CN114853821B - Method for separating saponin from canned asparagus processing wastewater - Google Patents
Method for separating saponin from canned asparagus processing wastewater Download PDFInfo
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- 229930182490 saponin Natural products 0.000 title claims abstract description 91
- 150000007949 saponins Chemical class 0.000 title claims abstract description 90
- 239000001397 quillaja saponaria molina bark Substances 0.000 title claims abstract description 63
- 239000002351 wastewater Substances 0.000 title claims abstract description 55
- 235000005340 Asparagus officinalis Nutrition 0.000 title claims abstract description 37
- 238000012545 processing Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 25
- 244000003416 Asparagus officinalis Species 0.000 title abstract 3
- 239000006260 foam Substances 0.000 claims abstract description 76
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 68
- 238000000926 separation method Methods 0.000 claims abstract description 48
- 230000000813 microbial effect Effects 0.000 claims abstract description 42
- 244000063299 Bacillus subtilis Species 0.000 claims abstract description 16
- 235000014469 Bacillus subtilis Nutrition 0.000 claims abstract description 16
- 241000589517 Pseudomonas aeruginosa Species 0.000 claims abstract description 16
- 240000006024 Lactobacillus plantarum Species 0.000 claims abstract description 15
- 235000013965 Lactobacillus plantarum Nutrition 0.000 claims abstract description 15
- 229940072205 lactobacillus plantarum Drugs 0.000 claims abstract description 15
- 150000001875 compounds Chemical class 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000007664 blowing Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 235000017709 saponins Nutrition 0.000 claims description 85
- 241000234427 Asparagus Species 0.000 claims description 34
- 239000007788 liquid Substances 0.000 claims description 28
- 239000002131 composite material Substances 0.000 claims description 13
- 239000002068 microbial inoculum Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000009423 ventilation Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000000605 extraction Methods 0.000 abstract description 18
- 230000001580 bacterial effect Effects 0.000 abstract description 17
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 1
- 238000011084 recovery Methods 0.000 description 34
- 238000002474 experimental method Methods 0.000 description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 238000011835 investigation Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 150000005856 steroid saponins Chemical class 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- KYWSCMDFVARMPN-LCSVLAELSA-N Saikosaponin D Chemical compound O([C@@H]1[C@@H](O)[C@H](O[C@@H]2[C@@]([C@H]3[C@]([C@@H]4[C@@]([C@@]5(C[C@@H](O)[C@]67CO[C@]5([C@@H]6CC(C)(C)CC7)C=C4)C)(C)CC3)(C)CC2)(C)CO)O[C@@H]([C@@H]1O)C)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O KYWSCMDFVARMPN-LCSVLAELSA-N 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000002054 inoculum Substances 0.000 description 3
- 229930192014 saikosaponin Natural products 0.000 description 3
- 239000000344 soap Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 241000186000 Bifidobacterium Species 0.000 description 2
- 241000202726 Bupleurum Species 0.000 description 2
- RGSFGYAAUTVSQA-UHFFFAOYSA-N Cyclopentane Chemical compound C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 2
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 2
- 235000014680 Saccharomyces cerevisiae Nutrition 0.000 description 2
- 238000005273 aeration Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000287 crude extract Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
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- 241000193388 Bacillus thuringiensis Species 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
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- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
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- 239000013543 active substance Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229940097012 bacillus thuringiensis Drugs 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000003433 contraceptive agent Substances 0.000 description 1
- 230000002254 contraceptive effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- WQLVFSAGQJTQCK-UHFFFAOYSA-N diosgenin Natural products CC1C(C2(CCC3C4(C)CCC(O)CC4=CCC3C2C2)C)C2OC11CCC(C)CO1 WQLVFSAGQJTQCK-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000469 ethanolic extract Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 125000003147 glycosyl group Chemical group 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002949 hemolytic effect Effects 0.000 description 1
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- NWMIYTWHUDFRPL-UHFFFAOYSA-N sapogenin Natural products COC(=O)C1(CO)C(O)CCC2(C)C1CCC3(C)C2CC=C4C5C(C)(O)C(C)CCC5(CCC34C)C(=O)O NWMIYTWHUDFRPL-UHFFFAOYSA-N 0.000 description 1
- -1 saponin compounds Chemical class 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000001612 separation test Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000003270 steroid hormone Substances 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G3/00—Glycosides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Water Treatments (AREA)
Abstract
The invention belongs to the technical field of saponin extraction, and particularly relates to a method for separating saponin from canned asparagus processing wastewater by utilizing a foam separation device. The specific method comprises the steps of uniformly stirring the wastewater and a compound microbial agent, wherein the compound microbial agent accounts for 0.02-0.3% of the canned asparagus processing wastewater, the compound microbial agent consists of pseudomonas aeruginosa bacterial agent, lactobacillus plantarum bacterial agent and bacillus subtilis bacterial agent, and the proportion of 3 is 2-5: 1: 3-5, after fully mixing, introducing the mixture into a foam separation device, blowing air by a gas distributor, generating bubbles, and collecting foam with saponin; the method has the advantages that the saponin components are successfully extracted at 15-40 ℃ for 5-10 min, the extraction efficiency is remarkably improved by at least 2-3 times compared with other modes, the collected saponin enrichment ratio is about 9-11, and the extraction is simpler by matching with a foam separation device, so that the method is more suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of saponin extraction, and particularly relates to a method for separating saponin from canned asparagus processing wastewater.
