CN112028961A - Method and equipment for removing carbendazim in ginsenoside extract - Google Patents
Method and equipment for removing carbendazim in ginsenoside extract Download PDFInfo
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- CN112028961A CN112028961A CN202010823595.6A CN202010823595A CN112028961A CN 112028961 A CN112028961 A CN 112028961A CN 202010823595 A CN202010823595 A CN 202010823595A CN 112028961 A CN112028961 A CN 112028961A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J17/00—Normal steroids containing carbon, hydrogen, halogen or oxygen, having an oxygen-containing hetero ring not condensed with the cyclopenta(a)hydrophenanthrene skeleton
- C07J17/005—Glycosides
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- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/25—Araliaceae (Ginseng family), e.g. ivy, aralia, schefflera or tetrapanax
- A61K36/258—Panax (ginseng)
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D2311/00—Details relating to membrane separation process operations and control
- B01D2311/26—Further operations combined with membrane separation processes
- B01D2311/263—Chemical reaction
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- B01D2311/26—Further operations combined with membrane separation processes
- B01D2311/2649—Filtration
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Abstract
The invention relates to the technical field of ginsenoside extract extraction, in particular to a method and equipment for removing carbendazim in a ginsenoside extract, which comprises the steps of preparing a ginsenoside extract solution; obtaining a ginsenoside extract solution, and adjusting the pH value of the ginsenoside extract solution; obtaining the ginsenoside extract solution after the pH is adjusted, and carrying out primary membrane separation treatment on the ginsenoside extract solution after the pH is adjusted to obtain a ginsenoside extract filtrate; obtaining a ginsenoside extract filtrate, and performing a second membrane separation treatment on the ginsenoside extract filtrate to obtain a ginsenoside extract retentate; the method comprises the steps of obtaining a ginsenoside extract trapped fluid, concentrating the ginsenoside extract trapped fluid, and drying to obtain the ginsenoside extract.
Description
Technical Field
The invention relates to the technical field of ginsenoside extract extraction, in particular to a method and equipment for removing carbendazim in 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 CN201410503585.9 discloses a method for extracting ginsenoside, comprising 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%.
Carbendazim is a broad-spectrum bactericide, has control effect on diseases of crops caused by fungi, has wide application range in China, but can cause liver diseases and chromosome distortion of human bodies and be toxic to mammals due to residues. Ginseng generally needs to be planted for more than 3 years before being harvested, and a large amount of pesticide is applied to prevent and treat various plant diseases and insect pests in the period. The carbendazim has stable chemical property, remains in the using part of ginseng and is difficult to wash, and the residual quantity in the ginsenoside extract prepared by the method and the traditional extraction process can reach more than 1ppm to 10 ppm. The methods for removing carbendazim or pesticide residues reported at present mainly comprise an organic solvent extraction method, a resin adsorption method and the like, the methods are high in production cost and complicated to operate, a certain amount of organic solvent is introduced while pesticide residues are removed, and the industrial application is limited to a certain extent.
Disclosure of Invention
In order to solve the technical problems, the technical scheme solves the problems that the existing method for removing pesticide residues is complex to operate, a certain amount of organic solvent is introduced while the pesticide residues are removed, and the industrial application is limited to a certain extent.
In order to achieve the above purposes, the technical scheme adopted by the invention is as follows:
the method for removing carbendazim in the ginsenoside extract comprises the following steps:
preparing a ginsenoside extract solution;
obtaining the ginsenoside extract solution, and adjusting the pH value of the ginsenoside extract solution;
obtaining the ginsenoside extract solution after the pH is adjusted, and carrying out primary membrane separation treatment on the ginsenoside extract solution after the pH is adjusted to obtain a ginsenoside extract filtrate;
obtaining the ginsenoside extract filtrate, and performing secondary membrane separation treatment on the ginsenoside extract filtrate to obtain ginsenoside extract retentate;
and (3) obtaining the ginsenoside extract trapped fluid, concentrating the ginsenoside extract trapped fluid, and drying to obtain the ginsenoside extract with carbendazim less than 10 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 20-30 times the weight of the ginsenoside extraction raw product, and dissolving the ginsenoside extraction raw product to obtain ginsenoside extract solution.
Optionally, the ginsenoside extract solution is obtained, and one of hydrochloric acid and acetic acid is used for adjusting the pH value of the ginsenoside extract solution, so as to adjust the pH value of the ginsenoside extract solution to 2-5.
Optionally, the first membrane separation treatment is performed by using a ceramic membrane for clarification treatment, wherein the pore diameter of the ceramic membrane is 100-800nm, and the pressure of the ceramic membrane clarification treatment is 0.05-0.1 mpa.
Optionally, the ginsenoside extract filtrate is obtained, and a second membrane separation treatment is performed on the ginsenoside extract filtrate to obtain a ginsenoside extract retentate, which specifically comprises:
obtaining the ginsenoside extract filtrate, and performing circulating ultrafiltration treatment by using an ultrafiltration membrane, wherein the molecular weight of the ultrafiltration membrane is 1000-10000 Dalton, the permeation pressure is 0.05-0.2mpa, and the circulating ultrafiltration time is 3-6 hours.
