CN110812518A - Low-temperature sterilization method and device for liquid substances such as plant extract liquid based on graphene nano material - Google Patents
Low-temperature sterilization method and device for liquid substances such as plant extract liquid based on graphene nano material Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
- A61L2/16—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using chemical substances
- A61L2/23—Solid substances, e.g. granules, powders, blocks, tablets
- A61L2/232—Solid substances, e.g. granules, powders, blocks, tablets layered or coated
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
- A61L2/02—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using physical phenomena
- A61L2/025—Ultrasonics
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
- A61L2/16—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using chemical substances
- A61L2/23—Solid substances, e.g. granules, powders, blocks, tablets
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2202/00—Aspects relating to methods or apparatus for disinfecting or sterilising materials or objects
- A61L2202/20—Targets to be treated
- A61L2202/21—Pharmaceuticals, e.g. medicaments, artificial body parts
Abstract
The invention relates to a low-temperature sterilization method for liquid substances such as plant extract liquid based on a graphene nano material, which comprises the following steps: enabling the liquid to be sterilized to flow through the graphene sterilization object to obtain sterilized liquidAnd storing the body; the graphene sterilization substance is one or more of graphene oxide, fluorinated graphene oxide and graphene composite sterilization substances; the graphene composite sterilization substance is a graphene oxide/silver nanoparticle composite material, a graphene oxide quantum dot/silver nanoparticle composite material, and graphene oxide/gamma-Fe2O3Nanocomposite and graphene oxide quantum dot/Fe3O4Any one or more of a composite material, a graphene oxide/cuprous oxide nanocomposite material and a zinc oxide/graphene oxide composite material. According to the invention, the graphene which is a substance with a sterilization function is used, so that liquid sterilization can be completed at normal temperature, and thus, the thermal unstable substances in the liquid are prevented from being degraded.
Description
Technical Field
The invention relates to the technical field of sterilization processes, in particular to a low-temperature sterilization method and device for liquid substances such as plant extract liquid based on graphene nano materials.
Background
In order to preserve these heat-unstable substances in the plant extract, various bacteria in the extract cannot be removed by adopting a high-temperature sterilization method, because the heat-unstable nutritive substances are decomposed while the microorganisms such as bacteria are removed at high temperature, the utilization value of the liquid substance is greatly reduced.
Therefore, it is necessary to develop a low-temperature sterilization method to effectively remove microorganisms such as bacteria in plant extracts and other liquids and simultaneously protect thermally unstable nutrients in the liquids from pyrolysis, so as to maximally retain nutritional or medicinal effective components in liquid substances such as plant extracts and improve the utilization value of the liquid substances.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a method and an apparatus for low-temperature sterilization of liquid materials such as plant extracts based on graphene nanomaterials.
A low-temperature sterilization method for liquid substances such as plant extract based on graphene nano materials comprises the following steps:
enabling the liquid to be sterilized to flow through the graphene sterilization object to obtain sterilized liquid and storing the sterilized liquid;
the graphene sterilization substance is one or more of graphene oxide, fluorinated graphene oxide and graphene composite sterilization substances; the graphene composite sterilization substance is a graphene oxide/silver nanoparticle composite material or a graphene oxide quantum dot/silver nanoparticle composite materialGraphene oxide/gamma-Fe2O3Nanocomposite and graphene oxide quantum dot/Fe3O4Any one or more of a composite material, a graphene oxide/cuprous oxide nanocomposite material and a zinc oxide/graphene oxide composite material.
Compared with the prior art, the low-temperature sterilization method for liquid substances such as the plant extract based on the graphene nanomaterial utilizes the graphene, as the diameter of carbon atoms forming the graphene is very small and belongs to the nanometer level, and the diameter of bacteria is 0.5-5 microns, when the bacteria in the liquid substances such as the plant extract are contacted with the carbon atoms in the graphene, bacterial cells are cut by the carbon atoms with smaller diameters, so that the bacteria die, and the sterilization effect is achieved; therefore, bacteria can be killed at normal temperature without high temperature and high pressure, so that thermally unstable substances in the liquid to be sterilized are prevented from being degraded, and the plant extract to be sterilized is still rich in various nutrient substances after being sterilized. Meanwhile, the graphene oxide has a smaller diameter than graphene, and the surface of the graphene oxide is provided with a plurality of irregular columnar or needle-point-shaped protrusions, so that bacterial cells can be broken easily; the fluorinated graphene contains a fluorocarbon bond, the fluorocarbon bond can release a small amount of fluorine ions, the fluorine ions can inhibit the synthesis of polysaccharide and lipoteichoic acid, and the polysaccharide and the lipoteichoic acid are important components forming bacterial cell walls and cell membranes, so that the fluorine example can inhibit the multiplication of bacteria, and the higher the concentration of the fluorine ions is, the more the bacterial number is reduced; the fluorinated graphene oxide has the sterilization advantages of both fluorinated graphene and oxidized graphene. This application jointly uses the graphene sterilization material that after multiple improvement, have stronger bactericidal effect to disinfect, has effectively promoted bactericidal effect, obtains disinfecting more thorough liquid.
Further, the liquid to be sterilized is sterilized by ultrasonic wave with the frequency of 20KHz-95 KHz. The ultrasonic wave can destroy the cell structures of bacteria and parasitic ova, thereby playing the role of assisting the graphene sterilizing material in sterilizing and killing or blocking parasites.