Background
The bioactive substances in asparagus are mainly steroid saponins. Steroid saponins are saponins with cyclopentane polyhydrophenanthrene mother nucleus structure, which exist widely in nature, besides being used as raw materials for synthesizing steroid hormone and contraceptive, the steroid saponins have wide pharmacological actions and important biological activities, such as preventing and treating cardiovascular diseases, resisting tumors, regulating immunity, resisting fungi, reducing blood sugar, killing insects and the like (Zhang Rejie. Extraction, purification and hemolytic activity research of asparagus saponins).
During the processing of asparagus, a large amount of processed wastewater is generated, and the wastewater contains high-concentration saponins. Especially, the content concentration of the saponin in the wastewater generated in the pre-boiling step in the canned asparagus processing technology can reach 500-5000 mg/L, and if the wastewater from asparagus processing is recycled, the added value of the asparagus processing industry can be improved by extracting the saponin compounds in the wastewater, thereby conforming to the development direction of the current industry.
Steroid saponins are soluble in water, are easily soluble in hot water and dilute alcohol, and are hardly soluble in lipophilic solvents such as petroleum ether, benzene, diethyl ether and the like.
The extraction method is usually selected from hot extraction, microwave-assisted extraction, ultrasonic-assisted extraction, and ultrahigh pressure-assisted extraction. At present, ethanol is most commonly used as solvent for extraction in a laboratory, ethanol is generally used for extraction, then the ethanol extract is suspended in water, and water saturated n-butanol is used for extraction, so that the total saponins are obtained.
However, the method is only suitable for extracting from asparagus or processed leftover stem and bark, the concentration of saponin in the asparagus processing wastewater is relatively lower than that of the asparagus or processed leftover stem and bark, and the method is time-consuming and labor-consuming, has higher cost and is not suitable for use any more.
CN 103142664B discloses a method for extracting total saponins of bupleurum by using a two-stage foam separation method, which comprises the following specific steps: drying and crushing bupleurum decoction pieces, extracting by a solvent cold leaching method, filtering to obtain a crude extract of saikosaponin, recovering a solvent in the crude extract, taking the obtained aqueous solution of saikosaponin as an initial feed liquid, separating the initial feed liquid in a first-stage foam separation tower, breaking foam layers, stopping ventilation when foam cannot flow out from the top of the foam separation tower, and breaking foam flowing out from the top of the first-stage foam separation tower to obtain a first-stage defoaming liquid; after the residual liquid in the tower is taken as the feed of the second-stage foam separation to enter the second-stage foam separation tower for separation, foam flowing out of the tower top is broken into second-stage defoaming liquid, and when the foam cannot flow out of the tower top of the foam separation tower, the ventilation is stopped, and the second-stage defoaming liquid and the crude saikosaponin extract are mixed and added into the feed of the first-stage foam separation tower; evaporating the foam breaking liquid in vacuum to obtain concentrated solution, regulating pH value to slight alkali, and freeze drying to obtain the product. The method has high yield which can reach 87-92%.
However, the above documents have the following disadvantages: (1) Each stage of foam separation has a period of 1-2 hours and has low efficiency; the enrichment ratio of (2) is 5-8, and the enrichment ratio is still to be improved.
