top is a first-stage defoaming solution, namely a perilla protein concentrated solution, the volume of the perilla protein concentrated solution is 6.2% of the volume of a perilla cake leaching liquor, the concentration of the perilla protein is 3.2g/L, and the perilla protein concentrated solution is directly used as a raw material for producing perilla protein powder; the concentration of the perilla protein in the residual liquid discharged from the bottom of the flotation tower is 98.7mg/L, and the liquid enters a discharged liquid storage pool to be used as a feeding liquid for secondary foam flotation.
Third, second stage froth flotation
And (3) allowing the first-stage residual liquid in the discharged liquid storage pool to enter a second-stage foam flotation tower, wherein the diameter of the flotation tower is 60mm, the height of the flotation tower is 1.1m, and no hourglass-shaped member is added in the tower. And performing secondary froth flotation at room temperature, wherein the apparent gas velocity is 0.9mm/s, the height of a froth layer is 0.6m, collecting and defoaming the froth flowing out of the top of the flotation tower, stopping aeration when the froth cannot flow out of the top of the flotation tower, and the operation time is 2.1 h. The liquid obtained after defoaming the foam collected from the tower top is a second stage defoaming liquid, the volume of the second stage defoaming liquid is 13.8 percent of the volume of the second stage feeding liquid, and the concentration of the perilla protein is 276.8 mg/L; the liquid is close to the concentration of the leaching liquor of the perilla cake pulp and can be returned to the regulating tank to be used as the first-stage feeding liquid of the next production period. The concentration of perilla protein in the residual liquid discharged from the bottom of the flotation tower is 70.4mg/L, and the residual liquid can be used as a raw material for extracting perilla flavone, rosmarinic acid, polysaccharide and other active ingredients.
Through the two-stage froth flotation process, the recovery rate of the perilla protein is 80.4 percent, and the enrichment ratio is 11.1; when the first-stage foam flotation adopts a foam flotation tower without an hourglass-shaped component and other conditions are consistent to perform experiments, the enrichment ratio of the perilla protein is only 5.8.
Example 10: preparation of concentrated perilla protein solution
First, preparation of perilla cake leaching liquor
Removing impurities from dried perilla seeds, squeezing at low temperature to remove oil, mashing, crushing by a high-speed crusher, and sieving by a 80-mesh sieve to obtain perilla cake meal powder. Weighing 10g of perilla cake meal powder, adding distilled water according to a feed-liquid ratio of 1:0.8(g/L), adjusting the pH value of the mixed solution to 9.0, stirring at 40 ℃ and 500r/min (rotating speed) for 0.6h, cooling to room temperature, centrifuging at 5000r/min for 5min, taking supernatant, placing in an adjusting tank, and adjusting the pH value to 6.5 to obtain perilla cake meal leaching liquor, wherein the concentration of perilla protein is 428.5 mg/L.
Second, first stage froth flotation
The perilla cake leaching solution in the equalizing basin was injected into the first stage froth flotation tower (first stage froth flotation tower in example 5). And performing first-stage foam flotation at room temperature, wherein the apparent gas velocity is 0.5mm/s, the height of a foam layer is 1.2m, collecting and defoaming foam flowing out of the top of the flotation tower, stopping ventilation when the foam cannot flow out of the top of the flotation tower, and operating for 1.7 h. The liquid obtained by defoaming the foam collected from the tower top is a first-stage defoaming solution, namely a perilla protein concentrated solution, the volume of the perilla protein concentrated solution is 7.5% of the volume of a perilla cake leaching liquor, the concentration of the perilla protein is 4.0g/L, and the perilla protein concentrated solution is directly used as a raw material for producing perilla protein powder; the concentration of the perilla protein in the residual liquid discharged from the bottom of the flotation tower is 138.7mg/L, and the liquid enters a discharged liquid storage pool to be used as a feeding liquid for secondary foam flotation.