The invention also provides a low temperature of liquid substances such as plant extract of the graphene nano materialA sterilization apparatus comprising a pump-in valve, a cryogenic sterilization unit, and a sump; the pump-in valve presses the liquid to be sterilized into the low-temperature sterilization unit; the low-temperature sterilization unit performs low-temperature sterilization on liquid to be sterilized to obtain sterilized liquid; the collector collects and stores the sterilized liquid; and a graphene sterilizing object is arranged in the low-temperature sterilizing unit. The graphene sterilization substance is one or more of graphene oxide, fluorinated graphene oxide and graphene composite sterilization substances; the graphene composite sterilization substance is a graphene oxide/silver nanoparticle composite material, a graphene oxide quantum dot/silver nanoparticle composite material, and graphene oxide/gamma-Fe2O3Nanocomposite and graphene oxide quantum dot/Fe3O4Any one or more of a composite material, a graphene oxide/cuprous oxide nanocomposite material and a zinc oxide/graphene oxide composite material.
Compared with the prior art, the low-temperature sterilization device for liquid substances such as plant extract based on graphene nano materials utilizes graphene, because the diameter of carbon atoms forming the graphene is very small and belongs to a nano level, and the diameter of bacteria is 0.5-5 microns, when the bacteria in the liquid substances such as the plant extract are contacted with the carbon atoms in the graphene, bacterial cells are cut by the carbon atoms with smaller diameters, so that the bacteria die, and the sterilization effect is achieved; therefore, bacteria can be killed at normal temperature without high temperature and high pressure, so that thermally unstable substances in the liquid to be sterilized are prevented from being degraded, and the plant extract to be sterilized is still rich in various nutrient substances after being sterilized. Meanwhile, the graphene oxide has a smaller diameter than graphene, and the surface of the graphene oxide is provided with a plurality of irregular columnar or needle-point-shaped protrusions, so that bacterial cells can be broken easily; the fluorinated graphene contains carbon-fluorine bonds capable of sterilization; the fluorinated graphene oxide has the advantages of both fluorinated graphene and oxidized graphene. Simultaneously, the graphene sterilization substance with various improved and stronger sterilization effects is used for sterilization, so that the sterilization effect is effectively improved, and more thorough liquid for sterilization is obtained. In addition, the low-temperature sterilization device only comprises the pumping valve, the low-temperature sterilization unit and the storage tank, and has the advantages of simple integral structure, easy manufacture and installation and easy popularization.
Further, the low temperature sterilization unit includes the sterilization post, the sterilization screen cloth of a plurality of levels is provided with along the direction of liquid flow inside the sterilization post, sterilization screen cloth surface coating the graphite alkene fungus thing that disinfects.
Further, a sterilization bag is arranged inside the sterilization column and is positioned between the sterilization screens of adjacent levels; the graphene sterilization objects are wrapped on the sterilization bag, and meshes are arranged on the sterilization bag.
Further, the sterilization screen is a high-defect graphene oxide screen and/or a laser-induced graphene screen.
Furthermore, the mesh number of the high-defect graphene oxide screen is sequentially increased along the flowing direction of the liquid, and the mesh number of the laser-induced graphene screen is sequentially increased along the flowing direction of the liquid.
Further, the low-temperature sterilization unit further comprises a sterilization tank located between the sterilization column and the sump; the graphene sterilizing material is placed in the sterilizing tank, and an ultrasonic generator is arranged in the sterilizing tank.
Further, the graphene sterilization substance in the sterilization bag is fluorinated graphene oxide; the graphene sterilizing material in the sterilizing tank is a graphene composite sterilizing material, and the graphene composite sterilizing material is a graphene oxide/silver nanoparticle composite material, a graphene oxide quantum dot/silver nanoparticle composite material, graphene oxide/gamma-Fe2O3Nanocomposite and graphene oxide quantum dot/Fe3O4One or more of a composite material, a graphene oxide/cuprous oxide nanocomposite material, and a zinc oxide/graphene oxide composite material; the ultrasonic generator emits ultrasonic waves with the frequency of 20KHz-95 KHz. The sterilization bag increases the sterilization strength by using the fluorinated graphene oxide which has the respective sterilization characteristics of fluoride and graphene oxide.
Further, the sterilization column comprises a first sterilization column and a second sterilization column; the high-defect graphene oxide screens are arranged in the first sterilization column in a plurality of levels, the sterilization bag and the laser-induced graphene screens are arranged in the second sterilization column in a plurality of levels, and the sterilization bag and the laser-induced graphene screens are arranged in sequence along the flowing direction of liquid; valves are respectively arranged among the first sterilizing column, the second sterilizing column, the sterilizing pool and the storage tank.
