AU2021102534A4 - Low-temperature sterilization method and device for liquid substances such as Theaceae plant extracts based on graphene nano materials - Google Patents
Low-temperature sterilization method and device for liquid substances such as Theaceae plant extracts based on graphene nano materials Download PDFInfo
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- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
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- 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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Abstract
The invention relates to a low-temperature sterilization method for liquid substances such as
plant extracts based on graphene nano materials, which comprises the following steps of
enabling liquid waiting for sterilization to flow through graphene sterilization substances to
obtain sterilized liquid and store the sterilized liquid. The graphene sterilization substance is
one or more of graphene oxide, fluorinated graphene, fluorinated graphene oxide and
functionalized graphene nanocomposites. Specifically, the graphene nanocomposite
sterilization substance is any one or more of graphene oxide/silver nano particle
nanocomposite, graphene oxide quantum dots/silver nano particle composite, graphene
oxide/y-Fe203 nanocomposite, graphene oxide quantum dots/Fe304 composites, graphene
oxide/cuprous oxide nanocomposite, zinc oxide/graphene oxide composite. According to the
invention, the liquid sterilization can be completed at normal temperature by using the
substance with sterilization function, namely graphene, so that the heat-labile substances in the
liquid are prevented from being degraded.
Description
Low-temperature sterilization method and device for liquid substances such as
Theaceae plant extracts based on graphene nano materials
The invention relates to the technical field of sterilization technology, in particular to a
low-temperature sterilization method and a device for liquid substances such as Theaceae
plant extracts based on graphene nano materials.
Many liquids, especially Theaceae plant extracts, contain some nutrients which are easy
to decompose at high temperature. For example, tea polyphenols, B vitamins, vitamin C,
vitamin E, various amino acids, -carotene and other substances in Camellia nitidissima
Chi extracts will decompose at high temperature and cannot exist stably. In order to
preserve these heat-labile substances in plant extracts, it is impossible to use high
temperature sterilization to remove all kinds of bacteria in the extracts, because the heat
labile nutritional substances are decomposed at the same time when bacteria and other
microorganisms are removed at high temperature, which greatly reduces the utilization
value of liquid substances.
Therefore, it is necessary to develop a low-temperature sterilization method to effectively
remove microorganisms such as bacteria in Theaceae plant extracts and other liquids, and
at the same time protect the heat-labile nutrients in the liquids from high-temperature
decomposition, so as to maximize the retention of nutritional or medicinal ingredients in
liquid substances such as plant extracts and improve their utilization value.
Therefore, it is an object of the present invention to provide a method and a device for
low-temperature sterilization of liquid substances such as plant extracts based on
graphene nano materials.
A low-temperature sterilization method for liquid substances such as Theaceae plant
extracts based on graphene nano materials comprises the following steps of enabling
liquid waiting for sterilization to flow through graphene sterilization substances to obtain
sterilized liquid and store the sterilized liquid.
Wherein, the graphene sterilization substance is one or more of graphene oxide,
fluorinated graphene, fluorinated graphene oxide and functionalized graphene
nanocomposite sterilization substances. Specifically, the graphene composite sterilization
substance is any one or more of graphene oxide/silver nano particle composite, graphene
oxide quantum dots/silver nano particle composite, graphene oxide/y-Fe203
nanocomposite, graphene oxide quantum dots/Fe304 composites, graphene oxide/cuprous
oxide nanocomposite, zinc oxide/graphene oxide composite.
Compared with the prior technologies, the method for low-temperature sterilization of
liquid substances such as Theaceae plant extracts based on graphene nano materials
utilizes graphene, and because the diameter of carbon atoms composing graphene is very
small and belongs to nanometer level, while the diameter of bacteria is between 0.5 and 5
microns, when bacteria in liquid substances such as plant extracts contact with carbon
atoms in graphene, bacterial cells will be split by carbon atoms with smaller diameters,
thus causing bacteria to die and achieving the sterilization effect. Therefore, the bacteria
can be killed at normal temperature without high temperature and high pressure, so that the heat-labile substances in the liquid to be sterilized are prevented from being degraded, and the Theaceae plant extracts to be sterilized is still rich in various nutrients after being sterilized. At the same time, graphene oxide and functionalized graphene have similar diameters than graphene, and the surface has a plurality of irregular columnar or needle like protrusions, which is more conducive to breaking bacterial cells. Fluorinated graphene contains carbon-fluorine bonds, which can release a small amount of fluoride ions. Fluorine ions can inhibit the synthesis of polysaccharide and lipoteichoic acid, which are important components of bacterial cell wall and cell membrane, so fluorine ions can inhibit the reproduction of bacteria, and the higher the concentration of fluoride ions, the more the number of bacteria decreases. Fluorinated graphene oxide has the sterilization advantages of fluorinated graphene and oxidized graphene. According to the application, various improved graphene sterilization substances with stronger sterilization effect are used for sterilization, so that the sterilization effect is effectively improved, and a liquid with more thorough sterilization is obtained.
Furthermore, the liquid to be sterilized is also sterilized by ultrasonic wave with the
frequency of 20KHz95KHz. Ultrasonic wave can destroy the cell structure of bacteria
and parasite eggs, thus playing the role of assisting graphene sterilization and killing or
blocking parasites.