Third, second stage froth flotation
And injecting the first-stage residual liquid in the discharge liquid storage pool into a second-stage foam flotation tower, wherein the diameter of the flotation tower is 60mm, the height of the flotation tower is 1.1m, and no hourglass-shaped component is added in the tower. And performing secondary froth flotation at room temperature, wherein the apparent gas velocity is 1.0mm/s, the height of a froth layer is 0.7m, collecting and defoaming the froth flowing out of the top of the flotation tower, stopping aeration when the froth cannot flow out of the top of the flotation tower, and operating for 2.2 h. The liquid obtained after defoaming the foam collected from the tower top is a second stage defoaming liquid, the volume of the second stage defoaming liquid is 15.1% of the volume of the second stage feeding liquid, and the concentration of the perilla protein is 419.2 mg/L; the liquid is close to the concentration of the leaching liquor of the perilla cake pulp and can be returned to the regulating tank to be used as the first-stage feeding liquid of the next production period. The concentration of perilla protein in the residual liquid discharged from the bottom of the flotation tower is 88.3mg/L, and the residual liquid can be used as a raw material for extracting perilla flavone, rosmarinic acid, polysaccharide and other active ingredients.
Through the two-stage froth flotation process, the recovery rate of the perilla protein is 83.7 percent, and the enrichment ratio is 9.2; when the first-stage foam flotation adopts a foam flotation tower without an hourglass-shaped component and other conditions are consistent to perform experiments, the enrichment ratio of the perilla protein is only 4.5.
According to the embodiment, the liquid discharge is strengthened by the foam flotation tower with the hourglass-shaped member according to the expansion and contraction principle in the foam rising process, the protein denaturation is avoided at normal temperature, and the industrial production is facilitated. In conclusion, the two-stage foam flotation method effectively strengthens foam liquid discharge and reduces the volume of defoaming solution on the basis of ensuring the high recovery rate of the perillain, so that the perillain is highly concentrated, and meanwhile, the method has the advantages of greenization of the process, low energy consumption, less investment, simple steps and the like.
The invention is not the best known technology.
Claims (9)
1. A two-stage froth flotation method for concentrating and separating protein in perilla seed cakes is characterized by comprising the following steps:
preparing a perilla cake leaching liquor;
performing primary foam flotation by taking the perilla cake leaching liquor as a primary feeding liquid, collecting foam and defoaming to obtain a primary defoaming liquid, namely a perilla protein concentrated solution, performing secondary foam flotation by taking residual liquid of the primary foam flotation as a secondary feeding liquid, collecting foam and defoaming to obtain a secondary defoaming liquid;
the apparent air speed of the first-stage froth flotation is 0.3-0.7 mm/s, and the aeration is stopped when the froth cannot flow out; the first-stage foam flotation is carried out in a hollow cylindrical first-stage foam flotation tower, an hourglass-shaped member is installed in the first-stage foam flotation tower, the hourglass-shaped member is formed by butt joint of top edges of two identical hollow bottomless circular truncated cones, the bottom edges of the circular truncated cones are in seamless connection with the inner wall of the first-stage foam flotation tower, the diameter of the top surfaces of the circular truncated cones is 1/2 of the diameter of the bottom surfaces, the diameter of the bottom surfaces of the circular truncated cones is equal to the diameter of the first-stage foam flotation tower, the vertical height of the hourglass-shaped member is 1/4 of the height of a foam phase, and the junction of the two circular truncated cones is located in the middle of the foam phase;
and the apparent air speed of the second-stage froth flotation is 0.7-1.1 mm/s, the aeration is stopped when the froth cannot flow out, and the second-stage froth flotation is carried out in a hollow cylindrical second-stage froth flotation tower.
2. A two stage froth flotation process according to claim 1, wherein the second stage defoaming solution is used as the first stage feed solution, either alone or in combination with a perilla meal leach solution.