Drawings
Fig. 1 is a schematic structural diagram of a low-temperature sterilization device for liquid substances such as plant extract based on graphene nano-materials, and the like, according to the present invention;
FIG. 2 is a photograph of fluorinated graphene oxide used in the present invention, wherein FIG. 2a is a real image of fluorinated graphene oxide, and FIG. 2b is a transmission electron micrograph of fluorinated graphene oxide;
FIG. 3 is a flow chart of the low-temperature sterilization of the Camellia nitidissima extract from Fanghong in example II;
FIG. 4 is a GC-MS detection result diagram of various amino acids in the anti-hong Kong golden camellia extract liquid after the sterilization treatment of the low-temperature sterilization device of liquid substances such as the plant extract liquid based on the graphene nano material and the like;
FIG. 5 is a graph showing the GC-MS detection results of various amino acids in the extract of Camellia nitidissima from Turkey harbor after sterilization treatment by the conventional high-temperature sterilization technique; wherein, the high-temperature sterilization conditions are as follows: treating at 121 deg.C for 30 min.
Detailed Description
The principle of the low-temperature sterilization method of liquid substances such as plant extract liquid based on graphene nano materials is as follows: the graphene is a two-dimensional carbon nanomaterial, the diameter of carbon atoms forming the graphene is very small and is in a nanometer level, the diameter of bacteria is 0.5-5 micrometers, and after bacteria in liquid substances such as plant extract liquid and the like are contacted with the carbon atoms in the graphene, bacterial cells can be cut by the carbon atoms with the smaller diameter, so that the bacteria die, and the sterilization effect is achieved. Meanwhile, the ultrasonic wave with the frequency of 20KHz-95KHz has high energy quickly contained in vibration, and can disturb the normal metabolism of bacteria so as to play a sterilization role. The graphene sterilizing material and the ultrasonic wave can kill bacteria at normal temperature by utilizing the performance of the graphene sterilizing material and the ultrasonic wave without high temperature and high pressure, thereby preventing thermally unstable substances in the liquid to be sterilized from being damaged, and leading the plant extract liquid to be sterilized to be still rich in various nutrient substances after being sterilized.
Furthermore, the graphene oxide has a smaller diameter compared with graphene, and the surface of the graphene oxide is provided with a plurality of irregular columnar or needle-point-shaped protrusions, so that bacterial cells can be broken easily; the fluorinated graphene contains a fluorocarbon bond, the fluorocarbon bond can release a small amount of fluorine ions, the fluorine ions can inhibit the synthesis of polysaccharide and lipoteichoic acid, and the polysaccharide and the lipoteichoic acid are important components forming bacterial cell walls and cell membranes, so that the fluorine example can inhibit the multiplication of bacteria, and the higher the concentration of the fluorine ions is, the more the bacterial number is reduced; the fluorinated graphene oxide has the advantages of fluorinated graphene and oxidized graphene, and has stronger bactericidal capacity.
The invention discloses a low-temperature sterilization method for liquid substances such as plant extract based on graphene nano materials, which comprises the following steps of:
s1: enabling the liquid to be sterilized to flow through the graphene sterilization object to obtain sterilized liquid;
the graphene sterilization substance is one or more of graphene oxide, fluorinated graphene oxide and graphene composite material sterilization substances; the graphene composite sterilization substance is a graphene oxide/silver nanoparticle composite material, a graphene oxide quantum dot/silver nanoparticle composite material, and graphene oxide/gamma-Fe2O3Nanocomposite and graphene oxide quantum dot/Fe3O4Any one or more of a composite material, a graphene oxide/cuprous oxide nanocomposite material and a zinc oxide/graphene oxide composite material.
S2: storing the sterilized liquid;
and (5) introducing the sterilized liquid into a storage device for storage.
In the low-temperature sterilization method of liquid substances such as plant extract based on graphene nano materials, if the liquid to be sterilized is the extract, the extract needs to be obtained by a low-temperature extraction method; the low-temperature extraction method is any one of a supercritical fluid technology, a subcritical extraction technology, a molecular distillation technology and a low-temperature solute extraction technology.
The specific structure of the low-temperature sterilization apparatus for liquid substances such as a graphene nanomaterial-based plant extract according to the present invention will be described below. Please refer to fig. 1, which is a schematic structural diagram of a low-temperature sterilization apparatus for liquid substances such as plant extract based on graphene nano-materials according to the present invention. The low-temperature sterilization device for liquid substances such as plant extract based on graphene nano materials comprises a pumping valve 10, a low-temperature sterilization unit 20 and a collecting and storing device 30 in sequence from front to back. Wherein the pump-in valve 10 is used to press the liquid to be sterilized into the sterilization unit 20; the low-temperature sterilization unit 20 is used for performing low-temperature sterilization on the liquid to be sterilized to obtain sterilized liquid; the sump 30 is used to collect and store the sterilized liquid.
The low-temperature sterilization unit 20 comprises a first sterilization column 21, a second sterilization column 22 and a sterilization pool 23; and a first valve 24 is arranged between the first sterilizing column 21 and the second sterilizing column 22, a second valve 25 is arranged between the second sterilizing column 22 and the sterilizing pond 23, and a third valve 26 is arranged between the sterilizing pond 23 and the sump 30. The first valve 24, the second valve 25 and the third valve 26 are responsible for controlling the flow of the liquid sterilized in the previous part into the next part, so as to prevent the liquid from flowing into the next part due to insufficient sterilization in the previous part and prevent the liquid which enters the next part and is sterilized from flowing back to the previous part.
The first sterilizing column 21 is internally provided with a 3-15-level high-defect graphene oxide screen 211. The mesh number of the high-defect graphene oxide screen 211 is gradually increased along the liquid flowing direction, and the adding proportion of the high-defect graphene oxide in the high-defect graphene oxide screen is 5% -12.5%.