Optionally, the ginsenoside extract retentate is obtained, concentrated and dried, and the obtained ginsenoside extract with carbendazim less than 10ppb is dried by one of spray drying and freeze drying.
Further, the equipment for removing carbendazim in the ginsenoside extract comprises an ultrafiltration system, wherein the ultrafiltration system comprises ultrafiltration equipment, a water inlet pipeline, a water production pipeline, a concentrated water pipeline and a filter element replacement mechanism, the ultrafiltration equipment is a column type ultrafiltration membrane filter, the ultrafiltration equipment is set to be at least one, the bottom and the top of the ultrafiltration equipment are provided with the water inlet pipeline and the water production pipeline, the water inlet pipeline is provided with water inlet branch pipes with the same number as the ultrafiltration equipment, the water inlet branch pipes are in one-to-one correspondence with the ultrafiltration equipment and are communicated with the corresponding interior of the ultrafiltration equipment, the water production pipeline is provided with water production branch pipes with the same number as the ultrafiltration equipment, the water production branch pipes are in one-to-one correspondence with the ultrafiltration equipment and are communicated with the corresponding interior of the ultrafiltration equipment, the top of the ultrafiltration equipment is also provided with the concentrated water pipeline, the concentrated water branch pipes with the same number as the ultrafiltration, and communicate with the inside that corresponds ultrafiltration apparatus, every inside all can be dismantled and be connected with an ultrafiltration membrane group of ultrafiltration apparatus, can dismantle on the ultrafiltration membrane group and be connected with at least one filter core that is vertical state, all be equipped with filter core replacement mechanism on every dense water branch pipe, filter core replacement mechanism is used for controlling opening and closure that corresponds the ultrafiltration apparatus top, under filter core replacement mechanism open state, ultrafiltration membrane group and filter core can follow the separation of ultrafiltration apparatus, under filter core replacement mechanism locking state, ultrafiltration membrane group and filter core are located inside the ultrafiltration apparatus.
Optionally, the filter element replacing mechanism comprises a rotary table, positioning sleeves, a plunger, a movable push plate, an electric push rod, a movable part and a fixing part, wherein the top end of each ultrafiltration device is rotatably connected with the rotary table, the side part of the rotary table is provided with a driving component for driving the rotary table to rotate along the central shaft of the ultrafiltration device, the rotary table comprises a disc body, an outer convex surface and an inner concave surface, the disc body is arranged in an annular shape, the top end of the disc body is alternately provided with a plurality of outer convex surfaces and a plurality of inner concave surfaces, the disc body, the outer convex surfaces and the inner concave surfaces are integrally formed, the top part of the rotary table is provided with at least one positioning sleeve, the positioning sleeves are distributed along the circumference of the central shaft of the ultrafiltration device, the positioning sleeves are arranged in a radial extension manner along the ultrafiltration device, one end parts of the positioning sleeves, which are far away from, the output end of the electric push rod is correspondingly connected with a movable push plate, the end part of one end of the positioning sleeve, which is close to the circle center of the ultrafiltration equipment, is provided with a movable part, each concentrated water branch pipe is sleeved with a fixing part, and the movable part is in sliding connection with the fixing part.
Optionally, the movable part comprises a connecting ring, a vertical rod, teeth, an arc rod and a guide slip, top cap and reset spring, the mounting includes the lantern ring, a fixed base, opening and gear, it is equipped with a lantern ring all to overlap on every dense water branch pipe, the peripheral circumference of the lantern ring distributes and has the fixing base that equals with positioning sleeve quantity, the opening has been seted up on the fixing base, the opening internal rotation is connected with the gear, the go-between cover is established and is close to the one end tip in the ultrafiltration apparatus centre of a circle at positioning sleeve, the go-between top is equipped with the montant that is vertical state, one of them terminal surface of montant is equipped with the tooth with gear engagement, another terminal surface of montant is equipped with the arc pole, be equipped with the direction cutting of protrusion in the montant on the montant, the arc pole, the direction cutting all with opening sliding connection, the top of montant is equipped.
