A method for separating and purifying phenolic substances by embedding ultrasonic coupling celery cell wall fixed bed adsorption desorption

Abstract

The application discloses a method for separating and purifying phenolic substances by embedding ultrasonic coupling celery cell wall fixed bed adsorption and desorption. The method combines ultrasonic technology with fixed bed equipment and applies to the adsorption and desorption process of fruit and vegetable polyphenols on celery cell wall materials. Under the combined action of ultrasonic cavitation effect and mechanical effect, the texture of the celery cell wall material is changed in the adsorption / desorption process, and then the adsorption / desorption mass transfer parameters are changed, so that the adsorption and desorption of the celery cell wall on the polyphenols are strengthened, the breakthrough adsorption and desorption amounts are significantly improved, the desorption time is shortened, the purity of the polyphenols is improved, the breakthrough adsorption amount is increased by 15-23%, the desorption amount is increased by 17-26%, the desorption time is saved by 20-30%, and the purity of the polyphenols is increased by about 65%.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of food processing, and particularly relates to a method for separating and purifying phenolic substances by embedding ultrasonic coupling celery cell wall fixed bed adsorption / desorption. BACKGROUND

[0002] Fruits and vegetables are an important source of human food, providing a good eating experience and rich nutrients. In addition to fresh consumption, fruits and vegetables are often used to process fruit and vegetable juice and wine products. The fruit and vegetable processing industry generates a large amount of waste residues. At present, most of the fruit and vegetable waste is directly or roughly processed into feed or fertilizer, and a large part of the fruit and vegetable residues is incinerated as garbage waste, causing resource waste and environmental pressure. Fruits and vegetables contain a large amount of polyphenols such as anthocyanins, flavonoids, flavonols, and phenolic acids, which have health-promoting effects such as anti-inflammatory, antioxidant damage, anticancer, heart protection, liver protection, diabetes improvement, and immune enhancement. Therefore, purification and recovery of polyphenols from fruit and vegetable residues can help improve the comprehensive utilization efficiency of fruit and vegetable resources. The main components of plant cell walls include large molecules such as cellulose, hemicellulose, and pectin, as well as a small amount of protein. Plant cell walls are an important component of plant cells. After plant cells are broken, the contents flow out with the cell sap, and the remaining part is considered to be the cell wall component. Fixed bed separation is often used for purification of polyphenol extracts, but the commonly used filler resin has the disadvantages of large amount and high price. Cell wall materials have been proven to be useful for polyphenol purification. As the main component of fruit and vegetable residues, cell wall materials have a wide source and low price, and have good development prospects. Using fruit and vegetable cell wall materials as fixed bed fillers for polyphenol purification is a new direction for the comprehensive utilization of fruit and vegetable waste, and is conducive to promoting the value-added of the fruit and vegetable processing industry. Ultrasonic waves are mechanical waves with a frequency higher than 20 kHz. The mechanical and cavitation effects generated by the propagation of ultrasonic waves in liquid media can promote the migration of substances during processing, improve the separation and purification efficiency without damaging the effective components. Therefore, using ultrasonic coupling celery cell wall fixed bed adsorption / desorption is one of the effective ways to improve the purification efficiency of polyphenols.

[0003] In the prior art, patent CN 202222590210.3 discloses a fixed bed activated carbon adsorber, which comprises an adsorber body, an activated carbon support grid, a plurality of wire meshes, an alumina ball or gravel or other ceramic material layer, an activated carbon layer, a single layer of wire mesh, an adsorber gas inlet and an adsorber gas outlet. The device can avoid the influence of the adsorption process on the fixed bed layer, but it is only suitable for gas adsorption and is not suitable for liquid and other material adsorption. Patent CN 201980001691.8 discloses a method for separating and purifying grape polyphenols by using resin, which comprises the following steps: using an alkali solution to extract wine mud to obtain a polyphenol alkali extraction solution, using NKA-9 type or HPD600 type macroporous resin to adsorb the polyphenol components in the alkali extraction solution, and finally using ethanol to elute and recover the grape polyphenols. Although the method can obtain a high yield of grape waste polyphenols, the alkaline condition is not conducive to the stability of anthocyanins and other polyphenols, and the price of the resin used is high, which is not suitable for large-scale extraction of polyphenols in factories at low cost. SUMMARY