The interior of the second sterilization column 22 is filled with fluorinated graphene oxide 221, and a 3-8-level laser-induced graphene screen 222 is disposed at one end close to the sterilization tank 23. Please refer to fig. 2, which is a picture of the fluorinated graphene oxide used in the present invention, wherein fig. 2a is a picture of the fluorinated graphene oxide, and fig. 2b is a transmission electron microscope picture of the fluorinated graphene oxide. The fluorinated graphene oxide 221 is wrapped in 100-325 mesh regenerated fiber cloth or glass fiber cloth, and the fluorine doping proportion in the fluorinated graphene oxide 221 is 0.25% -1.25%. The mesh number of the graphene sterilization grids 222 increases along the flowing direction of the liquid.
The sterilizing tank 23 is filled with graphene sterilizing material 231 and is provided with an ultrasonic generator 232. The graphene sterilization object 231 is a graphene oxide/silver nanoparticle composite material, a graphene oxide quantum dot/silver nanoparticle composite material, and graphene oxide/gamma-Fe2O3Nanocomposite and graphene oxide quantum dot/Fe3O4Any one or more of a composite material, a graphene oxide/cuprous oxide nanocomposite material and a zinc oxide/graphene oxide composite material. The frequency of the ultrasonic wave generated by the ultrasonic wave generator 232 is 20KHz-95KHz, and the working time is 15-30 min.
The first sterilizing column, the second sterilizing column, the high-defect graphene oxide screen, the laser-induced graphene screen and the sterilizing tank are made of one of stainless steel, ceramic, glass, polyvinylidene fluoride, polytetrafluoroethylene and polyether ether ketone; the pump of the pump-in valve can be one of a peristaltic pump, a plunger pump or a diaphragm pump; the size of the laser-induced graphene screen is matched with the inner diameter of the second sterilization column, and the edge of the laser-induced graphene screen is provided with a protrusion device matched with the longitudinal groove on the inner wall of the second sterilization column, so that the laser-induced graphene screen is convenient to replace and clean; high defect oxidation graphite alkene screen cloth size matches with first sterilization post internal diameter, and its edge is provided with the vertical recess assorted projection means of first sterilization post inner wall, is convenient for change, washs. In addition, the high-defect graphene oxide screen can be prepared by directly forming a high-defect graphene oxide coating of 0.01-0.8 μm on a screen of a relevant size. The laser-induced graphene screen is prepared by forming a coating with the thickness of 0.01-0.8 mu m on a screen with a relevant size by adopting a laser-induced graphene nano material; in particular, laser-induced graphene nanomaterialsThe preparation method comprises the following steps: soaking a 6H-SiC silicon carbide wafer in acetone, removing organic residues on the surface by ultrasonic treatment for 15 minutes, and then irradiating a sample for 60 nanoseconds by using a xenon chloride excimer laser with the wavelength of 308nm, wherein the specific parameter of the xenon chloride excimer laser is that the single pulse energy density is 1.08J/cm2Frequency 5Hz, pulse number 60, defocus amount 3cm2The area of the light spot is 0.45cm2Mask area 8mm2And obtaining two layers of substances after laser irradiation, namely a polysilicon layer on the upper layer and a laser-induced graphene layer on the lower layer, then irradiating for 60 nanoseconds by using 193nm argon fluorine laser or 248nm krypton fluorine laser, wherein the frequency is 9Hz, the pulse number is 90, and laser irradiation is performed again to sublimate silicon, so that only the laser-induced graphene nano material is left.
The use method of the low-temperature sterilization device for liquid substances such as plant extract liquid based on the graphene nano material comprises the following steps: pumping the liquid to be sterilized into the first sterilizing column 21 by using the pump-in valve 10, and allowing the liquid to be sterilized to flow through the plurality of layers of high-defect graphene oxide screens 211 inside the first sterilizing column 21 in sequence for first sterilization to obtain a liquid for first sterilization; the liquid subjected to primary sterilization flows into the second sterilization column 22 through the first valve 24, and flows through the graphene fluoride oxide 221 and the 3-8-level graphene sterilization grid 222 in sequence for secondary sterilization to obtain liquid subjected to secondary sterilization; the liquid after the secondary sterilization flows into the sterilization tank 23 through the second valve 25, flows through the graphene sterilization object 231, and is subjected to ultrasonic sterilization at 20KHz-95KHz for 15-30min to obtain liquid after the tertiary sterilization; the liquid after the third sterilization is guided into the sump through the third valve 26 and the conduit, and meanwhile, the inert gas is introduced for sealing and storing.
The low-temperature sterilization apparatus for liquid substances such as plant extracts based on graphene nanomaterials of the present invention may have various modifications, for example, the sterilization screen may have a mesh structure such as a sterilization grid or a sterilization permeable membrane, as well as the shape of the screen; the sterilization screen can be not only a high-defect graphene oxide screen and a laser-induced graphene screen, but also a fluorinated graphene screen and the like; the number of the layers of the high-defect graphene oxide screen can be any, more than 3-15 layers; likewise, the number of layers of the laser-induced graphene screen can be any number of layers, more than 3-8 layers.
