CN112125947A - Method and equipment for removing plasticizer from ginsenoside extract - Google Patents

Method and equipment for removing plasticizer from ginsenoside extract Download PDF

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CN112125947A
CN112125947A CN202010823501.5A CN202010823501A CN112125947A CN 112125947 A CN112125947 A CN 112125947A CN 202010823501 A CN202010823501 A CN 202010823501A CN 112125947 A CN112125947 A CN 112125947A
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ginsenoside
connecting rod
extract
ginsenoside extract
gear
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胡晓雁
孙振蛟
张竹
郑树元
李伟
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Ganzhou HLKJ Biotechnology Co ltd
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Ganzhou HLKJ Biotechnology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07JSTEROIDS
    • C07J17/00Normal steroids containing carbon, hydrogen, halogen or oxygen, having an oxygen-containing hetero ring not condensed with the cyclopenta(a)hydrophenanthrene skeleton
    • C07J17/005Glycosides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/25Araliaceae (Ginseng family), e.g. ivy, aralia, schefflera or tetrapanax
    • A61K36/258Panax (ginseng)
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14Ultrafiltration; Microfiltration
    • B01D61/145Ultrafiltration
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14Ultrafiltration; Microfiltration
    • B01D61/16Feed pretreatment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14Ultrafiltration; Microfiltration
    • B01D61/18Apparatus therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2311/00Details relating to membrane separation process operations and control
    • B01D2311/26Further operations combined with membrane separation processes
    • B01D2311/2626Absorption or adsorption
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2311/00Details relating to membrane separation process operations and control
    • B01D2311/26Further operations combined with membrane separation processes
    • B01D2311/2673Evaporation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2311/00Details relating to membrane separation process operations and control
    • B01D2311/26Further operations combined with membrane separation processes
    • B01D2311/2688Biological processes

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Abstract

The invention relates to the technical field of ginsenoside extraction, in particular to a method and equipment for removing a plasticizer from a ginsenoside extract, which comprises the following steps of preparing a ginsenoside extract solution; obtaining a ginsenoside extract solution, heating the ginsenoside extract solution to a certain temperature, and adding an enzyme preparation for enzymolysis to obtain a ginsenoside enzymolysis liquid; obtaining ginsenoside enzymolysis liquid, and performing first membrane separation treatment on the ginsenoside enzymolysis liquid to obtain ginsenoside extract clarified liquid; obtaining a ginsenoside extract clear solution, and performing adsorption treatment on the ginsenoside extract clear solution to obtain a ginsenoside lower column solution; the method comprises the steps of obtaining ginsenoside lower column liquid, carrying out vacuum low-temperature concentration treatment on the ginsenoside lower column liquid, and then carrying out spray drying to obtain a ginsenoside extract.

Description

Method and equipment for removing plasticizer from ginsenoside extract
Technical Field
The invention relates to the technical field of ginsenoside extraction, in particular to a method and equipment for removing a plasticizer from a ginsenoside extract.
Background
Ginsenoside (Ginsenoside) is a steroid compound, triterpene saponin. Mainly exists in ginseng medicinal materials. Ginsenosides are considered as active ingredients in ginseng and thus have been the object of research. The total saponins of ginseng stem and leaf are the total saponins prepared by processing the dry stems and leaves of ginseng, and have slight odor and bitter taste. The main components comprise ginsenoside Rg1, Re, Rc, Rb1, Rb2, Rd and the like, and the ginsenoside has the functions of nourishing and strengthening, soothing the nerves and promoting intelligence and enhancing immunity, and the traditional extraction method of the ginsenoside mainly comprises water extraction or alcohol extraction.
Chinese patent CN214a53585.9 discloses a method for extracting ginsenoside, which comprises the following steps: treating raw materials; extracting with an extraction solvent; treating an extracting solution; resin adsorption refining; removing impurities by alkali washing; eluting the components; decoloring the eluent; and (4) concentrating and the like. The method adopts specific alkaline washing impurity removal process, and combines with corresponding water extraction or alcohol extraction method, so that the product yield of the prepared ginsenoside extract is greatly improved to 7-7.5%, and the content of ginsenoside (Rb1+ Rb2+ Rc + Rd + Re + Rg1) is more than or equal to 45%.
The plasticizer is a polymer material auxiliary agent widely used in industrial production, mainly comprises phthalate, and is widely applied to plastic packaging bags and plastic pipelines. The ginsenoside extract is very easy to contact with the products in the processes of storage, transportation and processing of raw materials, and meanwhile, the general ginsenoside extract is prepared by extracting with organic solvent solvents such as ethanol and the like, and the organic solvent is very easy to dissolve out a plasticizer, so that the risk of exceeding the standard in the ginsenoside extract is very high. There are already defined limits on plasticizer specifications for food safety in europe, taiwan, etc.
Disclosure of Invention
In order to solve the technical problems, the technical scheme solves the problem that the risk that the plasticizer in the ginsenoside extract exceeds the standard in the existing preparation process is very high, and the method and the equipment hydrolyze the carboxylic ester on the molecular structure of the phthalate plasticizer under the action of enzyme to decompose the carboxylic ester into phthalic acid and corresponding alcohols and adsorb and remove the phthalic acid by adopting anion resin.