[0004] In order to solve the problems of insufficient recovery of fruit and vegetable polyphenol active substances by traditional methods, insufficient utilization of fruit and vegetable cell wall adsorption function, high price of traditional macroporous resin adsorption and low adsorption efficiency of cell wall materials on polyphenol substances in waste, the present application provides a method for separating and purifying phenolic substances by embedding ultrasonic coupling celery cell wall fixed bed adsorption and desorption. The method can recover a large amount of fruit and vegetable polyphenol active ingredients, which not only improves the purification efficiency, but also reduces the production operation cost and energy consumption.

[0005] In order to achieve the above purpose, the present application adopts the following technical scheme:

[0006] A method for separating and purifying phenolic substances by embedding ultrasonic coupling celery cell wall fixed bed adsorption and desorption, which obtains celery cell wall material from celery residues and uses it as fixed bed equipment filler to adsorb and desorb polyphenols in fruits and vegetables, and directly acts on the column bed with the help of ultrasonic waves to improve the adsorption and desorption efficiency of celery cell wall.

[0007] The method for purifying polyphenols by celery cell wall fixed bed according to the present application comprises the following steps:

[0008] (1) Celery cell wall preparation:

[0009] The celery residue is mixed with 90% ethanol aqueous solution at a material liquid ratio of 1:3-1:5 (g / mL) and boiled, then filtered. The filter residue is repeatedly mixed with 70% ethanol aqueous solution at a material liquid ratio of 1:10-1:20 (g / mL), then placed and filtered. Finally, the obtained filter residue is placed in a 40-50℃ oven and dried for 12h to obtain celery cell wall filler.

[0010] (2) Preparation of fruit and vegetable polyphenol crude extract:

[0011] The fruit and vegetable residues or waste residues are extracted with 50% ethanol aqueous solution at a material-liquid ratio of 1:20-1:30 (g / mL) for 6-8 h, the residue is filtered, and the ethanol is removed by rotary evaporation, and the obtained liquid is a crude fruit and vegetable polyphenol extract;

[0012] (3) adsorbing polyphenols:

[0013] The celery cell wall filler is fully swelled in deionized water, transferred into a fixed bed with ultrasonic equipment, and the crude fruit and vegetable polyphenol extract prepared in step (2) is flowed into the fixed bed, and the celery cell wall is used to adsorb the fruit and vegetable polyphenols with the aid of ultrasonic wave strengthening.

[0014] (4) removing impurities:

[0015] After adsorption, pure water is used for washing to remove impurities such as sugars and organic acids in the fixed bed;

[0016] (5) desorbing polyphenols:

[0017] After removing the impurities, a desorption solution is flowed into the fixed bed, and the celery cell wall is used to desorb the fruit and vegetable polyphenols with the aid of ultrasonic wave strengthening.

[0018] In step (2), the fruit and vegetable residues and waste residues are one or more of blueberry residues, blackberry residues, grape residues, aronia melanocarpa residues, mulberry residues, and black currant residues.

[0019] In step (3), the cell wall filler has a height of 15-30 cm; the sample flow rate of the crude fruit and vegetable polyphenol extract is 6-8 mL / min, the sample concentration is 2-4 g / L, the cooling temperature is 20-25°C, the adsorption temperature is 20-25°C, and the adsorption time is 20-30 h.

[0020] In step (4), the pure water washing flow rate is 6-8 mL / min, and the washing time is 1.5-3 h.

[0021] In step (5), the desorption solution is an ethanol aqueous solution with a volume fraction of 60-80%, the washing flow rate is 6-8 mL / min, the cooling temperature is 20-25°C, the desorption temperature is 20-25°C, and the desorption time is 3-5 h.

[0022] In steps (3) and (5), the ultrasonic power is 8-20 W / cm 2 , preferably 18 W / cm 2 , and the ultrasonic frequency is 20 kHz.