Therefore, how to separate the saponin from the asparagus processing wastewater rapidly, efficiently and with low cost under the condition of considering the extraction cost is a problem to be solved.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for separating saponins in asparagus can processing wastewater, which uses the difference of the adsorption property of low-polarity component saponins at a gas-liquid two-phase interface, takes foam as a separating medium, adopts technical means such as efficient foaming, foam separation, component enrichment and the like to carry out optimized assembly, and adopts a research design to form a foam separating device in the asparagus processing wastewater, wherein the main structure comprises a gas distributor, an air pump, a foam separating barrel, a waste water barrel, a recovery tank and the like. The method realizes the efficient extraction, enrichment and recovery of the saponin in the canned asparagus processing wastewater, and optimizes the foam generation mode, the wastewater saponin concentration, and separation factors and conditions of different foaming agents. The results show that: the gas distributor has optimal effect, the content of 3000mg/L saponin is the optimal concentration for the extraction of foam separation saponin, and the composite microbial agent consisting of the pseudomonas aeruginosa bacterial agent, the lactobacillus plantarum bacterial agent and the bacillus subtilis bacterial agent can be used for the foam separation extraction of saponin wastewater with relatively low concentration, so that the air bubble efficiency can be obviously improved by at least 2-3 times compared with other modes.
The technical scheme of the invention is as follows:
The method for separating the saponin from the canned asparagus processing wastewater comprises the following steps:
(1) Uniformly stirring the saponin-containing canned asparagus processing wastewater and a compound microbial agent at 28-35 ℃, wherein the compound microbial agent accounts for 0.02-0.3% of the canned asparagus processing wastewater, and adjusting the pH value to 6-8 after fully mixing;
(2) Introducing the mixed solution in the step (1) into a foam separation device, blowing air by adopting a gas distributor to generate bubbles, and stopping ventilation when the foam cannot flow out from the top of the foam separation tower;
(3) Collecting the foam with saponin: separating at 15-40 deg.c for 5-10 min to collect foam;
(4) And (5) breaking foam of the collected foam to obtain defoaming liquid.
Preferably, the concentration of the saponin in the wastewater in the step (1) is 500-5000 mg/L, and the feeding amount is 100-150 mL.
Preferably, the concentration of the saponin in the wastewater in the above (1) is 3000mg/L.
Preferably, the compound microorganism strain in the step (1) consists of a pseudomonas aeruginosa microbial agent, a lactobacillus plantarum microbial agent and a bacillus subtilis microbial agent; pseudomonas aeruginosa agent: lactobacillus plantarum microbial inoculum: the bacillus subtilis microbial inoculum is 2-5: 1:3 to 5.
Preferably, in (1), the pseudomonas aeruginosa agent: lactobacillus plantarum microbial inoculum: the bacillus subtilis microbial inoculum is 5:1:3.
Preferably, in the step (1), the composite microbial agent accounts for 0.18% of the weight of the canned asparagus processing wastewater, and the pH value of the canned asparagus processing wastewater is between 6.8 and 7.6 after the composite microbial agent is fully mixed.
Preferably, in the above (2), the aeration flow rate of the gas distributor is 0.6 to 4.0L/min.
Preferably, in the above (3), the foam with saponin is collected; separating for 10min at 15-30 ℃.
Preferably, in the above (3), the foam with saponin is collected; separating for 10min at 15-25 ℃.
Preferably, in the above (4), the foam collected is left at 1 to 4℃for 8 to 10 hours to break foam, thereby obtaining a defoaming liquid.
The method of the present invention is realized by the foam separation apparatus described in (2), which is specifically as follows:
the invention has the beneficial effects that:
(1) The extraction temperature of the invention is room temperature (15-40 ℃), no heating treatment is needed, the extraction condition is loose, the energy consumption is low, the separation speed is high, and the separation time is only 5-10 min.
(2) The foam generation mode adopts a high-efficiency gas distributor, so that the recovery rate of the saponin is high; the recovery rate of the final saponin under the optimal process is up to 92.8 percent, and the enrichment ratio of the collected saponin is up to about 9 to 11.
(3) The concentration of the saponin in the wastewater is optimized, and the experiment shows that the content of 3000mg/L of saponin is the optimum concentration for extracting the foam separation saponin; the composite microbial agent consisting of the pseudomonas aeruginosa bacterial agent, the lactobacillus plantarum bacterial agent and the bacillus subtilis bacterial agent can be used for foam separation and extraction of relatively low-concentration active ingredient wastewater, and has high efficiency which is improved by 2-3 times compared with other modes.