In order to achieve the above purposes, the technical scheme adopted by the invention is as follows:
the method for removing the plasticizer from the ginsenoside extract comprises the following steps:
preparing a ginsenoside extract solution;
obtaining the ginsenoside extract solution, heating the ginsenoside extract solution to a certain temperature, adding an enzyme preparation for enzymolysis, and fully stirring to obtain a ginsenoside enzymolysis solution;
obtaining the ginsenoside enzymolysis liquid, and carrying out first membrane separation treatment on the ginsenoside enzymolysis liquid to obtain a ginsenoside extract clarified liquid;
obtaining the ginsenoside extract clear solution, and performing adsorption treatment on the ginsenoside extract clear solution to obtain ginsenoside lower column solution;
and (3) obtaining the ginsenoside lower column liquid, carrying out vacuum low-temperature concentration treatment on the ginsenoside lower column liquid, and then carrying out spray drying to obtain the ginsenoside extract with the phthalate plasticizer less than 5 ppb.
Optionally, the preparation of the ginsenoside extract solution specifically comprises:
obtaining untreated ginsenoside extraction raw products, wherein the ginsenoside extraction raw products are a ginseng root extract, an American ginseng extract, a ginseng stem and leaf extract and a panax notoginseng extract containing ginsenoside, and the content of the ginsenoside is 3-30%;
adding purified water 5-15 times the weight of the ginsenoside extraction raw product, and dissolving the ginsenoside extraction raw product to obtain ginsenoside extract solution;
obtaining the ginsenoside extract solution, and adjusting the pH of the ginsenoside extract solution to obtain the ginsenoside extract solution, wherein the pH is adjusted by using one or a mixture of citric acid and sodium citrate as buffer salt.
Optionally, the ginsenoside extract solution is obtained, the ginsenoside extract solution is heated to a certain temperature, an enzyme preparation is added for enzymolysis, the mixture is fully stirred, the ginsenoside extract solution in the ginsenoside enzymolysis liquid is heated to 3-5 ℃, the enzyme preparation is one or a combination of lipase, pig liver carboxylesterase and phospholipase, the adding amount of the enzyme preparation is 0.2-5% of the weight of the raw product of the ginsenoside extraction, and the enzymolysis time is 2-5 hours.
Optionally, a ceramic membrane is adopted for clarification in the first membrane separation treatment, and the aperture of the ceramic membrane is 5-30 nm.
Optionally, obtaining the ginsenoside extract clarified liquid, performing adsorption treatment on the ginsenoside extract clarified liquid to obtain ginsenoside lower column liquid, performing adsorption treatment on the obtained ginsenoside lower column liquid by using an adsorption column containing anion resin filler, and collecting the lower column liquid of the adsorption column to obtain the ginsenoside lower column liquid, wherein the anion resin filler is one of D31, D941 and LX-T5.
Optionally, the vacuum low-temperature concentration temperature is 5-70 ℃, and the vacuum degree is-0.06 mpa to-0.09 mpa.
Further, still provide the desorption equipment of plasticizing agent in ginsenoside extract product, including ultrafiltration system, ultrafiltration system includes column ultrafiltration filter, be equipped with the filter core in the ultrafiltration filter, the filter core includes outer barrel, the ceramic membrane filter core, first end cover and second end cover, outer barrel has the direction along axial extension, seted up a plurality of rings of through-hole layer on the outer wall of outer barrel, the through-hole layer includes a plurality of first through-holes, the first through-hole circumference of same through-hole layer distributes on the outer wall of outer barrel, the ceramic membrane filter core is installed in outer barrel, the ceramic membrane filter core includes a plurality of hollow membrane silks that are the linear type and set up, at one end of the ceramic membrane filter element, the end parts of the hollow membrane filaments are sealed, at the other end of the ceramic membrane filter element, the adjacent hollow membrane filaments are sealed, one end of the outer cylinder body is detachably connected with the first end cover, and the other end of the outer cylinder body is detachably connected with the second end cover.
Optionally, a water outlet is formed in the first end cover, a water outlet is formed in the second end cover, a water outlet nozzle is further arranged on the second end cover, one end of the water outlet nozzle is used for being connected with the outside, the other end of the water outlet nozzle is connected with the water outlet, at least one sealing ring groove is formed in the water outlet nozzle and used for installing a sealing ring for sealing, the ceramic membrane filter element is of a hollow structure, a plugging piece is arranged at one end, close to the ceramic membrane filter element, of the outer cylinder body, the plugging piece is installed in a hollow cavity at one end of the ceramic membrane filter element, a plurality of partition plates are further arranged on the filter element, the axis of the cylinder body except for the partition plates is uniformly distributed in the circumferential direction, one ends.
It is optional, first end cover includes first lid and the fixed barrel who matches with the cavity of ceramic membrane filter core, be provided with the outlet on the first lid, fixed barrel is hollow structure, the one end and the outlet butt joint of fixed barrel, the other end of fixed barrel stretches into in the cavity of ceramic membrane filter core one end, the other end tip of fixed barrel is equipped with the breach along the axis direction, the one end opening that the breach is close to the other end tip of fixed barrel is big, the one end opening that the other end tip of fixed barrel was kept away from to the breach is little, be equipped with a plurality of strengthening ribs on the outer wall of first end cover, form the guiding gutter between the adjacent strengthening rib.