[0023] The application discloses a device for separating and purifying phenolic substances by embedding ultrasonic coupling celery cell wall fixed bed adsorption and desorption.

[0024] As a further preferred embodiment of the application, the device for separating and purifying phenolic substances by embedding ultrasonic coupling celery cell wall fixed bed adsorption and desorption is based on a fixed bed type cell wall material adsorption and desorption equipment, and a temperature sensor is added to the inner wall of the fixed bed container, and a cooling device is additionally arranged on the outer wall.

[0025] The device for separating and purifying phenolic substances by embedding ultrasonic coupling celery cell wall fixed bed adsorption and desorption can be obtained by modifying the existing fixed bed equipment.

[0026] The device for separating and purifying phenolic substances by embedding ultrasonic coupling celery cell wall fixed bed adsorption and desorption comprises an ultrasonic adsorption / desorption main equipment, a control unit, a circulating device and a feeding device, wherein the ultrasonic adsorption / desorption main equipment is composed of a fixed bed type adsorption / desorption container, and temperature sensors are welded to the front and rear sides in the fixed bed type adsorption / desorption container; an ultrasonic probe is embedded in the column bed; the control unit is connected in parallel with an ultrasonic generator and a temperature controller; the circulating device is composed of a low-temperature cooling circulating pump and a pipeline; the feeding device is composed of a peristaltic pump feeding device and a pipeline; the ultrasonic adsorption / desorption main equipment, the circulating device and the feeding device are sequentially connected through pipelines in series, and the control unit is connected with the ultrasonic adsorption / desorption main equipment through a circuit.

[0027] The inner side of the ultrasonic adsorption / desorption main equipment adsorption container is a temperature sensor, the ultrasonic probe is directly embedded in the column bed, and the ultrasonic probe and the temperature sensor directly contact the adsorption liquid and the cell wall filler.

[0028] The outer side of the ultrasonic adsorption / desorption main equipment adsorption / desorption container is a cooling pipe filled with cooling circulating water, which can keep the temperature of the filler and the liquid in the fixed bed in real time and prevent local overheating caused by the heat effect of ultrasonic waves.

[0029] Compared with the prior art, the device has the following beneficial effects:

[0030] (1) The device combines ultrasonic technology and fixed bed equipment and applies them to the adsorption and desorption process of celery cell wall material on fruit and vegetable polyphenols, changes the texture of the celery cell wall material under the combined action of ultrasonic cavitation effect and mechanical effect in the adsorption / desorption process, and further changes the adsorption / desorption mass transfer parameters, thereby strengthening the adsorption and desorption of the celery cell wall on polyphenols and significantly improving the breakthrough adsorption capacity (in actual application, the fixed bed is generally adsorbed to the breakthrough state, that is, the breakthrough point of the adsorption isotherm is reached)A / C A0 =0.1) and desorption capacity, and shortens the desorption time, and improves the purity of polyphenols. Compared with the fixed bed adsorption / desorption, the "breakthrough" adsorption capacity can be increased by 15-23%, the desorption capacity can be increased by 17-26%, the desorption time can be saved by about 20-30%, and the purity of polyphenols can be increased by about 65%.

[0031] (2) The embedded ultrasonic auxiliary fixed bed type celery cell wall material adsorption and desorption separation and purification of phenolic substances can effectively remove impurities such as sugars and acids while improving the mass transfer rate and recovery rate of target substances, and improving the purity of polyphenols. Moreover, the method has low adsorbent cost and low energy consumption, is simple to operate, only uses ethanol and does not use other organic reagents, and the ethanol can be recycled and reused. The operation process is green and pollution-free, and is a high-efficiency and environmentally-friendly phenolic substance purification method. BRIEF DESCRIPTION OF DRAWINGS

[0032] Figure 1 The embedded ultrasonic coupling celery cell wall fixed bed adsorption and desorption separation and purification of phenolic substances device schematic diagram; wherein, 1-fixed bed ultrasonic adsorption / desorption container, 2-ultrasonic generator and temperature controller, 3-low temperature cooling circulating pump, 4-temperature sensor, 5-ultrasonic probe, 6-peristaltic pump, 7-cooling pipe, 8-liquid inlet, 9-cell wall material, 10-transport pipeline, 11-liquid outlet (with filter membrane), 12-cell wall material filling port, 13-cell wall material outlet.