Optionally, a plurality of interlayers are arranged in the ultrafiltration device, the interlayers are arranged close to the top end of the ultrafiltration device, each interlayer comprises three positioning clamping plates, the positioning clamping plates are arranged in a fan-shaped ring shape, the central angle of each positioning clamping plate is 60 degrees, the positioning clamping plates on the same interlayer are distributed along the circumference of the central shaft of the ultrafiltration device, the ultrafiltration membrane group comprises a first rod body, an inserting plate, a second rod body, a clapboard, a limiting plate, a rotating shaft and a butt plate, a plurality of layers of inserting layers are arranged on the first rod body, the inserting layers are arranged close to the top end of the first rod body, each layer of inserting plates comprises three inserting plates, the inserting plates are arranged in a fan-shaped ring shape, the central angle of each inserting plate is 60 degrees, the positioning clamping plates on the same inserting layer are distributed along the circumference of the central shaft of the inserting plate, the inserting plates are inserted between the two positioning clamping, the central angle of baffle is 60 and the baffle is located the picture peg under, can dismantle in the baffle and be connected with the filter core, on the baffle with the limiting plate of filter core butt, the bottom of the second body of rod is rotated and is connected with the pivot, the circumference distributes in the pivot has three butt plate, the butt plate sets up to fan ring shape, the central angle of butt plate is 60, the first body of rod, the second body of rod and pivot all with the coaxial setting of ultrafiltration apparatus and the first body of rod, the outer wall of the second body of rod and pivot all is equipped with certain clearance with the ultrafiltration apparatus inner wall.
Compared with the prior art, the invention has the beneficial effects that:
the method has the advantages that under the acidic condition, the water solubility of the carbendazim is greatly improved after the carbendazim is in a salt state, so that the carbendazim can more easily permeate the ultrafiltration membrane, and due to the three-dimensional property of the molecular structure, the effective components such as ginsenoside and the like cannot easily permeate the ultrafiltration membrane, so that the aim of separating the carbendazim and the ginsenoside is fulfilled, and the method is simple and convenient, stable in industrial application and low in operation cost.
Drawings
FIG. 1 is a schematic flow diagram of the process of the present invention;
FIG. 2 is a schematic flow chart of the method of the present invention, S100);
FIG. 3 is a schematic diagram of the structure of the apparatus of the present invention;
FIG. 4 is a schematic view of a filter cartridge changing mechanism of the apparatus of the present invention;
FIG. 5 is an enlarged schematic view at A in FIG. 4;
FIG. 6 is a schematic view of the filter cartridge changing mechanism of the apparatus of the present invention in another state;
FIG. 7 is a front elevational view of a cartridge changing mechanism of the apparatus of the present invention;
FIG. 8 is a schematic cross-sectional view taken along line B-B of FIG. 7;
FIG. 9 is a front view of the apparatus of the present invention at the ultrafiltration unit;
FIG. 10 is a schematic cross-sectional view taken along line A-A of FIG. 9;
FIG. 11 is a perspective cross-sectional view taken at A-A of FIG. 9;
FIG. 12 is a schematic diagram of an explosion at the ultrafiltration unit in the apparatus of the present invention;
FIG. 13 is a schematic view of the structure of the apparatus of the present invention in a state where a filter element is installed at the ultrafiltration membrane module;
FIG. 14 is a schematic structural view of the apparatus of the present invention in a state where no filter cartridge is installed in the ultrafiltration membrane module.
Description of reference numerals:
1-ultrafiltration equipment; 1 a-positioning splint;
2-a water inlet pipeline;
3-a water production pipeline;
4-a concentrated water pipeline; 4 a-a concentrated water branch pipe;
5-a filter element replacement mechanism; 5 a-a turntable; 5a 1-tray; 5a 2-outer convex surface; 5a 3-concave inner surface; 5 b-a positioning sleeve; 5b 1-locating holes; 5 c-a plunger; 5 d-movable push plate; 5 e-an electric push rod; 5 f-moving part; 5f 1-connecting ring; 5f 2-vertical bar; 5f 3-teeth; 5f 4-arc bar; 5f 5-guide slips; 5f 6-Top cover; 5f 7-return spring; 5 g-a fixing piece; 5g 1-Loop; 5g 2-fixed seat; 5g 3-open; 5g 4-gear;
6-ultrafiltration membrane group; 6 a-a first rod; 6 b-inserting plate; 6 c-a second rod; 6 d-a separator; 6 e-a limiting plate; 6 f-a rotating shaft; 6 g-abutting plates;
7-a filter element;
8-sealing the cover; 8 a-a seal ring; 8 b-locking block.
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:
s101) 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%;
s102) adding purified water with the weight 20-30 times of that of the original product of ginsenoside extraction, and dissolving the original product of ginsenoside extraction to obtain a ginsenoside extract solution;
s200) obtaining a ginsenoside extract solution, adjusting the pH value of the ginsenoside extract solution, in the embodiment, using one acid solution of hydrochloric acid and acetic acid for adjustment, and adjusting the pH value of the ginsenoside extract solution to 2-5;
s300) obtaining the ginsenoside extract solution after the pH is adjusted, and performing primary membrane separation treatment on the ginsenoside extract solution after the pH is adjusted to obtain a ginsenoside extract filtrate, wherein in the embodiment, a ceramic membrane is adopted for clarification treatment in the primary membrane separation treatment, the aperture of the ceramic membrane is 100-800 nanometers, and the pressure of the ceramic membrane clarification treatment is 0.05-0.1 mpa;
s400) obtaining a ginsenoside extract filtrate, and performing secondary membrane separation treatment on the ginsenoside extract filtrate to obtain a ginsenoside extract retentate, wherein in the embodiment, an ultrafiltration membrane is used in the secondary membrane separation treatment and is subjected to circulating ultrafiltration treatment through the ultrafiltration membrane, the molecular weight of the ultrafiltration membrane is 1000-10000 Dalton, the permeation pressure is 0.05-0.2mpa, and the circulating ultrafiltration time is 3-6 hours;
s500) obtaining a ginsenoside extract trapped fluid, concentrating the ginsenoside extract trapped fluid, and then drying to obtain a ginsenoside extract with carbendazim less than 10ppb, wherein in the embodiment, the drying mode is one of spray drying and freeze drying, and the recovery rate of the ginsenoside in the whole process is more than 95%.