Optionally, one end of the water outlet nozzle, which is far away from the second end cover, extends to the outside of the column type membrane separation filter, a lantern ring is sleeved on a part of the water outlet nozzle, which is exposed out of the column type membrane separation filter, a first rack is arranged on the lantern ring, and a lifting mechanism is arranged on the side part of the first rack;
the lifting mechanism comprises a fixed seat, a driving motor, a first gear, a second gear, a first connecting rod, a second connecting rod, a third connecting rod, a sliding rod, an installation sleeve, a fourth connecting rod, a fixed plate and a second rack, wherein:
a fixed seat is fixed on the side part of the first rack, a driving motor is arranged at one end of the fixed seat, an output shaft of the driving motor is in transmission connection with a first gear, the first gear is in rotary connection with the fixed seat, a second gear is arranged on the side part of the first gear, the second gear is in rotary connection with the fixed seat and is meshed with the first gear, a first connecting rod is eccentrically arranged on the first gear, a second connecting rod is eccentrically arranged on the second gear, one end of the first connecting rod is connected with the first gear, one end of the second connecting rod is connected with the second gear, and the other end of the first connecting rod is hinged with the other end of the second connecting rod;
first connecting rod and the articulated department of second connecting rod articulate there is the third connecting rod, the other end of third connecting rod is equipped with the slide bar, the sliding seat sliding connection who sets up on slide bar and the fixing base, another pot head of slide bar is equipped with two installation covers, all be equipped with the fourth connecting rod on every installation cover, parallel arrangement between two fourth connecting rods, be equipped with the driving piece on one of them fourth connecting rod, the driving piece is used for driving this fourth connecting rod and rotates, the one end and the installation cover of fourth connecting rod are connected, the other end of fourth connecting rod is connected with the fixed plate, be equipped with the second rack with first rack toothing on the fixed plate.
Compared with the prior art, the invention has the beneficial effects that:
the national and European standards adopt a GC-MS mode to carry out quantitative determination on the detection of the phthalate plasticizer, the detection limit is more than 0.1ppm, the regulations in Taiwan adopt LC-MS-MS to carry out determination, the detection limit is lower (0.05ppm), and the detection is more sensitive. After the ginsenoside extract is removed by adopting the method, the detection limit of the phthalate plasticizer by adopting the LC-MS-MS method can be less than 0.05 ppm.
In the method, carboxylic ester on the molecular structure of a phthalate plasticizer is hydrolyzed under the action of enzyme to be decomposed into phthalic acid and corresponding alcohols, and the phthalic acid is adsorbed and removed by adopting anion resin. Meanwhile, the introduced enzyme preparation is separated by utilizing the characteristic that macromolecular components are intercepted by the ceramic membrane after enzymolysis, and no additional additive is introduced into the final product.
The traditional plasticizer removal method mainly comprises an organic solvent extraction method and a supercritical extraction method. The organic solvent extraction method has a certain effect, can remove the phthalate plasticizer to the level of 0.1-1ppm, and simultaneously needs to use limiting solvents such as normal hexane, trichloromethane, dichloromethane and the like, and certain solvent residues can be introduced into the final product to influence the safety of the product. The supercritical extraction method has certain limitations in industrial application and higher cost. The whole process of the method is completed by adopting a biological enzyme technology, is green and safe, has little influence on the original components, and is very easy for industrial production.
Drawings
FIG. 1 is a schematic flow diagram of the process of the present invention;
FIG. 2 is a schematic view of a specific process in S100) of the present invention;
FIG. 3 is a first schematic structural diagram of the apparatus of the present invention;
FIG. 4 is a second schematic structural view of the apparatus of the present invention;
FIG. 5 is a schematic view of the construction of the lifting mechanism of the apparatus of the present invention;
FIG. 6 is a schematic view of the arrangement at the cartridge of the apparatus of the present invention;
FIG. 7 is a schematic illustration of an explosion at the cartridge in the apparatus of the present invention;
FIG. 8 is an enlarged solid view at A of FIG. 7;
FIG. 9 is a schematic view of the structure of the apparatus of the present invention at the first end cap;
FIG. 10 is a schematic view of the structure at the second end cap of the apparatus of the present invention;
fig. 11 is an enlarged schematic view at B in fig. 10.
Description of reference numerals:
1-outer cylinder; 1 a-a first via;
2-a ceramic membrane filter element;
3-a first end cap; 3 a-a water outlet; 3 b-reinforcing ribs; 3 c-a diversion trench; 3 d-a first cover; 3 e-fixing the cylinder; 3e 1-notch;
4-a second end cap; 4 a-a water outlet; 4 b-a water outlet nozzle; 4 c-sealing ring groove;
5-plugging piece;
6-a partition plate;
7-a collar;
8-a first rack;
9-lifting mechanism; 9 a-a fixed seat; 9a 1-sliding seat; 9 b-a drive motor; 9 c-a first gear; 9 d-second gear; 9 e-a first link; 9 f-a second link; 9 g-third link; 9 h-a slide bar; 9 i-mounting sleeve; 9 j-fourth link; 9 k-fixing plate; 9 m-second rack.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art.