(4) The invention adopts a specific foam separation device, and the stepped wall surfaces arranged on the inner wall of the box body and the outer wall of the separation cylinder in the device enhance the demulsification phenomenon and promote the generation of purified foam due to the existence of the edges and corners.
Drawings
FIG. 1 is a diagram showing the overall construction of a foam separation apparatus;
FIG. 2 is an interior view of a foam separation unit housing;
FIG. 3 is a cross-sectional view of the housing of the foam separation apparatus.
Detailed Description
The present invention will now be further described in connection with specific embodiments in order to enable those skilled in the art to better understand the invention.
In the foam separation technology, the solution contains surface active substances which are one of the necessary conditions for foam separation, and the invention discovers that the asparagus saponin has hydrophilic glycosyl and hydrophobic sapogenin which are excellent natural nonionic surface active components and have good foamability, so that the invention utilizes the foam separation technology to separate the saponin.
Example 1
(1) 150ML of canned asparagus processing wastewater containing saponins with different concentrations and different microbial agents are uniformly stirred at 30 ℃, and the pH value of the canned asparagus processing wastewater is adjusted to 7 after the canned asparagus processing wastewater is fully mixed;
The concentration of the saponin is examined to be 500mg/L, 1000mg/L, 2000mg/L, 3000mg/L, 4000mg/L and 5000mg/L respectively;
The microbial agents are examined to be 0.01%, 0.02%, 0.06%, 0.1%, 0.14%, 0.18%, 0.22%, 0.26%, 0.3%, 0.34% and 0.4% of the weight of the wastewater respectively, and the pH value is adjusted to 7 after the microbial agents are fully mixed;
The microbial agents examined were: bifidobacterium, saccharomyces cerevisiae, pseudomonas aeruginosa, lactobacillus plantarum, bacillus subtilis and composite microbial agents composed of the same;
in the early investigation, the ratio of the composite microbial agent consisting of two bacterial agents is 1:1, a step of; the ratio of the composite microbial agent consisting of the three bacterial agents is 3:1:3, a step of;
In the later investigation, a composite microbial agent consisting of a pseudomonas aeruginosa bacterial agent, a lactobacillus plantarum bacterial agent and a bacillus subtilis bacterial agent; the investigation proportion range is that the pseudomonas aeruginosa microbial inoculum: lactobacillus plantarum microbial inoculum: the bacillus subtilis microbial inoculum is 1 to 6:1:3 to 5;
(2) Introducing the mixed solution in the step (1) into a foam separation device, and blowing air at different air flow rates by using different foam generation modes to generate bubbles, and stopping ventilation when the foam cannot flow out from the top of the foam separation tower;
the gas flow rates (L/min) specifically examined were 0.02, 0.06, 0.08, 0.2, 0.6, 1, 1.4, 1.8, 2.2, 2.6, 2.8, 3.2, 3.6, 4.0, 4.4, respectively;
The foam generation modes examined were: directly blowing gas, distributing and homogenizing the gas;
(3) Collecting the foam with saponin: separating at 25deg.C for 10min;
(4) The collected foam was left at 2℃for 8 hours for foam breaking to obtain a defoaming liquid.
The method of the invention is to separate by using the foam separation device in (2), the device comprises a box body 1 with a sealed top, a foam outlet 4 is arranged at the upper part of the wall of the box body 1, a separation cylinder 2 is arranged in the box body 1, one side of the separation cylinder 2 is connected with a gas distributor 3, a liquid inlet pipe 5 passes through the box body 1 from outside the box body 1 to the inside of the separation cylinder 2, a return pipe 6 is also connected on the liquid inlet pipe 5, and the other end of the return pipe 6 is led to a position between the inner wall of the box body 1 and the outer wall of the separation cylinder 2.
Foam is blown up from the lower part of the liquid through the air pump, overflows in the separating cylinder 2, and contacts with the wall of the external box body 1 to cause demulsification, flows into a canal 8 at the bottom of the box body 1 along the wall of the box body 1, is recovered through a return pipe 6, and is filled into the separating cylinder 2 again for separation.
The gas distributor 3 comprises an air pipe and an air pump, the air pump is connected with a power supply, and the air pipe passes through the box body 1 from the outside of the box body 1 and is led into the lower part of the separation cylinder 2; the passage of gas from the lower part may be a longer flow of gas which favours the formation of bubbles.