Example one
The embodiment takes the anti-harbour golden camellia as an example, and specifically explains the low-temperature sterilization method and the use method of the device for the anti-harbour golden camellia extract liquid and other liquid substances based on the graphene nano material. Please refer to fig. 3, which is a flowchart illustrating a low-temperature sterilization process of the anti-harbour camellia nitidissima extract based on the graphene nanomaterial according to the embodiment.
Pretreatment: cleaning, crushing and grinding the flowers of the anti-hong Kong golden camellia, and then carrying out supercritical CO treatment2Extracting by a low-temperature extraction process to obtain an urban-harbor-preventing golden camellia flower extract to be sterilized;
s1: sterilizing the liquid to be sterilized by combining graphene sterilization substances and ultrasonic waves at low temperature to obtain sterilized liquid
Pumping the pre-treated extract to be sterilized into a pump valve 10; pumping an extract liquid to be sterilized into a first sterilizing column 21 by a pump valve 10, wherein the extract liquid to be sterilized sequentially flows through eight-level polytetrafluoroethylene high-defect graphene oxide screens 211 in the first sterilizing column 21 to obtain a primarily sterilized urban harbor prevention camellia nitidissima flower extract liquid, the mesh number of the eight-level high-defect graphene oxide screens is 20 meshes, 60 meshes, 170 meshes, 400 meshes, 650 meshes, 1100 meshes, 2000 meshes and 5000 meshes in sequence from front to back, and the adding proportion of the high-defect graphene oxide in the high-defect graphene oxide screens is 6%; opening a first valve 24, enabling the primarily sterilized extract liquor of the flowers of the harbour-preventing camellia nitidissima to enter a second sterilization column 22 made of ceramic materials to further inactivate residual bacteria in the extract liquor, enabling the extract liquor to firstly flow through a graphene fluoride oxide 221 wrapped by glass fiber cloth with the mesh number of 170 meshes in the second sterilization column 22, enabling the fluorine doping proportion of the graphene fluoride oxide to be 1.1%, and then flow through a five-layer laser-induced graphene sterilization grid 222 to obtain the secondarily sterilized extract liquor of the flowers of the harbour-preventing camellia nitidissima, wherein the mesh numbers of the five-layer laser-induced graphene sterilization grid are 10 meshes, 35 meshes, 100 meshes, 200 meshes and 325 meshes from front to back in sequence; and opening the second valve 25, enabling the secondarily sterilized extract of the flowers of the urban-harbor-prevention golden camellia to flow into the sterilization tank 23 filled with the graphene oxide/silver nanoparticle composite material as the graphene sterilization object 231, and simultaneously, emitting ultrasonic waves with the frequency of 60KHz by an ultrasonic generator in the sterilization tank 23 for auxiliary sterilization for 20min to obtain the thirdly sterilized extract of the flowers of the urban-harbor-prevention golden camellia.
S2: storing the sterilized liquid
And opening the third valve 26, so that the three times of sterilized extract liquor of the flowers of the urban-harbor golden camellia after being sterilized in the sterilizing tank 23 is guided by the guide pipe to enter the collecting and storing device 30, and is sealed and stored after being filled with inert gas, and the subsequent products are reserved for development, production and use.
The eight-level high-defect graphene oxide sterilization screen 211 in this embodiment can be prepared by directly forming a 0.1 μm high-defect graphene oxide coating on a screen of the relevant size, where the high-defect graphene oxide coating is prepared by hydrogen plasma acting on graphene oxide, and the graphene oxide is obtained by Hummers method; the laser-induced graphene sterilization grid is prepared by forming a 0.08-micrometer nano coating on the surface of ceramic by using a silver oxide-laser-induced graphene nano composite material 222.
And (3) effect detection:
dividing the preprocessed anti-urban-harbor honeysuckle extract into two groups, wherein one group is subjected to low-temperature sterilization by a low-temperature sterilization device for liquid substances such as the plant extract based on the graphene nano material; sterilizing the other group by conventional high temperature sterilization technology (treatment at 121 deg.C for 30 min); and then, respectively detecting amino acids in the two groups of sterilized extract liquor of the honeysuckle in urban harbor by adopting CC-MS.
Please refer to fig. 4, which is a GC-MS detection result diagram of various amino acids in the extract of camellia nitidissima from urban harbor defense after the sterilization treatment of the low-temperature sterilization device for liquid substances such as the plant extract based on the graphene nanomaterial of the present invention. As can be seen from fig. 4, after the anti-urban-port golden camellia extraction liquid is subjected to low-temperature sterilization by using the low-temperature sterilization device based on the graphene nanotechnology of the invention, 17 amino acid active ingredients including Thr, Val, Leu, Ile, Cys, Pro, Met, Asp, Phe, Glu, Lys, Tyr, His and Arg can be detected from the sterilized anti-urban-port golden camellia extraction liquid, wherein the amino acid active ingredients include seven Essential Amino Acids (EAAs) for human body, including Thr, Val, Leu, Ile, Met, Phe and Lys.