Referring to fig. 1, the method includes the following steps:
s100) preparing a ginsenoside extract solution, specifically, referring to fig. 2, including the steps of:
s110) obtaining an untreated ginsenoside extraction raw product, wherein the ginsenoside extraction raw product is a ginseng root extract, an American ginseng extract, a ginseng stem and leaf extract and a panax notoginseng extract containing ginsenoside, and the content of the ginsenoside is 3-30%;
s120) adding purified water which is 5-15 times of the weight of the ginsenoside extraction raw product, and dissolving the ginsenoside extraction raw product to obtain a ginsenoside extract dissolving solution;
s130) obtaining a ginsenoside extract solution, and adjusting the pH of the ginsenoside extract solution to obtain a ginsenoside extract solution, wherein the pH is adjusted by using one or a mixture of citric acid and sodium citrate as a buffer salt;
s200) obtaining a ginsenoside extract solution, heating the ginsenoside extract solution to 3-5 ℃, adding an enzyme preparation for enzymolysis, and fully stirring to obtain a ginsenoside enzymolysis liquid, wherein the enzyme preparation is one or a combination of more of lipase, pig liver carboxylesterase and phospholipase, the adding amount of the enzyme preparation is 0.2-5% of the weight of a raw product of ginsenoside extraction, and the enzymolysis time is 2-5 hours;
s300) obtaining ginsenoside enzymolysis liquid, and carrying out first membrane separation treatment on the ginsenoside enzymolysis liquid to obtain ginsenoside extract clarified liquid, wherein in the embodiment, the ceramic membrane pore diameter is 5-30 nm;
s400) obtaining a ginsenoside extract clarified liquid, performing adsorption treatment on the ginsenoside extract clarified liquid by using an adsorption column containing an anion resin filler, and collecting a lower column liquid of the adsorption column to obtain a ginsenoside lower column liquid, wherein the anion resin filler is one of D31, D941 and LX-T5;
s500) obtaining ginsenoside lower column liquid, carrying out vacuum low-temperature concentration treatment on the ginsenoside lower column liquid, and then carrying out spray drying to obtain the ginsenoside extract with the phthalate plasticizer being less than 5ppb, wherein in the embodiment, the vacuum low-temperature concentration temperature is 5-70 ℃, and the vacuum degree is-0.06 mpa-0.09 mpa.
Referring to fig. 6, 7, 8, 9, 10 and 11, the filter element comprises an outer cylinder 1, a ceramic membrane filter element 2, a first end cap 3 and a second end cap 4, the outer cylinder 1 has a direction extending along an axial direction, a plurality of rings of through hole layers are arranged on the outer wall of the outer cylinder 1, each through hole layer comprises a plurality of first through holes 1a, the first through holes 1a of the same through hole layer are circumferentially distributed on the outer wall of the outer cylinder 1, the ceramic membrane filter element 2 is arranged in the outer cylinder 1, the ceramic membrane filter element 2 comprises a plurality of hollow membrane wires arranged in a linear type, the end parts of the hollow membrane wires are sealed at one end of the ceramic membrane filter element 2, the other end of the ceramic membrane filter element 2 is sealed between adjacent hollow membrane wires, one end of the outer cylinder 1 is detachably connected with the first end cap 3, the first end cap 3 is connected with one end of the outer cylinder 1 close to the ceramic membrane filter element 2 in a sealing manner, the other end of, the second end cover 4 is connected with the other end of the outer cylinder body 1 close to the ceramic membrane filter element 2 in a sealing way.
In this embodiment, the via layer of each layer all is equipped with a plurality of first through-holes 1a, and the interval between the adjacent via layer equals, the outer barrel 1's of being convenient for intake and drainage. The ceramic membrane filter element 2 can be installed in the outer cylinder body 1 in an adhesive packaging mode, the packaging is reliable, and the sealing performance is good.
The hollow membrane silk has the filtration pore for hollow fiber membrane separation membrane silk, has set up the filtration pore and be used for promoting the filter effect on hollow membrane silk, and what hollow membrane silk wholly adopted is that the physics screening filters the principle, and all can both be held back by hollow membrane silk, and then can thoroughly get rid of biological nature safety factor, guarantee the filter effect. The end parts of the hollow membrane filaments are sealed by gluing, and the adjacent hollow membrane filaments are sealed by gluing, so that the packaging is convenient and the sealing performance is good.
The water outlet 3a is arranged on the first end cover 3, the water outlet 4a is arranged on the second end cover 4, the water outlet nozzle 4b is further arranged on the second end cover 4, one end of the water outlet nozzle 4b is used for being connected with the outside, the other end of the water outlet nozzle 4b is connected with the water outlet 4a, at least one sealing ring groove 4c is arranged on the water outlet nozzle 4b, the sealing ring groove 4c is used for installing a sealing ring for sealing, and through the arrangement of the sealing ring groove 4c and the sealing ring, when the second end cover 4 is connected with the outside, the sealing performance during installation can be improved.