[0033] Figure 2 Adsorption flow breakthrough curve comparison of examples 1-3 and comparative example 1; wherein the adsorption temperature is 20°C, the adsorption time is 20h, only the fixed bed, 9W / cm 2 ultrasonic combined fixed bed device, 18W / cm 2 Adsorption flow breakthrough curve of ultrasonic combined fixed bed device.

[0034] Figure 3 Desorption curve comparison of examples 1-3 and comparative example 1; wherein the desorption temperature is 20°C, the desorption time is 3h, only the fixed bed, 9W / cm 2 ultrasonic combined fixed bed device, 18W / cm 2 Desorption curve of ultrasonic combined fixed bed device. DETAILED DESCRIPTION

[0035] Example 1

[0036] An embedded ultrasonic-coupled celery cell wall fixed-bed adsorption / desorption separation and purification device includes an ultrasonic adsorption / desorption main unit, a control unit, a circulation device, and a feeding device. The ultrasonic adsorption / desorption main unit is a fixed-bed adsorption / desorption container 1. Temperature sensors 4 are welded to the front and rear sides inside the container, and ultrasonic probes 5 are directly embedded in the column bed. The ultrasonic probes 4 and temperature sensors 5 are in direct contact with the adsorption liquid. A cooling pipe 7 is located in the outer jacket of the container 1, which can maintain the temperature of the cell wall packing, adsorption liquid, and desorption liquid in real time to prevent local overheating caused by ultrasound. The control unit consists of an ultrasonic generator and a temperature controller 2 connected in parallel. The circulation device consists of a low-temperature cooling circulation pump 3 and connected pipes. The feeding device consists of a peristaltic pump 6 and related pipes. The ultrasonic adsorption / desorption main unit, the circulation device, and the feeding device are connected in series, and the control unit is connected to the ultrasonic adsorption / desorption main unit through a circuit.

[0037] Example 2

[0038] (1) The celery residue was mixed with 90% ethanol aqueous solution at a material-to-liquid ratio of 1:3 (g / mL) and boiled for 30 min. The ethanol was removed by filtration. The residue was mixed with 70% ethanol aqueous solution at a material-to-liquid ratio of 1:10 (g / mL). After standing, the residue was filtered and collected. This process was repeated six times. The final residue was placed in an oven at 40℃ and dried for 12 h to obtain celery cell wall material.

[0039] (2) The blueberry pomace was extracted with a 50% ethanol aqueous solution at a material-to-liquid ratio of 1:20 (g / mL) for 6 hours, the residue was filtered, and the ethanol was removed by rotary evaporation to obtain the adsorbed liquid.

[0040] (3) Fill the water tank of the low-temperature cooling liquid circulation pump with clean water, turn on the cooling circulation pump and set the cooling temperature to 15℃. Pour 175g of fully swollen celery cell wall material into the adsorption container through the feed inlet. Turn on the main cooling and ultrasonic switch, set the adsorption temperature of the adsorption container to 20℃, and wait for the cooling temperature to reach the set requirement. Turn on the peristaltic pump power, set the pure water flow rate to 6mL / min, and equilibrate for 1.5h. After the column bed is equilibrated, set the injection flow rate of the crude polyphenol extract to 6mL / min and rotate the ultrasonic knob to set the ultrasonic power to 9W / cm. 2 The ultrasonic frequency was 20kHz, and adsorption was performed for 20 hours.

[0041] (4) Turn the ultrasonic power knob back to 0W, turn off the upper and lower peristaltic pumps to stop adsorption; turn on the upper and lower peristaltic pumps, set the pure water flow rate to 6mL / min, and perform 1.5h of impurity rinsing.