The inner bottom surface of the box body 1 is of a structure which is slightly inclined from the middle to the periphery, a canal 8 is formed at the junction of the bottom surface of the box body 1 and the side wall of the box body 1, the canal 8 gradually deepens towards the joint direction of the return pipe 6, and the return pipe 6 is communicated with the canal 8.
The bottom surface structure can enable the demulsified water to automatically flow into the canal 8 under the action of gravity, and then flow into the return pipe 6 from high to low along the canal 8.
The inner wall of the box body 1 and the outer wall of the separating cylinder 2 are provided with stepped wall surfaces; the existence of the stepped wall surface due to the edges and corners is beneficial to the demulsification phenomenon and the purification of foam.
The inner wall surface of the separating cylinder 2 is spirally provided, and the uneven inner wall can make the collision of the flow and the liquid more intense, thereby facilitating the generation of foam.
A filter screen is arranged on the outer wall of the separating cylinder 2, the filter screen is respectively connected with the inner wall of the box body 1 and the outer wall of the separating cylinder 2, and the filter screen is positioned at the upper part or the middle part of the outer wall of the separating cylinder 2; the filter screen is parallel to the upper top surface of the box body 1, and the existence of the filter screen can support bubbles without influencing the downward flow of liquid.
The mesh of the filter screen is circular, and the area of the mesh is 3mm 2.
The liquid inlet pipe 5 is provided with a water pump, and the return pipe 6 is provided with a one-way valve.
The highest point of the return pipe 6 is not higher than the joint of the return pipe and the wall of the box body 1, and a universal wheel is arranged at the bottom outside the box body 1.
Be connected with agitator 7 on the feed liquor pipe 5, the back flow 6 is located between agitator 7 and the box 1 with the junction of feed liquor pipe 5, and liquid can be more even through stirring distribution before entering separating drum 2, and the foam quality that obtains is high, and also can make the foam produce more easily.
Specific investigation of
(1) The invention detects the influence of different foam generation modes on the recovery rate of saponin through experiments, and the experimental results are as follows:
TABLE 1 influence of different foam Generation modes and time on the recovery of saponins
It can be seen that by using a gas distributor for aeration in the present invention, the recovery of saponins is highest, while it is highly likely that the concentration of saponins and other substances separated may be the highest, but the time has little effect on its recovery of saponins, probably because the bubbles that can be swelled in the first few minutes have been mostly swelled; and finally, the gas distributor is selected to blow the gas for the next test.
(2) The invention detects the influence of different gas flow rates in the gas distributor on the recovery rate of the saponin through experiments, and the experimental results are as follows:
TABLE 2 influence of different gas flow rates on the recovery of saponins
| Air flow rate (L/min) | Recovery of saponins (%) |
| 0.02 | 40.2 |
| 0.06 | 45.0 |
| 0.08 | 54.5 |
| 0.2 | 54.4 |
| 0.6 | 65.2 |
| 1 | 66.0 |
| 1.4 | 68.2 |
| 1.8 | 70.3 |
| 2.2 | 71.1 |
| 2.6 | 72.0 |
| 2.8 | 78.1 |
| 3.2 | 77.6 |
| 3.6 | 74.3 |
| 4.0 | 73.4 |
| 4.4 | 68.9 |
The results show that the ventilation flow rate of the gas distributor is in the range of 0.6-4.0L/min, the influence on the recovery rate of the saponin is large, the recovery rate of the saponin can reach 65.2-78.1%, and the recovery rate of the saponin at the gas flow rate of 2.8L/min reaches the highest value of 78.1%.
(3) According to the invention, the influence of wastewater with different concentrations on the recovery rate of saponin is detected through experiments, and the experimental results are as follows:
TABLE 3 influence of the concentration of saponins in wastewater on the recovery of saponins
| Concentration of saponins (mg/L) | Recovery of saponins (%) |
| 500 | 48.3 |
| 1000 | 60.8 |
| 2000 | 68.5 |
| 3000 | 75.9 |
| 4000 | 78.3 |
| 5000 | 78.0 |
It can be seen that the recovery rate of the saponin in the wastewater with high concentration is also larger, and the wastewater with the concentration of 3000mg/L is finally selected for the next experiment in consideration of the fact that the concentration of the wastewater generated in actual industrial production is unlikely to be too high.