When the membrane separation treatment is carried out, liquid to be treated enters from one side of the first end cover 3, enters the hollow membrane filaments from the outside of the hollow membrane filaments through the first through holes 1a in the outer cylinder body 1, flows out from the middle of the hollow membrane filaments at the other end of the ceramic membrane filter element 2 after being filtered by the hollow membrane filaments, and then flows out through the water outlet 4a in the second end cover 4. When backwashing or cleaning is carried out, cleaning water is introduced into the water outlet 4a, the cleaning water flows into the middle of the hollow membrane filaments at the other end of the ceramic membrane filter element 2 for washing, and the washed sewage flows to the water outlet 3a through one end of the ceramic membrane filter element 2 and is discharged or is discharged through the first through hole 1 a. This filter core is through the cavity membrane silk that adopts the linear type setting to carry out the encapsulation of different forms respectively sealed to cavity membrane silk both ends, can make the liquid of pending all be the middle outflow of the cavity membrane silk from ceramic membrane filter core 2's the other end through the water after the membrane separation handles, effectively ensure the safety of filtering the back water, and easily later stage backwash and washing, repeated repetitious usage, long service life reduces the maintenance cost.
The ceramic membrane filter element 2 is of a hollow structure, one end of the outer cylinder body 1, which is close to the other end of the ceramic membrane filter element 2, is provided with a plugging piece 5, and the plugging piece 5 is arranged in a hollow cavity at the other end of the ceramic membrane filter element 2; first end cover 3 includes first lid 3d and the fixed barrel 3e that matches with the cavity of ceramic membrane filter core 2, is provided with outlet 3a on the first lid 3d, and fixed barrel 3e is hollow structure, and the one end of fixed barrel 3e docks with outlet 3a, and the other end of fixed barrel 3e stretches into in the cavity of ceramic membrane filter core 2 one end. By adopting the structure, the ceramic membrane filter element 2 with the hollow structure has large filling area, can increase the filtering area and has large water yield during filtering. The fixing cylinder 3e can extend into the hollow cavity at one end of the ceramic membrane filter element 2, so that one end of the ceramic membrane filter element 2 is fixed in the circumferential direction, the hollow membrane filaments at one end of the ceramic membrane filter element 2 are prevented from being loose under the impact of raw water, and the raw water can be ensured to reliably enter the hollow membrane filaments; the plugging piece 5 can plug the hollow cavity at the other end of the ceramic membrane filter element 2, so that liquid after membrane separation can flow out from the middle of the hollow membrane wire at the other end of the ceramic membrane filter element 2, and the safety of a filtered water body is ensured; the fixed cylinder 3e is in butt joint with the water outlet 3a, and sewage after flushing can flow into the fixed cylinder 3e through the hollow cavity of the ceramic membrane filter element 2 during flushing and then is discharged through the water outlet 3 a.
The plugging piece 5 is a plugging cover body structure matched with the hollow cavity of the ceramic membrane filter element 2, and the side wall of the plugging piece 5 is connected with the cavity wall of the hollow cavity of the ceramic membrane filter element 2 in a sealing mode. Specifically, the side wall of the plugging piece 5 can be connected with the wall of the ceramic membrane filter element 2 through adhesion, the sealing performance is good, and the packaging is reliable. By adopting the structure, the plugging piece 5 can reliably plug the hollow cavity at the other end of the ceramic membrane filter element 2, and ensures that liquid after membrane separation flows out from the middle of the hollow membrane wire at the other end of the ceramic membrane filter element 2, thereby effectively ensuring the safety of the filtered water body. Still be equipped with a plurality of division boards 6 on the filter core, division board 6 is along circumference evenly distributed with the axis of barrel 1 outside as the center, and the one end and the outer barrel 1 of division board 6 are connected, and the other end and the shutoff piece 5 of division board 6 are connected. Through setting up two at least division boards 6, division board 6 can carry out the subregion to the cavity membrane silk, improves the homogeneity that the membrane silk distributes, and then improves the homogeneity that filters back water and go out water. Because the axis of the outer cylinder body 1 of the partition plate 6 is uniformly distributed along the circumferential direction as the center, the partitioning effect is good, and meanwhile, the outer cylinder body 1, the plugging piece 5 and the partition plate 6 are of an integrally formed structure, so that the forming and the manufacturing are convenient.
A plurality of reinforcing ribs 3b are arranged on the outer wall of the first end cover 3, and a diversion trench 3c is formed between the adjacent reinforcing ribs 3 b. The setting of guiding gutter 3c for when the sewage after washing the filter core was discharged through first through-hole 1a, accessible guiding gutter 3c was carried out the water conservancy diversion, and then can reduce the filth and remain the dead angle, improves the cleanliness factor of blowdown, easily the blowdown.