[0042] (5) Return the ultrasonic power knob to 0W, turn off the upper and lower peristaltic pumps to stop rinsing; set the desorption temperature of the adsorption container to 20℃, and wait until the desorption temperature reaches the set requirement. Then, turn on the upper and lower peristaltic pumps, set the flow rate of the 60% ethanol aqueous solution to 6mL / min, and rotate the ultrasonic knob to set the ultrasonic power to 9W / cm. 2 The ultrasonic frequency was 20kHz, followed by 3 hours of desorption.

[0043] (6) Turn the ultrasonic power knob back to 0W, turn off the cooling switch, the main ultrasonic switch, and the peristaltic pump in sequence to stop adsorption; collect the cell wall from the adsorbent outlet, and turn off the peristaltic pump after the material collection is completed.

[0044] (7) Pour the washing water into the adsorption container through the feed inlet, turn on the cooling and ultrasonic main switch, turn on the ultrasonic and peristaltic pump for 30 minutes of cleaning, then turn off the cooling pump power and open the drain outlet under the water tank to drain the water.

[0045] Example 3

[0046] (1) The celery residue was mixed with 90% ethanol aqueous solution at a material-to-liquid ratio of 1:3 (g / mL) and boiled for 30 min. The ethanol was removed by filtration. The residue was mixed with 70% ethanol aqueous solution at a material-to-liquid ratio of 1:10 (g / mL). After standing, the residue was filtered and collected. This process was repeated six times. The final residue was placed in an oven at 40℃ and dried for 12 h to obtain celery cell wall material.

[0047] (2) The blueberry pomace was extracted with a 50% ethanol aqueous solution at a material-to-liquid ratio of 1:20 (g / mL) for 6 hours, the residue was filtered, and the ethanol was removed by rotary evaporation to obtain the adsorbed liquid.

[0048] (3) Fill the water tank of the low-temperature cooling liquid circulation pump with clean water, turn on the cooling circulation pump and set the cooling temperature to 15℃. Pour 175g of fully swollen celery cell wall material into the adsorption container through the feed inlet, set the adsorption temperature of the adsorption container to 20℃, and wait for the cooling temperature to reach the set requirement. Turn on the peristaltic pump power, set the pure water flow rate to 6mL / min, and equilibrate for 1.5h. After the column bed is equilibrated, set the injection flow rate of the crude polyphenol extract to 6mL / min and rotate the ultrasonic knob to set the ultrasonic power to 18W / cm. 2 The ultrasonic frequency was 20kHz, and adsorption was performed for 20 hours.

[0049] (4) Turn the ultrasonic power knob back to 0W, turn off the upper and lower peristaltic pumps to stop adsorption; turn on the upper and lower peristaltic pumps, set the pure water flow rate to 6mL / min, and perform 1.5h of impurity rinsing.

[0050] (5) Return the ultrasonic power knob to 0W, turn off the upper and lower peristaltic pumps to stop rinsing; set the desorption temperature of the adsorption container to 20℃, and wait until the desorption temperature reaches the set requirement. Then, turn on the upper and lower peristaltic pumps, set the flow rate of the 60% ethanol aqueous solution to 6mL / min, and rotate the ultrasonic knob to set the ultrasonic power to 18W / cm. 2 The ultrasonic frequency was 20kHz, followed by 3 hours of desorption.

[0051] (6) Turn the ultrasonic power knob back to 0W, turn off the cooling switch, the main ultrasonic switch, and the peristaltic pump in sequence to stop adsorption; collect the cell wall from the adsorbent outlet, and turn off the peristaltic pump after the material collection is completed.

[0052] (7) Pour the washing water into the adsorption container through the feed inlet, turn on the cooling and ultrasonic main switch, turn on the ultrasonic and peristaltic pump for 30 minutes of cleaning, then turn off the cooling pump power and open the drain outlet under the water tank to drain the water.

[0053] Table 1. Comparison of polyphenol purity after Examples 1-3 and fixed-bed adsorption / desorption only.