(4) According to the invention, the influence of different microbial agents on the recovery rate of saponin is detected through experiments, the microbial agents in the following table account for 0.2% of the weight of the canned asparagus processing wastewater, and the experimental results are as follows:
TABLE 4 Effect of different microbial inoculants and duty ratios on saponin recovery
The influence of different microbial agents on the saponin recovery rate is tested by using wastewater with the saponin concentration of 3000mg/L, and test results show that the influence of 3 microbial agents, namely the pseudomonas aeruginosa agent, the lactobacillus plantarum agent and the bacillus subtilis agent, on the saponin recovery rate is relatively small, but the saponin recovery rate generated by the compound microbial agent consisting of the pseudomonas aeruginosa agent, the lactobacillus plantarum agent and the bacillus subtilis agent 3 is the largest and is up to 91.5 percent, which is far higher than the saponin recovery rate of the compound microbial agent prepared by collocating any 2 microbial agents of the saccharomyces cerevisiae agent, the bifidobacterium and the 3 microbial agents;
And finally, selecting a composite microbial agent consisting of a pseudomonas aeruginosa bacterial agent, a lactobacillus plantarum bacterial agent and a bacillus subtilis bacterial agent for further testing.
(5) According to the invention, the influence of the compound microbial agents with different proportions on the recovery rate of saponin is detected through experiments, wherein the microbial agents in the following table account for 0.2% of the canned asparagus processing wastewater, and the proportions in the following table are pseudomonas aeruginosa microbial agents: lactobacillus plantarum microbial inoculum: the ratio of the bacillus subtilis microbial agents is as follows:
TABLE 5 influence of Compound microbial inoculants of different ratios on saponin recovery
| Different proportions | Recovery of saponins (%) |
| 1：1：3 | 77.8 |
| 1：1：4 | 72.9 |
| 1：1：5 | 77.7 |
| 2：1：2 | 89.2 |
| 2：1：3 | 86.0 |
| 2：1：4 | 86.5 |
| 2：1：5 | 85.0 |
| 2：1：6 | 77.3 |
| 3：1：3 | 85.8 |
| 3：1：4 | 85.2 |
| 3：1：5 | 87.0 |
| 4：1：3 | 88.8 |
| 4：1：4 | 85.4 |
| 4：1：5 | 84.8 |
| 5：1：3 | 91.7 |
| 5：1：4 | 85.0 |
| 5：1：5 | 83.3 |
| 5：1：6 | 76.5 |
| 6：1：3 | 75.8 |
| 6：1：4 | 78.4 |
| 6：1：5 | 80.5 |
The results showed that the pseudomonas aeruginosa agent: lactobacillus plantarum microbial inoculum: the bacillus subtilis microbial inoculum is 2-5: 1: the recovery rate of the saponin is greatly influenced within the range of 3 to 5, and is 85.0 to 91.7 percent, and the optimal ratio is 5:1:3, 91.7%.
(6) According to the invention, the influence of the composite microbial agents with different proportions in the canned asparagus processing wastewater on the recovery rate of the saponin is detected through experiments, and the experimental results are as follows:
TABLE 6 influence of Compound microbial inoculants of different ratios on saponin recovery
| Different duty cycle (%) | Recovery of saponins (%) |
| 0.01 | 73.8 |
| 0.02 | 86.6 |
| 0.06 | 90.0 |
| 0.10 | 92.1 |
| 0.14 | 92.5 |
| 0.18 | 92.8 |
| 0.22 | 91.6 |
| 0.26 | 92.0 |
| 0.30 | 91.2 |
| 0.34 | 88.9 |
| 0.40 | 89.2 |
The results show that the ratio of the composite microbial agent is in the range of 0.02-0.3%, the recovery rate of the saponin is greatly influenced, the ratio is 73.8-92.8%, and the optimal ratio is 0.18%.
Further, the invention observes the concrete change of the concentration of the saponin in the wastewater before and after the separation of the saponin, takes the wastewater with the concentration of the saponin of about 3000mg/L as the wastewater stock solution, adopts the optimal process condition of the screening to carry out six groups of soap base separation tests, and respectively detects the concentration of the soap base in the residual wastewater after the separation is finished, and the result is as follows:
The optimal process conditions adopted are as follows:
foam generation mode: the gas distributor is inflated;
flow rate of gas: 2.8L/min;
Composite microbial agent: pseudomonas aeruginosa agent: bacillus thuringiensis mycorrhizal preparation: the bacillus subtilis microbial inoculum is 5:1:3, a step of; the proportion of the asparagus can waste water is 0.18 percent.