Please refer to fig. 5, which is a graph showing the GC-MS detection results of various amino acids in the extract of camellia nitidissima after sterilization treatment by conventional high temperature sterilization (treatment at 121 ℃ for 30 min). As shown in FIG. 5, after the anti-urban-harbor golden camellia extract is subjected to high-temperature sterilization by using the traditional high-temperature sterilization technology, 14 amino acid active ingredients including Thr, Val, Leu, Ile, Pro, Asp, Phe, Glu, Lys, His and Arg can be detected from the sterilized anti-urban-harbor honeysuckle extract, wherein the amino acid active ingredients include six Essential Amino Acids (EAAs) for human body. In comparison with FIG. 4, Cys, Met, and Tyr were absent, indicating that these three amino acids were completely destroyed by high temperature sterilization; and the peak value of the remaining 14 amino acids is relatively low, which indicates that the 14 amino acids are partially degraded and lost after high-temperature sterilization; meanwhile, a more impurity peak appears in fig. 5, which is presumed to be the decomposition of the thermally destroyed amino acid nutrient into other non-nutrients.
Therefore, compared with the traditional high-temperature sterilization technology, the low-temperature sterilization technology based on the graphene nano material can effectively prevent the nutrient components in the liquid species from being decomposed, so that the liquid substance has richer nutrition.
Example two
The present embodiment takes a camellia chrysantha having clustered cores as an example, and specifically explains a method for sterilizing liquid substances such as a camellia chrysantha extract based on graphene nano materials at a low temperature and a method for using the device.
Pretreatment: after the leaves of the eurotium cristatum camellia are cleaned, crushed, ground and the like, the molecular distillation extraction process is carried out to extract the leaves of the eurotium cristatum camellia to be sterilized to obtain an extract liquid of the eurotium cristatum camellia;
s1: sterilizing the liquid to be sterilized by the combination of the sterilized object and the ultrasonic wave at low temperature to obtain the sterilized liquid
Pumping the pre-treated extract to be sterilized into a pump valve 10;the method comprises the steps that an extract liquid to be sterilized is pumped into a first sterilizing column 21 made of ceramic materials through a pump-in valve 10, the extract liquid to be sterilized sequentially flows through a six-level high-defect graphene oxide screen 211 made of polyether-ether-ketone materials in the first sterilizing column 21 to obtain a primarily sterilized golden camellia bunch leaf extract liquid, the mesh number of the six-level high-defect graphene oxide screen is 50 meshes, 120 meshes, 325 meshes, 540 meshes, 900 meshes and 1600 meshes from front to back, and the adding proportion of the high-defect graphene oxide in the high-defect graphene oxide screen is 10%; opening a first valve 24, enabling the primarily sterilized golden camellia leaf extract to enter a second sterilization column 22 made of toughened glass material to further inactivate residual bacteria in the extract, enabling the extract to flow through a graphene fluoride oxide 221 wrapped by glass fiber cloth with a grid mesh number of 120 meshes in the second sterilization column 22, enabling the fluorine doping proportion of the graphene fluoride oxide to be 0.5%, and then flowing through a five-layer laser-induced graphene sterilization grid 222 to obtain a secondarily sterilized golden camellia leaf extract, wherein the grid mesh number of the four-layer laser-induced graphene sterilization grid is sequentially 20 meshes, 80 meshes, 170 meshes and 400 meshes from front to back; opening the second valve 25, and allowing the secondary sterilized golden camellia leaf extract to flow into the container filled with graphene oxide/gamma-Fe2O3The nano composite material is used as a graphene sterilizing material 231 in a sterilizing tank 23, and meanwhile, an ultrasonic generator in the sterilizing tank 23 emits ultrasonic waves with the frequency of 45KHz for auxiliary sterilization for 30min, so that the camellia chrysantha leaf extract liquid with three times of sterilization is obtained.
S2: storing the sterilized liquid
And opening the third valve 26, so that the three times of sterilized golden camellia leaf extract obtained after sterilization in the sterilization tank 23 is guided by the guide pipe to enter the collecting and storing device 30, and is sealed and stored after inert gas is filled in, and the subsequent products are reserved for development, production and use.
The six-level high-defect graphene oxide sterilization screen 211 in this embodiment may be prepared by forming a 0.02 μm high-defect graphene oxide coating directly on a relevant size screen, and the high-defect graphene oxide is formed by excess strong oxide (KMnO)4，H2SO4，H2O2Etc.) is obtained by acting on graphene oxide, and the graphene oxide is prepared by an improved Hummers method; the laser-induced graphene sterilization grid 222 is prepared by forming a 0.05-micrometer nano coating on the surface of a polyether-ether-ketone polymer material by using a zinc oxide-laser-induced graphene nano composite material.
In addition to the pistachio camellia in the embodiment and the hongkong camellia in the embodiment, there may be camellia sinensis, longrui camellia, dongxing camellia chrysantha, small camellia chrysantha and its varieties, middle east camellia chrysantha, mao camellia chrysantha, venation camellia chrysantha, lamellate camellia, small camellia chrysantha, four season camellia chrysantha, mao seed camellia chrysantha, straight venation camellia chrysantha, multiple camellia chrysantha, lemon camellia chrysantha, yellow camellia chrysantha, thin camellia chrysantha, summer camellia chrysantha, long pillar camellia chrysantha, dragon zhou camellia chrysantha, wuming camellia chrysantha, flat camellia chrysantha, top camellia chrysantha, small camellia chrysantha, plucked camellia chrysantha, thin camellia chrysantha, hibiscus, anthrischianus, multiple camellia chrysantha, light yellow camellia chrysantha, light camellia chrysantha, bougainvillea, straight venation camellia chrysantha, blosson camellia chrysantha, five-chamber camellia chrysantha, four-river camellia chrysantha, zhou camellia chrysantha, and camellia chrysanth, Yunnan Camellia Chysantha, Yupisti Camellia Chysantha, Vietnam Tokyo Camellia Chysantha, Kuck Camellia Chysantha, Thick leaf Camellia Chysantha, Tamikan Camellia Chysantha, Hulong Camellia Chysantha, and Camellia luteopalida (T.Q.T.Nguyen & Luu), Camellia bugiamapensis (Orel, Curry, Luu & Q.D.), and Camellia capecitata (Orel, Curry & Luu, sp.nov.).