In this embodiment, the other end of the fixed cylinder 3e is provided with a notch 3e1 along the axial direction, the opening of the notch 3e1 at the end close to the other end of the fixed cylinder 3e is large, and the opening of the notch 3e1 at the end far from the other end of the fixed cylinder 3e is small. Through set up breach 3e1 on fixed barrel 3e, the installation of the fixed barrel 3e of being convenient for, through fine setting breach 3e1 size, the adaptable ceramic membrane filter core 2 that has the cavity of equidimension not of fixed barrel 3e, and then reduce the assembly precision of fixed barrel 3e, the assembly of being convenient for. In this embodiment, there are two notches 3e1, two notches 3e1 are symmetrically disposed on the fixing cylinder 3e, and the notch 3e1 extends to one end of the fixing cylinder 3 e. By adopting the structure, when the flushed sewage flows out through the hollow cavity of the ceramic membrane filter element 2, the sewage can flow to the water outlet 3a from the notch 3e1, so that the dead angle of sewage discharge can be further reduced, the residue is reduced, and the cleanness of the sewage discharge is improved.
Because ceramic membrane filter core 2 adopts the straight range encapsulation of the cavity membrane silk of high density, can make during the reliable follow outside entering cavity membrane silk of raw water, guarantee that the water after the filtration all is the middle outflow from the cavity membrane silk of the other end of ceramic membrane filter core 2, effectively ensure the safety of the water after the filtration, and easily wash, long service life, can repeat repetitious usage, can reduce cost, environmental protection more, through adopting hollow structure's ceramic membrane filter core 2, easily installation, the wholeness of being convenient for filters the security inspection, the filling area is big, it is big to filter the water yield, it is easy to clean, high safety.
Referring to fig. 3, 4 and 5, one end of the water outlet nozzle 4b away from the second end cap 4 extends to the outside of the column type membrane separation filter, and a portion of the water outlet nozzle 4b exposed out of the column type membrane separation filter is sleeved with a collar 7, a first rack 8 is arranged on the collar 7, and a lifting mechanism 9 is arranged on a side portion of the first rack 8.
The lifting mechanism 9 comprises a fixed seat 9a, a driving motor 9b, a first gear 9c, a second gear 9d, a first connecting rod 9e, a second connecting rod 9f, a third connecting rod 9g, a sliding rod 9h, a mounting sleeve 9i, a fourth connecting rod 9j, a fixed plate 9k and a second rack 9m, wherein:
a fixed seat 9a is fixed on the side part of the first rack 8, one end of the fixed seat 9a is provided with a driving motor 9b, an output shaft of the driving motor 9b is connected with a first gear 9c in a transmission way, the first gear 9c is rotationally connected with the fixed seat 9a, the side part of the first gear 9c is provided with a second gear 9d, the second gear 9d is rotationally connected with the fixed seat 9a and is meshed with the first gear 9c, a first connecting rod 9e is eccentrically arranged on the first gear 9c, a second connecting rod 9f is eccentrically arranged on the second gear 9d, one end of the first connecting rod 9e is connected with the first gear 9c, one end of the second connecting rod 9f is connected with the second gear 9d, the other end of the first connecting rod 9e is hinged with the other end of the second connecting rod 9f, a third connecting rod 9g is hinged at the hinged point of the first connecting rod 9e and the second connecting rod 9f, and the other end of the third connecting rod 9, the sliding rod 9h is connected with a sliding seat 9a1 arranged on the fixed seat 9a in a sliding manner, the other end of the sliding rod 9g is sleeved with two mounting sleeves 9i, each mounting sleeve 9i is provided with a fourth connecting rod 9j, the two fourth connecting rods 9j are arranged in parallel, one of the fourth connecting rods 9j is provided with a driving part, the driving part is used for driving the fourth connecting rod 9j to rotate, and the driving part can also be an electric motor. One end of the fourth connecting rod 9j is connected with the mounting sleeve 9i, the other end of the fourth connecting rod 9j is connected with a fixing plate 9k, and a second rack 9m meshed with the first rack 8 is arranged on the fixing plate 9 k.
When the driving motor 9b works, the first gear 9c is driven to rotate, when the first gear 9c rotates, the second gear 9d is driven to rotate together, and simultaneously, when the second gear 9d rotates, the first connecting rod 9e and the second connecting rod 9f synchronously rotate along with the first gear 9c and the second gear 9d, respectively, under the action of the first connecting rod 9e and the second connecting rod 9f, the third connecting rod 9g and the sliding rod 9h are pulled to perform axial movement along the axis of the sliding rod 9h, so that the mounting sleeve 9i, the fourth connecting rod 9j, the fixing plate 9k and the second rack 9m mounted on the sliding rod 9g approach the first rack 8, at the moment, the driving piece starts to work again, the fourth connecting rod 9j, the fixing plate 9k and the second rack 9m are driven to perform planar movement, the second rack 9m is meshed with the first rack 8, when the second rack 9m performs planar movement, the filter element is taken out integrally, so that the filter element is convenient to replace.