Referring to fig. 3, the apparatus includes an ultrafiltration system, the ultrafiltration system includes an ultrafiltration apparatus 1, a water inlet pipe 2, a water production pipe 3, a concentrated water pipe 4 and a filter element replacement mechanism 5, the ultrafiltration apparatus 1 is a column-type ultrafiltration membrane filter, the number of the ultrafiltration apparatuses 1 is at least one, the bottom and the top of the ultrafiltration apparatus 1 are provided with the water inlet pipe 2 and the water production pipe 3, the water inlet pipe 2 is provided with water inlet branch pipes equal in number to the ultrafiltration apparatuses 1, the water inlet branch pipes correspond to the ultrafiltration apparatuses 1 one by one and are communicated with the interiors of the corresponding ultrafiltration apparatuses 1, the water production pipe 3 is provided with water production branch pipes equal in number to the ultrafiltration apparatuses 1, the water production branch pipes correspond to the ultrafiltration apparatuses 1 one by one and are communicated with the interiors of the corresponding ultrafiltration apparatuses 1, the top of the ultrafiltration apparatuses 1 is further provided with the concentrated water pipe 4, the concentrated water pipe 4 is provided with concentrated water branch, dense water branch pipe 4a and ultrafiltration apparatus 1 one-to-one, and communicate with the inside that corresponds ultrafiltration apparatus 1, every ultrafiltration apparatus 1 is inside all can to dismantle and be connected with an ultrafiltration membrane group 6, can dismantle on the ultrafiltration membrane group 6 and be connected with at least one filter core 7 that is vertical state, all be equipped with filter core replacement mechanism 5 on every dense water branch pipe 4a, filter core replacement mechanism 5 is used for opening and closing on the control correspondence ultrafiltration apparatus 1 top, under 5 open states of filter core replacement mechanism, ultrafiltration membrane group 6 and filter core 7 can follow ultrafiltration apparatus 1 and separate, under 5 locking states of filter core replacement mechanism, ultrafiltration membrane group 6 and filter core 7 are located ultrafiltration apparatus 1 inside.
Referring to fig. 4, 5, 6, 7 and 8, the filter element replacing mechanism 5 includes a rotary disc 5a, a positioning sleeve 5b, a plunger 5c, a movable push plate 5d, an electric push rod 5e, a movable member 5f and a fixing member 5g, the top end of each ultrafiltration apparatus 1 is rotatably connected with the rotary disc 5a, the side of the rotary disc 5a is provided with a driving component for driving the rotary disc 5a to rotate along the central axis of the ultrafiltration apparatus 1, the rotary disc 5a includes a disc body 5a1, an outer convex surface 5a2 and an inner concave surface 5a3, the disc body 5a1 is annular, the top end of the disc body 5a1 is staggered with a plurality of outer convex surfaces 5a2 and a plurality of inner concave surfaces 5a3, the disc body 5a1, the outer convex surfaces 5a2 and the inner concave surfaces 5a3 are integrally formed, the top of the rotary disc 5a is provided with at least one positioning sleeve 5b, the positioning sleeves 5b are circumferentially distributed along the central axis of the ultrafiltration apparatus 1, the one end tip that the centre of a circle of ultrafiltration apparatus 1 was kept away from to positioning sleeve 5b is equipped with positioning hole 5b1, sliding connection has plunger 5c on positioning hole 5b1, the one end tip that positioning sleeve 5b was kept away from to plunger 5c is equipped with movable push pedal 5d, the lateral part of every positioning sleeve 5b all is equipped with an electric putter 5e, an activity push pedal 5d is connected to electric putter 5 e's output correspondence, the one end tip that positioning sleeve 5b is close to the centre of a circle of ultrafiltration apparatus 1 is equipped with moving part 5f, all the cover is equipped with a mounting 5g on every dense water branch pipe 4a, moving part 5f and mounting 5g sliding connection.