3. The two-stage froth flotation process according to claim 1, wherein the preparing of the perilla cake leaching liquor comprises adding water to perilla cake according to a feed-liquid ratio of 1: 0.6-1: 1(g/L), adjusting the pH value to 8.5-9.5, stirring, centrifuging, taking supernatant, adjusting the pH value to 6.5-7.5, stirring for 0.6-1 h at a temperature of 30-40 ℃ and a rotation speed of 300-500 r/min, and centrifuging for 5min at a rotation speed of 5000 r/min.
4. A two-stage froth flotation process according to claim 1, wherein the first stage froth flotation column has a height to diameter ratio of 25 to 35: 1; the height-diameter ratio of the second-stage froth flotation tower is 10-20: 1.
5. A two-stage froth flotation process according to claim 1, wherein the froth layer height of the first stage froth flotation is 3/5 to 4/5 the height of the first stage froth flotation column and the froth layer height of the second stage froth flotation is 2/5 to 3/5 the height of the second stage froth flotation column.
6. The two-stage froth flotation process according to claim 1, wherein the perilla cake meal is perilla cake meal, and the perilla cake meal is obtained by deoiling dried perilla seeds and then crushing the dried perilla seeds.
7. A two stage froth flotation process according to claim 1, wherein said defoaming is mechanical defoaming.
8. A two-stage froth flotation process according to any one of claims 1 to 7, comprising the steps of:
removing impurities from dried perilla seeds, squeezing at low temperature, deoiling, crushing, sieving with a 80-mesh sieve to obtain perilla cake meal powder, adding water into the perilla cake meal powder according to a material-liquid ratio of 1: 0.6-1: 1(g/L), adjusting the pH value to 8.5-9.5 by using a sodium hydroxide solution, stirring for 0.6-1 h at 30-40 ℃ and 300-500 r/min, cooling to room temperature, centrifuging for 5min at 5000r/min, taking supernatant, adjusting the pH value to 6.5-7.5 by using a hydrochloric acid solution to obtain a perilla cake meal leaching liquor;
injecting the perilla cake leaching liquor serving as a first-stage feeding liquid into a first-stage foam flotation tower, performing first-stage foam flotation at room temperature, wherein the apparent gas velocity is 0.3-0.7 mm/s, the height of a foam layer is 3/5-4/5 of the height of the first-stage foam flotation tower, collecting and defoaming foam flowing out of the top of the tower, stopping ventilation when the foam cannot flow out of the top of the flotation tower, and defoaming the foam collected from the top of the tower to obtain a first-stage defoaming liquid;
injecting the residual liquid discharged from the bottom of the first-stage foam flotation tower into a second-stage foam flotation tower, performing second-stage foam flotation at room temperature, wherein the apparent air speed is 0.7-1.1 mm/s, the height of a foam layer is 2/5-3/5 higher than that of the second-stage foam flotation tower, collecting and defoaming the foam flowing out of the top of the tower, stopping ventilation when the foam cannot flow out of the top of the second-stage foam flotation tower, defoaming the foam collected from the top of the tower to obtain a second-stage defoaming liquid, and combining the second-stage defoaming liquid and the perilla cake leaching liquor to obtain a first-stage feeding liquid.
9. The froth flotation tower for concentrating and separating protein in perilla seed cakes is characterized in that the froth flotation tower is hollow and cylindrical, the height-diameter ratio of the froth flotation tower is 25-35: 1, an hourglass-shaped component is installed in the froth flotation tower and is formed by butt joint of top edges of two identical hollow bottomless circular truncated cones, the bottom edge is in seamless connection with the inner wall of the froth flotation tower, the diameter of the top surface of each circular truncated cone is 1/2 of the diameter of the bottom surface, the diameter of the bottom surface of each circular truncated cone is equal to the diameter of the froth flotation tower, the vertical height of the hourglass-shaped component is 1/4 of the height of a froth phase, and the junction of the two circular truncated cones is located in the middle of the froth phase.
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