EXAMPLE III
In this embodiment, a Rou mountain ancient tree tea is taken as an example, and a method for sterilizing liquid substances such as Rou mountain ancient tree tea extract liquid based on graphene nano-materials at a low temperature and a method for using the device are specifically explained.
Pretreatment: cleaning, crushing, grinding and the like of Roujiang mountain ancient tree tea leaves, and extracting by an ethanol extraction process to obtain Roujiang mountain ancient tree tea leaf extract to be sterilized;
s1: sterilizing the liquid to be sterilized by the combination of the sterilized object and the ultrasonic wave at low temperature to obtain the sterilized liquid
Is obtained by pretreatmentThe extract to be sterilized is introduced into the pump valve 10; the method comprises the following steps that an extract liquid to be sterilized is pumped into a first sterilizing column 21 made of stainless steel through a pump-in valve 10, the extract liquid to be sterilized sequentially flows through a high-defect graphene oxide screen 211 made of eight-level polyvinylidene fluoride in the first sterilizing column 21 to obtain a Rou hole high mountain ancient tree tea leaf extract liquid subjected to primary sterilization, the mesh number of the seven-level high-defect graphene oxide screen is 20 meshes, 60 meshes, 150 meshes, 325 meshes, 650 meshes, 1100 meshes and 2000 meshes sequentially from front to back, and the adding proportion of the high-defect graphene oxide in the high-defect graphene oxide screen is 12.5%; opening a first valve 24, allowing the primarily sterilized Rou hole mountain ancient tree tea leaf extract to enter a second sterilization column 22 made of toughened glass material to further inactivate residual bacteria in the extract, allowing the extract to flow through a glass fiber cloth coated graphite fluoride oxide 221 with a mesh number of 120 meshes in the second sterilization column 22, wherein the fluorine doping proportion of the graphite fluoride oxide is 0.75%, and then flowing through a four-level laser-induced graphene sterilization grid 222 to obtain a secondarily sterilized Rou hole mountain ancient tree tea leaf extract, wherein the mesh numbers of the four-level laser-induced graphene sterilization grid are 50 meshes, 200 meshes, 325 meshes and 650 meshes from front to back in sequence; opening the second valve 25, and allowing the secondary sterilized Rou hole mountain ancient tree tea leaf extract to flow into the container filled with graphene oxide/Fe3O4The nano particle composite material is used as a graphene sterilizing material 231 in a sterilizing tank 23, and meanwhile, an ultrasonic generator in the sterilizing tank 23 emits ultrasonic waves with the frequency of 45KHz for assisting sterilization for 10min, so that the Rongshan mountain ancient tree tea leaf extract liquid subjected to three times of sterilization is obtained.
S2: storing the sterilized liquid
And opening the third valve 26, so that the tea leaf extract of the Rou-hole mountain ancient tree which is sterilized for three times and is obtained after the sterilization in the sterilization tank 23 is guided by the guide pipe to enter the collecting and storing device 30, and is sealed and stored after being filled with inert gas, and the subsequent products are reserved for development, production and use.
The six-level high-defect graphene oxide sterilization screen 211 in this embodiment may be prepared by directly forming a 0.35 μm high-defect graphene oxide coating on a screen of a relevant size, and the high-defect graphene oxide is obtained by three-dimensionally assembling graphene; the laser-induced graphene sterilization grid 222 is prepared by forming a 0.015-micrometer nano coating on the surface of ceramic by using a zinc oxide-laser-induced graphene nano composite material.
Besides the Rongchun alpine ancient tree tea in this embodiment, the Rongchun alpine Maojian tea may be tea leaves such as Biluochun tea, Xinyang Maojian tea, West lake Longjing tea, Junshan Yinzhen, Huangshan Maofeng tea, Wuyi Yangyan tea, Qimen black tea, Duyun Maojian tea, Tieguanyin tea, Liuan Guguapian, Fenghuandan tea, Rongguguan Guzhi tea, Lushan Yunwu tea, Yinde black tea, Lingyun pehao tea, Anhua black tea, Yunnan Pu' er tea, Wuyi mountain Dahongpao, Fujian Yizhen, Suzhou jasmine flower and.