[0054] Treatment group Polyphenol purity (%) Before purification 8.90±0.24c Fixed bed only 71.61±0.11b Fixed bed combined with ultrasound 9 W / cm 2 ]] 73.51±0.67a Fixed bed combined with ultrasound 18 W / cm 2 ]] 74.20±0.37a

[0055] Note: Different lowercase letters indicate significant differences in polyphenol purity (p<0.05).

[0056] As shown in Table 1, the purity of polyphenols before adsorption / desorption purification was only 8.90%. However, after purification with fixed-bed celery cell wall material, the purity of polyphenols in the crude extract of fruits and vegetables significantly increased to 71.61%. After purification with ultrasound-assisted fixed-bed celery cell wall material, the purity of polyphenols in the crude extract of fruits and vegetables increased to about 74%, indicating that ultrasound combined with a fixed-bed device can effectively improve the purity of polyphenols.

[0057] Table 2 Comparison of polyphenol "breakthrough" adsorption capacity between Examples 1-3 and fixed-bed adsorption only.

[0058] Treatment group Polyphenol "breakthrough" adsorption capacity (mg / g) Fixed bed only 47.44±3.17b Fixed bed combined with ultrasound 9 W / cm 2 ]] 54.57±2.88a Fixed bed combined with ultrasound 18 W / cm 2 ]] 58.34±5.16a

[0059] Note: Different lowercase letters indicate significant differences in the "breakthrough" adsorption capacity of polyphenols (p<0.05).

[0060] As shown in Table 2, the "breakthrough" adsorption capacity of polyphenols by the fixed-bed celery cell wall material alone was 47.44 mg / g. After the adsorption by the fixed-bed celery cell wall material with ultrasound assistance, the "breakthrough" adsorption capacity of polyphenols was significantly increased to 54.57 mg / g and 58.34 mg / g, indicating that the ultrasound combined with the fixed-bed device can effectively improve the adsorption capacity of celery cell wall material for polyphenols.

[0061] Comparative Example 1

[0062] Except for the ultrasonic probe, the other conditions are the same as in Example 2, and the polyphenols in the crude extract of fruit and vegetable polyphenols are purified using only a fixed bed without ultrasonication.

[0063] Depend on Figure 2 It can be seen that embedded ultrasonic coupling adsorption in a fixed bed of celery cell walls can effectively improve the adsorption capacity of celery cell wall materials. When the adsorption "breakthrough" state is reached (C... A / C A0 =0.1), with only the fixed bed on, the adsorption "breakthrough" was reached in about 756 minutes, with an adsorption capacity of 47.44 mg / g and 18 W / cm². 2 Ultrasonic adsorption reached its adsorption "breakthrough" at around 865 minutes, with an adsorption capacity as high as 58.34 mg / g.

[0064] Depend on Figure 3 It can be seen that embedded ultrasonic coupling adsorption in a fixed bed of celery cell walls can effectively improve the desorption rate and significantly increase the desorption capacity. Desorption under fixed bed treatment alone reached equilibrium in 150 min (desorption rate reached 95%), with a desorption capacity of 45.10 mg / g and 18 W / cm². 2 Ultrasonic-assisted desorption reached desorption equilibrium in 115 min, with a desorption capacity of 56.48 mg / g.

[0065] The embodiments of the present invention have been described in detail above, but these are merely examples for ease of understanding and should not be considered as limiting the scope of the present invention. Similarly, any person skilled in the art can make various possible equivalent changes or substitutions based on the technical solutions and preferred embodiments described in the present invention, but all such changes or substitutions should fall within the protection scope of the claims of the present invention.