TABLE 7 concentration variation of saponins in wastewater before and after soap base separation
As shown in the table above, the concentration of saponin in the defoaming liquid after separation is very high, the enrichment ratio is as high as 9.1-11.1%, and the concentration of saponin in the residual liquid is only 80.6-100.5 mg/L; this is matched with the higher recovery of saponins in the experimental results above, further confirming that the process of the invention has higher recovery of saponins.
Claims (4)
1. The method for separating the saponin from the canned asparagus processing wastewater is characterized by comprising the following steps of:
(1) Uniformly stirring saponin-containing canned asparagus processing wastewater and a compound microbial agent at 28-35 ℃, wherein the compound microbial agent accounts for 0.18% of the weight of the canned asparagus processing wastewater, and adjusting the pH value to 6-8 after fully mixing;
The composite microbial agent is pseudomonas aeruginosa agent: lactobacillus plantarum microbial inoculum: bacillus subtilis preparation = 5:1:3, a step of;
(2) Introducing the mixed solution in the step (1) into a foam separation device, and blowing air by adopting a gas distributor to generate bubbles, wherein the ventilation flow rate of the gas distributor is 2.8L/min;
(3) Collecting the foam with saponin: separating for 5-10 min at 15-40 ℃ and collecting foam;
(4) The foam is broken up, and defoaming liquid is obtained;
Wherein the foam separation apparatus described in (2) comprises: the top of the box body is sealed, a foam outlet is formed in the upper part of the wall of the box body, a separating cylinder is arranged in the box body, one side of the separating cylinder is connected with a gas distributor, a liquid inlet pipe penetrates through the box body from outside the box body and is led into the separating cylinder, a return pipe is also connected to the liquid inlet pipe, and the other end of the return pipe is led to a position between the inner wall of the box body and the outer wall of the separating cylinder; foam is blown up from the lower part of the liquid through the air pump, overflows in the separating cylinder, contacts the outer tank wall to cause demulsification, flows into the canal at the bottom of the tank along the tank wall, is recycled through the return pipe, and is filled into the separating cylinder again for separation;
the gas distributor comprises an air pipe and an air pump, the air pump is connected with a power supply, and the air pipe passes through the box body from outside the box body and is led into the lower part of the separating cylinder;
The bottom surface in the box body is of a structure which is slightly inclined from the middle to the periphery, a canal is formed at the junction of the bottom surface of the box body and the side wall of the box body, the depth of the canal gradually deepens towards the interface direction of a return pipe, and the return pipe is communicated with the canal;
The inner wall of the box body and the outer wall of the separating cylinder are provided with stepped wall surfaces, and the inner wall surface of the separating cylinder is provided with a spiral shape; a filter screen is arranged on the outer wall of the separating cylinder, the filter screen is respectively connected with the inner wall of the box body and the outer wall of the separating cylinder, and the filter screen is positioned at the upper part or the middle part of the outer wall of the separating cylinder; the filter screen is parallel to the upper top surface of the box body, the grid of the filter screen is round, and the area of the filter screen is 3 mm 2;
a water pump is arranged on the liquid inlet pipe, and a one-way valve is arranged on the return pipe;
the highest point of the return pipe is not higher than the joint of the return pipe and the wall of the box body, and the bottom outside the box body is provided with a universal wheel;
the liquid inlet pipe is connected with a stirring barrel, and the joint of the return pipe and the liquid inlet pipe is positioned between the stirring barrel and the box body.
2. The method for separating saponins from canned asparagus processing wastewater as claimed in claim 1, wherein in (1), the concentration of saponins in the wastewater is 500-5000 mg/mL.
3. The method for separating saponins from canned asparagus processing wastewater as claimed in claim 1 wherein in (1), a concentration of saponins in the wastewater is 3000 mg/L.
4. The method for separating saponins from canned asparagus waste water as claimed in claim 1, wherein in (4), the collected foam is placed at 1-4 ℃ for 8-10 hours for foam breaking to obtain defoaming liquid.
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| 植物乳杆菌发酵转化人参皂苷的研究;陈旸 等;《中国中药杂志》;20140430;第39卷(第8期);摘要以及第1437页 * |
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