The equipment realizes the functions of the invention through the following steps, thereby solving the technical problems provided by the invention:
step one, after the ginsenoside enzymolysis liquid is prepared, introducing the ginsenoside enzymolysis liquid into a membrane separation system, and carrying out first membrane separation treatment on the ginsenoside enzymolysis liquid;
step two, liquid to be treated enters from one side of the first end cover 3, enters the hollow membrane filaments from the outside of the hollow membrane filaments through the first through holes 1a on the outer cylinder 1, flows out from the middle of the hollow membrane filaments at the other end of the ceramic membrane filter element 2 after being filtered by the hollow membrane filaments, and then flows out through the water outlet 4a on the second end cover 4;
step three, when backwashing or cleaning is needed, cleaning water is introduced into the water outlet 4a, the cleaning water flows into the hollow membrane filaments at the other end of the ceramic membrane filter element 2 for cleaning, and the cleaned sewage flows to the water outlet 3a through one end of the ceramic membrane filter element 2 and is discharged or is discharged through the first through hole 1 a;
and step four, when the filter element needs to be replaced, the driving motor 9b is started, when the driving motor 9b works, the first connecting rod 9e and the second connecting rod 9f can synchronously rotate along with the first gear 9c and the second gear 9d respectively, under the action of the first connecting rod 9e and the second connecting rod 9f, the third connecting rod 9g and the sliding rod 9h can be pulled to carry out axial movement along the axis of the sliding rod 9h, at the moment, the driving piece starts to work again, the fourth connecting rod 9j, the fixing plate 9k and the second rack 9m are driven to carry out plane movement, the second rack 9m is meshed with the first rack 8, when the second rack 9m carries out plane movement, the filter element is integrally taken out, and the filter element is convenient to replace.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (10)

1. A method for removing a plasticizer from a ginsenoside extract is characterized by comprising the following steps:
preparing a ginsenoside extract solution;
obtaining the ginsenoside extract solution, heating the ginsenoside extract solution to a certain temperature, adding an enzyme preparation for enzymolysis, and fully stirring to obtain a ginsenoside enzymolysis solution;
obtaining the ginsenoside enzymolysis liquid, and carrying out first membrane separation treatment on the ginsenoside enzymolysis liquid to obtain a ginsenoside extract clarified liquid;
obtaining the ginsenoside extract clear solution, and performing adsorption treatment on the ginsenoside extract clear solution to obtain ginsenoside lower column solution;
and (3) obtaining the ginsenoside lower column liquid, carrying out vacuum low-temperature concentration treatment on the ginsenoside lower column liquid, and then carrying out spray drying to obtain the ginsenoside extract with the phthalate plasticizer being less than 50 ppb.
2. The method for removing the plasticizer from the ginsenoside extract according to claim 1, wherein the preparation of the ginsenoside extract solution specifically comprises:
obtaining untreated ginsenoside extraction raw products, wherein the ginsenoside extraction raw products are a ginseng root extract, an American ginseng extract, a ginseng stem and leaf extract and a panax notoginseng extract containing ginsenoside, and the content of the ginsenoside is 3-30%;
adding purified water 5-15 times the weight of the ginsenoside extraction raw product, and dissolving the ginsenoside extraction raw product to obtain ginsenoside extract solution;
obtaining the ginsenoside extract solution, and adjusting the pH of the ginsenoside extract solution to obtain the ginsenoside extract solution, wherein the pH is adjusted by using one or a mixture of citric acid and sodium citrate as buffer salt.
3. The method for removing the plasticizer from the ginsenoside extract according to claim 2, wherein the ginsenoside extract solution is obtained, the ginsenoside extract solution is heated to a certain temperature, an enzyme preparation is added for enzymolysis, the mixture is fully stirred, the ginsenoside extract solution in the ginsenoside enzymolysis solution is heated to 30-50 ℃, the enzyme preparation is one or a combination of lipase, pig liver carboxylesterase and phospholipase, the adding amount of the enzyme preparation is 0.2-5% of the weight of the raw ginsenoside extract product, and the enzymolysis time is 2-5 hours.
4. The method for removing the plasticizer from the ginsenoside extract of claim 3, wherein the first membrane separation treatment is performed by using a ceramic membrane with a pore diameter of 50-300 nm.
5. The method for removing the plasticizer from the ginsenoside extract according to claim 4, wherein the ginsenoside extract clarified liquid is obtained and is subjected to adsorption treatment to obtain a ginsenoside lower column liquid, the ginsenoside lower column liquid is subjected to adsorption treatment by using an adsorption column containing an anionic resin filler, and the lower column liquid of the adsorption column is collected to obtain the ginsenoside lower column liquid, wherein the anionic resin filler is one of D301, D941 and LX-T5.
6. The method for removing the plasticizer from the ginsenoside extract of claim 5, wherein the vacuum low-temperature concentration temperature is 50-70 ℃ and the vacuum degree is-0.06 mpa to-0.09 mpa.
7. The utility model provides a desorption equipment of plasticizing agent in ginsenoside extract product, including the membrane separation system, a serial communication port, the membrane separation system includes column type membrane separation filter, be equipped with the filter core in the membrane separation filter, the filter core includes outer barrel (1), ceramic membrane filter core (2), first end cover (3) and second end cover (4), outer barrel (1) has the direction along the axial extension, seted up a plurality of rings of through-hole layer on the outer wall of outer barrel (1), the through-hole layer includes a plurality of first through-holes (1a), the first through-hole (1a) circumference of same through-hole layer distributes on the outer wall of outer barrel (1), ceramic membrane filter core (2) are installed in outer barrel (1), ceramic membrane filter core (2) include a plurality of hollow membrane silks that are the linear type setting, at one of them one end of ceramic membrane filter core (2), the tip of hollow membrane silk is sealed, at the other end of ceramic membrane filter core, the adjacent hollow membrane wires are sealed, one end of the outer cylinder body (1) is detachably connected with the first end cover (3), and the other end of the outer cylinder body (1) is detachably connected with the second end cover (4).