Claims

1. A method for separating and purifying phenolic substances by adsorption-desorption in an embedded ultrasonic-coupled celery cell wall fixed bed, characterized in that, The method obtains celery cell wall material from celery residue as an adsorbent. While using a fixed-bed device to adsorb and desorb phenolic substances in fruits and vegetables, ultrasound is directly applied to the column bed to enhance the adsorption and desorption of phenolic substances by the cell wall material. The method includes the following steps: (1) Preparation of celery cell walls: Celery residue was mixed with 90% ethanol aqueous solution at a material-to-liquid ratio of 1:3-1:5 (g / mL), boiled, and then filtered. The filter residue was repeatedly mixed with 70% ethanol aqueous solution at a material-to-liquid ratio of 1:10-1:20 (g / mL), allowed to stand, and filtered. The final filter residue was placed in an oven at 40-45℃ and dried for 12 hours to obtain celery cell wall filler. (2) Preparation of crude extract of fruit and vegetable polyphenols: Extract fruit and vegetable residues or waste residues with 50% ethanol aqueous solution at a material-to-liquid ratio of 1:20-1:30 (g / mL) for 6-8 hours. Filter the residue and remove the ethanol by rotary evaporation. The resulting liquid is the crude extract of fruit and vegetable polyphenols. (3) Adsorption of polyphenols: The celery cell wall packing was fully swollen in deionized water and transferred into a fixed bed equipped with an ultrasonic device. The column bed was fully balanced with pure water. The crude extract of fruit and vegetable polyphenols prepared in step (2) was then flowed into the fixed bed. The adsorption of fruit and vegetable polyphenols by the celery cell wall was enhanced by ultrasonic waves. (4) Remove impurities: After adsorption is complete, rinse with pure water to remove sugar and organic acid impurities from the fixed bed. (5) Desorption of polyphenols: After removing impurities, desorption liquid is flowed into the fixed bed, and ultrasound is used to enhance the desorption of fruit and vegetable polyphenols by the celery cell wall. In steps (3) and (5), the ultrasonic power is 8-20 W / cm. 2 The ultrasonic frequency is 20kHz; In step (3), the height of the cell wall packing is 15-30cm; the injection flow rate of the crude extract of fruit and vegetable polyphenols is 6-8mL / min, the injection concentration is 2-4g / L, the cooling temperature is 20-25℃, the adsorption temperature is 20-25℃, and the adsorption time is 20-30h. In step (4), the flow rate of pure water rinsing is 6-8 mL / min, and the rinsing time is 1.5-3 h. In step (5), the desorption solution is an ethanol aqueous solution with a volume fraction of 60-80%, the rinsing flow rate is 6-8 mL / min, the cooling temperature is 20-25℃, the desorption temperature is 20-25℃, and the desorption time is 3-5 h.

2. The method according to claim 1, characterized in that... The fruit and vegetable residues and waste residues are one or more of the following: blueberry residue, blackberry residue, strawberry residue, grape residue, raspberry residue, mulberry residue, and blackcurrant residue.

3. An embedded ultrasonic-coupled celery cell wall fixed bed adsorption-desorption separation and purification device for the method of claim 1 is based on a fixed bed adsorption-desorption device, using celery cell walls as packing material, embedding an ultrasonic probe in the fixed bed layer, adding a temperature sensor to the inner side of the fixed bed container wall, and adding a cooling device to the outer wall.

4. The apparatus for embedded ultrasonic coupling of celery cell wall fixed bed adsorption-desorption separation and purification of phenolic substances according to claim 3, characterized in that, The device includes an ultrasonic adsorption / desorption main unit, a control unit, a circulation device, and a feeding device. The ultrasonic adsorption / desorption main unit consists of a fixed-bed adsorption / desorption container, with temperature sensors welded to the front and rear sides inside the container. An ultrasonic probe is embedded in the column bed. The control unit consists of an ultrasonic generator and a temperature controller connected in parallel. The circulation device consists of a low-temperature cooling circulation pump and pipelines. The feeding device consists of a peristaltic pump feeding device and pipelines. The ultrasonic adsorption / desorption main unit, the circulation device, and the feeding device are connected in series via pipelines, and the control unit is connected to the ultrasonic adsorption / desorption main unit via a circuit.

5. The apparatus for embedded ultrasonic coupling of celery cell wall fixed bed adsorption-desorption separation and purification of phenolic substances according to claim 4, characterized in that, The outer side of the adsorption / desorption container of the ultrasonic adsorption / desorption main equipment is a cooling pipe filled with circulating cooling water.

Images