The movable piece 5f comprises a connecting ring 5f1, a vertical rod 5f2, teeth 5f3, an arc rod 5f4, a guide slip 5f5, a top cover 5f6 and a return spring 5f7, the fixed piece 5g comprises a lantern ring 5g1, a fixed seat 5g2, an opening 5g3 and a gear 5g4, each concentrated water branch pipe 4a is sleeved with a lantern ring 5g1, the fixed seats 5g1 with the number equal to that of the positioning sleeves 5b are distributed on the periphery of the lantern ring 5g1, the fixed seat 5g1 is provided with the opening 5g1, the opening 5g1 is rotatably connected with the gear 5g1, the connecting ring 5f1 is sleeved at one end part of the positioning sleeve 5b close to the circle center of the ultrafiltration device 1, the top end of the vertical rod 5f1 is provided with the vertical rod 5f1 in a vertical state, one end face of the vertical rod 5f1 is provided with the teeth 5f1 meshed with the teeth 1 meshed with the vertical rod 1, the vertical rod 1 protruding from the guide slip 1, arc pole 5f4, direction cutting 5f5 all with opening 5g3 sliding connection, the top of montant 5f2 is equipped with top cap 5f6, is equipped with reset spring 5f7 on the top cap 5f6, and the one end and the top cap 5f6 of reset spring 5f7 are connected, and the other end and the fixing base 5g2 of reset spring 5f7 are connected.
The driving assembly is used for driving the rotary disc 5a to rotate along the central shaft of the ultrafiltration device 1, so that the positioning sleeve 5b is in contact with the outer convex surface 5a2 and the inner concave surface 5a3 in a switching manner, the positioning sleeve 5b is lifted or lowered, the positioning sleeve 5b does bumping motion, the electric push rod 5e at the side part of the positioning sleeve 5b is fixedly arranged, when the electric push rod 5e works, the movable push plate 5d and the insert rod 5c are driven to do linear motion, when the insert rod 5c is aligned with the positioning hole 5b1, the insert rod 5c can be inserted into the positioning hole 5b1, the insert rod 5c locks the positioning sleeve 5b, at the moment, the top end of the ultrafiltration device 1 is in a closed state, at the moment, the ultrafiltration membrane group 6 and the filter element 7 in the ultrafiltration device 1 cannot be separated from the ultrafiltration device 1, when the insert rod 5c is not inserted into the positioning hole 5b1, the insert rod 5c loosens the, the top end of the ultrafiltration device 1 is now in an open state, and the ultrafiltration membrane module 6 and the filter element 7 inside the ultrafiltration device 1 can be removed from the ultrafiltration device 1 for replacing the filter element 7 and maintaining the ultrafiltration membrane module 6.
When the positioning sleeve 5b does a bumping motion, the positioning sleeve 5b drives the connecting ring 5f1, the vertical rod 5f2, the teeth 5f3, the arc rod 5f4 and the guide inserting bar 5f5 to do a lifting motion along the opening 5g3, the arc rod 5f4 and the guide inserting bar 5f5 are arranged, and is in sliding fit with the opening 5g3, the guide function of the lifting process of the movable piece 5f is realized, meanwhile, the teeth 5f3 are meshed with the gear 5g4, the gear 5g4 can buffer the lifting process of the moving piece 5f, the moving piece 5f is prevented from being excessively popped up due to stress, the top end of the guide inserting strip 5f5 is provided with the top cover 5f6, the top cover 5f6 is provided with the return spring 5f7, the return spring 5f7 enables the moving piece 5f to be integrally soothing, during the rotation of the turntable 5a, the positioning sleeve 5b is brought into contact with the outer convex surface 5a2 and the inner concave surface 5a3 to raise or lower the positioning sleeve 5 b.
Referring to fig. 9, 10, 11, 12, 13 and 14, a plurality of interlayers are arranged in the ultrafiltration apparatus 1, the interlayers are arranged near the top end of the ultrafiltration apparatus 1, each interlayer comprises three positioning splints 1a, the positioning splints 1a are arranged in a fan-ring shape, the central angle of the positioning splints 1a is 60 degrees, the positioning splints 1a on the same interlayer are distributed along the circumference of the central shaft of the ultrafiltration apparatus 1, the ultrafiltration membrane group 6 comprises a first rod body 6a, an insertion plate 6b, a second rod body 6c, a partition plate 6d, a limiting plate 6e, a rotating shaft 6f and an insertion plate 6g, the first rod body 6a is provided with a plurality of layers of insertion layers, the insertion layers are arranged near the top end of the first rod body 6a, each layer of insertion layer comprises three insertion plates 6b, the insertion plates 6b are arranged in a fan-ring shape, the central angle of the insertion plates 6b is 60 degrees, and the positioning splints 1a on the, the picture peg 6b is pegged graft between two sandwich positioning splint 1a, the bottom of the first body of rod 6a is equipped with the second body of rod 6c, the circumference distributes and has three baffle 6d on the second body of rod 6c, baffle 6d sets up to fan ring shape, baffle 6 d's central angle is 60 and baffle 6d is located picture peg 6b under, can dismantle in the baffle 6d and be connected with filter core 7, limiting plate 6e with filter core 7 butt on the baffle 6d, the bottom of the second body of rod 6c rotates and is connected with pivot 6f, the circumference distributes and has three butt plate 6g on the pivot 6f, butt plate 6g sets up to fan ring shape, the central angle of butt plate 6g is 60, the first rod body 6a, the second rod body 6c and the rotating shaft 6f are all coaxially arranged with the ultrafiltration device 1, and certain gaps are arranged between the outer walls of the first rod body 6a, the second rod body 6c and the rotating shaft 6f and the inner wall of the ultrafiltration device 1.