8. The equipment for removing the plasticizer from the ginsenoside extract according to claim 7, wherein a water outlet (3a) is formed in the first end cover (3), a water outlet (4a) is formed in the second end cover (4), a water outlet nozzle (4b) is further formed in the second end cover (4), one end of the water outlet nozzle (4b) is used for being connected with the outside, the other end of the water outlet nozzle (4b) is connected with the water outlet (4a), at least one sealing ring groove (4c) is formed in the water outlet nozzle (4b), the sealing ring groove (4c) is used for installing a sealing ring for sealing, the ceramic membrane filter element (2) is of a hollow structure, a plugging piece (5) is arranged at one end, close to the ceramic membrane filter element (2), of the outer cylinder body (1), the plugging piece (5) is installed in a hollow cavity at one end of the ceramic membrane filter element (2), and a plurality of partition plates (6), the partition plates (6) are uniformly distributed along the circumferential direction by taking the axis of the outer cylinder body (1) as the center, one ends of the partition plates (6) are connected with the outer cylinder body (1), and the other ends of the partition plates (6) are connected with the plugging piece (5).
9. The equipment for removing the plasticizer from the ginsenoside extract of claim 8, wherein the first end cover (3) comprises a first cover body (3d) and a fixed cylinder body (3e) matched with the hollow cavity of the ceramic membrane filter element (2), a water outlet (3a) is arranged on the first cover body (3d), the fixed cylinder body (3e) is of a hollow structure, one end of the fixed cylinder body (3e) is butted with the water outlet (3a), the other end of the fixed cylinder body (3e) extends into the hollow cavity of one end of the ceramic membrane filter element (2), a notch (3e1) is arranged at the end part of the other end of the fixed cylinder body (3e) along the axial direction, one end of the notch (3e1) close to the end part of the fixed cylinder body (3e) is opened to a large extent, one end of the notch (3e1) far away from the end part of the fixed cylinder body (3e) is opened to a small extent, a plurality of reinforcing ribs (3b) are arranged on the outer wall of the, a diversion trench (3c) is formed between the adjacent reinforcing ribs (3 b).
10. The equipment for removing the plasticizer from the ginsenoside extract of claim 9, wherein one end of the water outlet nozzle (4b) far away from the second end cover (4) extends to the outside of the column type membrane separation filter, a sleeve ring (7) is sleeved on the part of the water outlet nozzle (4b) exposed out of the column type membrane separation filter, a first rack (8) is arranged on the sleeve ring (7), and a lifting mechanism (9) is arranged on the side part of the first rack (8);
lifting mechanism (9) includes fixing base (9a), driving motor (9b), first gear (9c), second gear (9d), first connecting rod (9e), second connecting rod (9f), third connecting rod (9g), slide bar (9h), installation cover (9i), fourth connecting rod (9j), fixed plate (9k) and second rack (9m), wherein:
a fixed seat (9a) is fixed on the side of the first rack (8), a driving motor (9b) is arranged at one end of the fixed seat (9a), an output shaft of the driving motor (9b) is in transmission connection with a first gear (9c), the first gear (9c) is in rotary connection with the fixed seat (9a), a second gear (9d) is arranged on the side of the first gear (9c), the second gear (9d) is in rotary connection with the fixed seat (9a) and is meshed with the first gear (9c), a first connecting rod (9e) is eccentrically arranged on the first gear (9c), a second connecting rod (9f) is eccentrically arranged on the second gear (9d), one end of the first connecting rod (9e) is connected with the first gear (9c), one end of the second connecting rod (9f) is connected with the second gear (9d), and the other end of the first connecting rod (9e) is hinged with the other end of the second connecting rod (9 f);
a third connecting rod (9g) is hinged at the hinged point of the first connecting rod (9e) and the second connecting rod (9f), a sliding rod (9h) is arranged at the other end of the third connecting rod (9g), the sliding rod (9h) is in sliding connection with a sliding seat (9a1) arranged on a fixed seat (9a), two mounting sleeves (9i) are sleeved at the other end of the sliding rod (9g), a fourth connecting rod (9j) is arranged on each mounting sleeve (9i), and the two fourth connecting rods (9j) are arranged in parallel, a driving piece is arranged on one fourth connecting rod (9j), the driving piece is used for driving the fourth connecting rod (9j) to rotate, one end of the fourth connecting rod (9j) is connected with the mounting sleeve (9i), the other end of the fourth connecting rod (9j) is connected with a fixing plate (9k), and a second rack (9m) meshed with the first rack (8) is arranged on the fixing plate (9 k).
CN202010823501.5A 2020-08-17 2020-08-17 Method and equipment for removing plasticizer from ginsenoside extract Pending CN112125947A (en)

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Application publication date: 20201225