Compared with the prior art, the low-temperature sterilization method for liquid substances such as plant extract based on the graphene nanomaterial performs liquid sterilization by using the improved nanomaterial such as graphene oxide, graphene fluoride and graphene fluoride oxide with stronger sterilization function together with ultrasonic waves, so that the sterilization of liquid substances such as the plant extract can be efficiently completed at normal temperature without high temperature, thereby avoiding the degradation of heat-unstable substances in the liquid substances, and reserving nutritional or medicinal effective components in the liquid substances such as the plant extract to the maximum extent; meanwhile, the low-temperature sterilization device for liquid substances such as plant extract liquid based on the graphene nano material has the advantages of simple overall structure, simplicity and easiness in manufacturing, installation and operation and easiness in popularization.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. A low-temperature sterilization method for liquid substances such as plant extract based on graphene nano materials is characterized by comprising the following steps:
enabling the liquid to be sterilized to flow through the graphene sterilization object to obtain sterilized liquid and storing the sterilized liquid;
the graphene sterilization substance is graphene oxide or fluorinated grapheneOne or more of fluorinated graphene oxide and graphene composite sterilization substances; the graphene composite sterilization substance is a graphene oxide/silver nanoparticle composite material, a graphene oxide quantum dot/silver nanoparticle composite material, and graphene oxide/gamma-Fe2O3Nanocomposite and graphene oxide quantum dot/Fe3O4Any one or more of a composite material, a graphene oxide/cuprous oxide nanocomposite material and a zinc oxide/graphene oxide composite material.
2. The method for low-temperature sterilization of liquid substances such as graphene nanomaterial-based plant extract according to claim 1, wherein the method comprises the following steps: the liquid to be sterilized is sterilized by ultrasonic wave with the frequency of 20KHz-95 KHz.
3. A low temperature sterilization device of liquid substances such as plant extract based on graphene nano-materials is characterized in that: comprises a pump-in valve, a low-temperature sterilization unit and a storage tank; the pump-in valve presses the liquid to be sterilized into the low-temperature sterilization unit; the low-temperature sterilization unit performs low-temperature sterilization on liquid to be sterilized to obtain sterilized liquid; the collector collects and stores the sterilized liquid; a graphene sterilizing object is arranged in the low-temperature sterilizing unit; the graphene sterilization substance is one or more of graphene oxide, fluorinated graphene oxide and graphene composite sterilization substances; the graphene composite sterilization substance is a graphene oxide/silver nanoparticle composite material, a graphene oxide quantum dot/silver nanoparticle composite material, and graphene oxide/gamma-Fe2O3Nanocomposite and graphene oxide quantum dot/Fe3O4Any one or more of a composite material, a graphene oxide/cuprous oxide nanocomposite material and a zinc oxide/graphene oxide composite material.
4. The device for low-temperature sterilization of liquid substances such as plant extract liquid based on graphene nano-materials according to claim 3, is characterized in that: the low temperature sterilization unit includes the post that disinfects, the inside sterilization screen cloth that is provided with a plurality of levels along the direction of liquid flow of post that disinfects, sterilization screen cloth surface coating the graphite alkene sterilization thing.
5. The device for low-temperature sterilization of liquid substances such as plant extract liquid based on graphene nano-materials according to claim 6, is characterized in that: a sterilization bag is further arranged inside the sterilization column and is positioned between the sterilization screens of adjacent levels; the graphene sterilization objects are wrapped on the sterilization bag, and meshes are arranged on the sterilization bag.
6. The device for low-temperature sterilization of liquid substances such as plant extract liquid based on graphene nano-materials according to claim 5, is characterized in that: the sterilization screen is a high-defect graphene oxide screen and/or a laser-induced graphene screen.
7. The device for low-temperature sterilization of liquid substances such as plant extract liquid based on graphene nano-materials according to claim 4, is characterized in that: the mesh number of the high-defect graphene oxide screen is sequentially increased along the flowing direction of the liquid, and the mesh number of the laser-induced graphene screen is sequentially increased along the flowing direction of the liquid.
8. The device for low-temperature sterilization of liquid substances such as plant extracts based on graphene nano-materials according to any one of claims 3 or 7, characterized in that: the low-temperature sterilization unit further comprises a sterilization tank located between the sterilization column and the sump; the inside graphite alkene sterilization thing of placing of sterilizing tank to be provided with supersonic generator.
9. The device for low-temperature sterilization of liquid substances such as plant extract liquid based on graphene nano-materials according to claim 8, wherein: the graphene sterilization substance in the sterilization bag is fluorinated graphene oxide; the graphene sterilizing material in the sterilizing tank is grapheneThe graphene composite sterilization substance is a graphene oxide/silver nanoparticle composite material, a graphene oxide quantum dot/silver nanoparticle composite material, and graphene oxide/gamma-Fe2O3Nanocomposite and graphene oxide quantum dot/Fe3O4One or more of a composite material, a graphene oxide/cuprous oxide nanocomposite material, and a zinc oxide/graphene oxide composite material; the ultrasonic generator emits ultrasonic waves with the frequency of 20KHz-95 KHz.
10. The device for low-temperature sterilization of liquid substances such as plant extracts based on graphene nano-materials according to any one of claims 8 or 9, characterized in that: the sterilizing column comprises a first sterilizing column and a second sterilizing column; the high-defect graphene oxide screens are arranged in the first sterilization column in a plurality of levels, the sterilization bag and the laser-induced graphene screens are arranged in the second sterilization column in a plurality of levels, and the sterilization bag and the laser-induced graphene screens are arranged in sequence along the flowing direction of liquid; valves are respectively arranged among the first sterilizing column, the second sterilizing column, the sterilizing pool and the storage tank.
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