When installing filter core 7 on ultrafiltration membrane group 6, rotate pivot 6f earlier for three butt joint board 6g on the pivot 6f is in crisscross state with three baffle 6d, can insert filter core 7 to baffle 6d in the top of the second body of rod 6c this moment, and the setting of limiting plate 6e has played the effect of making things convenient for the installation of filter core 7 and restriction mounted position. After the filter element 7 is installed, the rotating shaft 6f is rotated again, so that the three abutting plates 6g on the rotating shaft 6f are respectively positioned right below the three partition plates 6 d. Then, an ultrafiltration membrane group 6 and a filter element 7 are installed in the ultrafiltration device 1, the ultrafiltration membrane group 6 and the filter element 7 are inserted into an opening and closing port at the top end of the ultrafiltration device 1, then the ultrafiltration membrane group 6 is rotated, a plug board 6b arranged on the ultrafiltration membrane group 6 is correspondingly inserted between the two positioning clamp plates 1a, and then a sealing cover 8 can be inserted for sealing. In this embodiment, the closing cap 8 includes seal ring 8a and locking piece 8b, and seal ring 8a sets up to the annular, and the top of seal ring 8a is equipped with three locking piece 8b along the axial extension setting of seal ring 8a, and locking piece 8b sets up to the arc, and locking piece 8b is located between two adjacent location splint 1a in same intermediate layer, inserts locking piece 8b to between two adjacent location splint 1a in same intermediate layer, accomplishes the closure to ultrafiltration apparatus 1.
The equipment realizes the functions of the invention through the following steps, thereby solving the technical problems provided by the invention:
step one, after a ginsenoside extract filtrate is obtained through preparation, introducing the ginsenoside extract filtrate into a water inlet pipeline 2, introducing the ginsenoside extract filtrate into the water inlet pipeline 2, introducing the ginsenoside extract filtrate into each ultrafiltration device 1 along a liquid inlet branch pipe, and performing ultrafiltration treatment on the ginsenoside extract filtrate in each ultrafiltration device 1 to obtain a ginsenoside extract retentate, wherein the ginsenoside extract retentate flows out along a water production branch pipe and a water production pipeline 3;
step two, when the electric push rod 5e works, the movable push plate 5d and the insert rod 5c are driven to do linear motion, when the insert rod 5c is aligned with the positioning hole 5b1, the insert rod 5c can be inserted into the positioning hole 5b1, the insert rod 5c locks the positioning sleeve 5b, at this time, the top end of the ultrafiltration device 1 is in a closed state, at this time, the ultrafiltration membrane group 6 and the filter element 7 inside the ultrafiltration device 1 cannot be separated from the ultrafiltration device 1, when the insert rod 5c is not inserted into the positioning hole 5b1, the insert rod 5c releases the positioning sleeve 5b, at this time, the top end of the ultrafiltration device 1 is in an open state, at this time, the ultrafiltration membrane group 6 and the filter element 7 inside the ultrafiltration device 1 can be detached from the ultrafiltration device 1, and are used for replacing the filter element 7 and maintaining the ultrafiltration membrane group 6;
step three, when installing filter core 7 on ultrafiltration membrane group 6, rotate pivot 6f earlier for three butt joint board 6g on the pivot 6f is in crisscross state with three baffle 6d, can insert filter core 7 to baffle 6d in from the top of the second body of rod 6c this moment, and the setting of limiting plate 6e has played the effect of making things convenient for filter core 7 installation and restriction mounted position. After the filter element 7 is installed, the rotating shaft 6f is rotated again, so that the three abutting plates 6g on the rotating shaft 6f are respectively positioned right below the three partition plates 6 d. Then, an ultrafiltration membrane group 6 and a filter element 7 are installed in the ultrafiltration device 1, the ultrafiltration membrane group 6 and the filter element 7 are inserted into an opening and closing port at the top end of the ultrafiltration device 1, then the ultrafiltration membrane group 6 is rotated, a plug board 6b arranged on the ultrafiltration membrane group 6 is correspondingly inserted between the two positioning clamp plates 1a, and then a sealing cover 8 can be inserted for sealing.
The working principle of the invention is as follows:
the method has the advantages that under the acidic condition, the water solubility of the carbendazim is greatly improved after the carbendazim is in a salt state, so that the carbendazim can more easily permeate the ultrafiltration membrane, and due to the three-dimensional property of the molecular structure, the effective components such as ginsenoside and the like cannot easily permeate the ultrafiltration membrane, so that the aim of separating the carbendazim and the ginsenoside is fulfilled, and the method is simple and convenient, stable in industrial application and low in operation cost.
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 carbendazim in a ginsenoside extract is characterized by comprising the following steps:
preparing a ginsenoside extract solution;
obtaining the ginsenoside extract solution, and adjusting the pH value of the ginsenoside extract solution;
obtaining the ginsenoside extract solution after the pH is adjusted, and carrying out primary membrane separation treatment on the ginsenoside extract solution after the pH is adjusted to obtain a ginsenoside extract filtrate;
obtaining the ginsenoside extract filtrate, and performing secondary membrane separation treatment on the ginsenoside extract filtrate to obtain ginsenoside extract retentate;
and (3) obtaining the ginsenoside extract trapped fluid, concentrating the ginsenoside extract trapped fluid, and drying to obtain the ginsenoside extract with carbendazim less than 10 ppb.
2. The method for removing carbendazim from a ginsenoside extract as claimed in 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 20-30 times the weight of the ginsenoside extraction raw product, and dissolving the ginsenoside extraction raw product to obtain ginsenoside extract solution.
3. The method as claimed in claim 2, wherein the ginsenoside extract solution is obtained, and the pH of the ginsenoside extract solution is adjusted to 2-5 by using one of hydrochloric acid and acetic acid.
4. The method for removing carbendazim from a ginsenoside extract as in claim 3, wherein the first membrane separation treatment is performed by using a ceramic membrane for clarification, the pore diameter of the ceramic membrane is 100-800nm, and the pressure of the ceramic membrane clarification treatment is 0.05-0.1 mpa.
5. The method for removing carbendazim from a ginsenoside extract according to claim 4, wherein the ginsenoside extract filtrate is obtained and subjected to a second membrane separation treatment to obtain a ginsenoside extract retentate, and the method specifically comprises the following steps:
obtaining the ginsenoside extract filtrate, and performing circulating ultrafiltration treatment by using an ultrafiltration membrane, wherein the molecular weight of the ultrafiltration membrane is 1000-10000 Dalton, the permeation pressure is 0.05-0.2mpa, and the circulating ultrafiltration time is 3-6 hours.
6. The method for removing carbendazim from a ginsenoside extract according to claim 5, wherein the ginsenoside extract retentate is obtained, concentrated and dried to obtain the ginsenoside extract with carbendazim less than 10ppb, wherein the drying mode is one of spray drying and freeze drying.
7. A device for removing carbendazim from ginsenoside extracts comprises an ultrafiltration system, and is characterized in that the ultrafiltration system comprises ultrafiltration equipment (1), a water inlet pipeline (2), a water production pipeline (3), a concentrated water pipeline (4) and a filter element replacement mechanism (5), the ultrafiltration equipment (1) is a column type ultrafiltration membrane filter, at least one ultrafiltration equipment (1) is arranged, the bottom and the top of the ultrafiltration equipment (1) are provided with the water inlet pipeline (2) and the water production pipeline (3), the water inlet pipeline (2) is provided with water inlet branch pipes with the same number as that of the ultrafiltration equipment (1), the water inlet branch pipes are in one-to-one correspondence with the ultrafiltration equipment (1) and are communicated with the inside of the corresponding ultrafiltration equipment (1), the water production pipeline (3) is provided with water production branch pipes with the same number as that of the ultrafiltration equipment (1), the water production branch pipes are in one-to-one correspondence with the ultrafiltration equipment (1) and are communicated with the inside of the, the top of the ultrafiltration equipment (1) is also provided with concentrated water pipelines (4), the concentrated water pipelines (4) are provided with concentrated water branch pipes (4a) with the same number as the ultrafiltration equipment (1), the concentrated water branch pipes (4a) correspond to the ultrafiltration equipment (1) one by one and are communicated with the interior of the corresponding ultrafiltration equipment (1), the interior of each ultrafiltration equipment (1) can be detachably connected with an ultrafiltration membrane group (6), the ultrafiltration membrane group (6) is detachably connected with at least one filter element (7) in a vertical state, each concentrated water branch pipe (4a) is provided with a filter element replacement mechanism (5), the filter element replacement mechanism (5) is used for controlling the opening and closing of the top end of the corresponding ultrafiltration equipment (1), when the filter element replacement mechanism (5) is in an open state, the ultrafiltration membrane group (6) and the filter element (7) can be separated from the ultrafiltration equipment (1), when the filter element replacement mechanism (5) is in a locked state, the ultrafiltration membrane group (6) and the filter element (7) are positioned inside the ultrafiltration device (1).
8. The apparatus for removing carbendazim from ginsenoside extract of claim 7, wherein the filter element replacement mechanism (5) comprises a rotary disc (5a), a positioning sleeve (5b), a plunger (5c), a movable push plate (5d), an electric push rod (5e), a movable member (5f) and a fixed member (5g), the top end of each ultrafiltration apparatus (1) is rotatably connected with the rotary disc (5a), the side of the rotary disc (5a) is provided with a driving component for driving the rotary disc (5a) to rotate along the central axis of the ultrafiltration apparatus (1), the rotary disc (5a) comprises a disc body (5a1), an outer convex surface (5a2) and an inner concave surface (5a3), the disc body (5a1) is annular, the top end of the disc body (5a1) is provided with a plurality of outer convex surfaces (5a2) and a plurality of inner concave surfaces (5a3) in a staggered manner, the disc body (5a1), the outer convex surfaces (5a2) and the inner concave surfaces (5a3) are, the top of the turntable (5a) is provided with at least one positioning sleeve (5b), the positioning sleeves (5b) are distributed along the circumference of the central shaft of the ultrafiltration device (1), the positioning sleeves (5b) are arranged along the radial extension of the ultrafiltration device (1), one end part of each positioning sleeve (5b) far away from the circle center of the ultrafiltration device (1) is provided with a positioning hole (5b1), an insert rod (5c) is connected on the positioning hole (5b1) in a sliding manner, one end part of each insert rod (5c) far away from the positioning sleeve (5b) is provided with a movable push plate (5d), the side part of each positioning sleeve (5b) is provided with an electric push rod (5e), the output end of each electric push rod (5e) is correspondingly connected with a movable push plate (5d), one end part of each positioning sleeve (5b) close to the circle center of the ultrafiltration device (1) is provided with a movable part (5f), each concentrated water, the movable piece (5f) is connected with the fixed piece (5g) in a sliding way.
9. The device for removing carbendazim from ginsenoside extracts of claim 8, wherein the movable member (5f) comprises a connecting ring (5f1), a vertical rod (5f2), teeth (5f3), an arc rod (5f4), a guide slip (5f5), a top cover (5f6) and a return spring (5f7), the fixed member (5g) comprises a lantern ring (5g1), fixed seats (5g2), an opening (5g3) and a gear (5g4), each concentrated water branch pipe (4a) is sleeved with a lantern ring (5g1), the number of the fixed seats (5g2) equal to that of the positioning sleeves (5b) are distributed on the periphery of the lantern ring (5g1), the opening (5g3) is formed in the fixed seat (5g2), the gear (5g4) is rotatably connected in the opening (5g3), the connecting ring (5f1) is sleeved at the end of the end part, which is close to the ultrafiltration device (1), the top end of the connecting ring (5f1) is provided with a vertical rod (5f2) in a vertical state, one end face of the vertical rod (5f2) is provided with teeth (5f3) meshed with the gears (5g4), the other end face of the vertical rod (5f2) is provided with an arc rod (5f4), the vertical rod (5f2) is provided with a guide inserting bar (5f5) protruding out of the vertical rod (5f2), the arc rod (5f4) and the guide inserting bar (5f5) are both in sliding connection with the opening (5g3), the top end of the vertical rod (5f2) is provided with a top cover (5f6), the top cover (5f6) is provided with a return spring (5f7), one end of the return spring (5f 6384) is connected with the top cover (5f6), and the other end of the return spring (5f7) is connected with the fixing seat (.
10. The apparatus for removing carbendazim from ginsenoside extracts of claim 9, wherein the ultrafiltration apparatus (1) is provided with a plurality of interlayers, the interlayers are disposed near the top end of the ultrafiltration apparatus (1), each interlayer comprises three positioning splints (1a), the positioning splints (1a) are disposed in a fan ring shape, the central angle of the positioning splints (1a) is 60 degrees, the positioning splints (1a) on the same interlayer are distributed along the circumference of the central shaft of the ultrafiltration apparatus (1), the ultrafiltration membrane group (6) comprises a first rod body (6a), an insertion plate (6b), a second rod body (6c), a partition plate (6d), a limiting plate (6e), a rotating shaft (6f) and an abutting plate (6g), the first rod body (6a) is provided with a plurality of insertion layers, the insertion layer is disposed near the top end of the first rod body (6a), each layer comprises three insertion plates (6b), the inserting plate (6b) is arranged to be fan-ring-shaped, the central angle of the inserting plate (6b) is 60 degrees, the positioning clamping plates (1a) on the same inserting layer are distributed along the circumference of the central shaft of the inserting plate (6b), the inserting plate (6b) is inserted between the two positioning clamping plates (1a) on the two layers of interlayers, the bottom end of the first rod body (6a) is provided with a second rod body (6c), three clapboards (6d) are distributed on the second rod body (6c) in the circumferential direction, the clapboards (6d) are arranged to be fan-ring-shaped, the central angle of the clapboards (6d) is 60 degrees, the clapboards (6d) are positioned under the inserting plate (6b), the clapboards (6d) are internally and detachably connected with a filter element (7), the limiting plates (6e) which are abutted to the filter element (7) are arranged on the clapboards (6d), the bottom end of the second rod body (6c) is rotatably connected, butt joint board (6g) set up to fan ring shape, and the central angle of butt joint board (6g) is 60, and the first body of rod (6a), the second body of rod (6c) and pivot (6f) all are equipped with certain clearance with ultrafiltration apparatus (1) inner wall with the coaxial setting of ultrafiltration apparatus (1) and the outer wall of the first body of rod (6a), the second body of rod (6c) and pivot (6 f).
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