The invention also provides a low-temperature sterilization device for liquid substances
such as plant extracts based on graphene nano materials, which comprises a pumping
valve, a low-temperature sterilization unit and a collection device. The pumping valve
presses the liquid to be sterilized into the low-temperature sterilization unit; the low
temperature sterilization unit performs low-temperature sterilization on the liquid to be sterilized to obtain sterilized liquid; the collection device collects and stores sterilized liquid; the low-temperature sterilization unit is provided with graphene sterilization substances. Wherein, the graphene sterilization substance is one or more of graphene oxide, fluorinated graphene, fluorinated graphene oxide and functionalized graphene nanocomposite sterilization substances. Specifically, the graphene composite sterilization substance is any one or more of graphene oxide/silver nano particle composite, graphene oxide quantum dots/silver nano particle composite, graphene oxide/y-Fe203 nanocomposite, graphene oxide quantum dots/Fe304 composites, graphene oxide/cuprous oxide nanocomposite, zinc oxide/graphene oxide composite.
Compared with the prior technologies, the device for low-temperature sterilization of
liquid substances such as Theaceae plant extracts based on graphene nano materials
utilizes graphene, and because the diameter of carbon atoms composing graphene is very
small and belongs to nanometer level, and the diameter of bacteria is between 0.5 and 5
microns, when bacteria in liquid substances such as plant extracts contact with carbon
atoms in graphene, bacterial cells will be split by carbon atoms with smaller diameters,
thus causing bacteria to die and achieving the sterilization effect. Therefore, the bacteria
can be killed at normal temperature without high temperature and high pressure, so that
the heat-labile substances in the liquid to be sterilized are prevented from being degraded,
and the plant extract to be sterilized is still rich in various nutrients after being sterilized.
At the same time, graphene oxide has a smaller diameter than graphene, and the surface
has a plurality of irregular columnar or needle-like protrusions, which is more conducive
to breaking bacterial cells. Fluorinated graphene contains carbon-fluorine bonds, which
can perform sterilization. Fluorinated graphene oxide has the sterilization advantages of fluorinated graphene and oxidized graphene. Besides, various improved graphene sterilization substances with stronger sterilization effect are used for sterilization, so that the sterilization effect is effectively improved, and a liquid with more thorough sterilization is obtained. In addition, the low-temperature sterilization device of the invention only comprises a pumping valve, a low-temperature sterilization unit and a collection device, indicating a simple overall structure, easy manufacture and installation and easy popularization.
Further, the low-temperature sterilization unit comprises a sterilization column, and
several levels of sterilization screens are arranged inside the sterilization column along
the liquid flow direction, and the surface of the sterilization screen is coated with the
graphene sterilization substance.
Further, a sterilization bag is also arranged inside the sterilization column, and the
sterilization bag is located between the sterilization screens at adjacent levels. The
sterilization bag is wrapped with the graphene sterilization substance 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.
Further, the mesh number of the high-defect graphene oxide screen is sequentially
increased along the liquid flow direction, and the mesh number of the laser-induced
graphene screen is sequentially increased along the liquid flow direction.
Further, the low-temperature sterilization unit further comprises a sterilization pool, and
the sterilization pool is located between the sterilization column and the collection device.
The graphene sterilization substance is placed inside the sterilization pool, and an
ultrasonic generator is arranged.
Further, the graphene sterilization substance in the sterilization bag is fluorinated
graphene oxide. The graphene sterilization substance in the sterilization pool is the
graphene composite sterilization substances. Specifically, the graphene composite
sterilization substance is any one or more of graphene oxide/silver nano particle
composite, graphene oxide quantum dots/silver nano particle composite, graphene
oxide/y-Fe203 nanocomposite, graphene oxide quantum dots/Fe304 composites, graphene
oxide/cuprous oxide nanocomposite, zinc oxide/graphene oxide composite. The
ultrasonic generator emits ultrasonic waves with a frequency of 20kHz-95kHz. The
sterilization bag uses fluorinated graphene oxide, which has the sterilization
characteristics of fluoride and graphene oxide, to increase the strength of sterilization.
Further, the sterilization column comprises a first sterilization column and a second
sterilization column. Several levels of high-defect graphene oxide screens are arranged
inside the first sterilization column and the sterilization bag and several levels of laser
induced graphene screens are arranged inside the second sterilization column, which are
sequentially the sterilization bag and several levels of laser-induced graphene screens
along the liquid flow direction. Valves are respectively arranged among the first
sterilization column, the second sterilization column, the sterilization pool and the
collection device.
Figure 1 is a structural schematic diagram of the low-temperature sterilization device for
liquid substances such as plant extracts based on graphene nano materials according to
the present invention.
Figure 2 shows the fluorinated graphene oxide used in the present invention, wherein Fig.
2a is a physical diagram of the fluorinated graphene oxide, and Fig. 2b is a transmission
electron microscope diagram of the fluorinated graphene oxide.
Figure 3 is a flow chart of the low-temperature sterilization of Fangchenggang Camellia
nitidissima extracts in Embodiment 2.
Figure 4 is a GC-MS detection result diagram of various amino acids in Fangchenggang
Camellia nitidissima extracts after being sterilized by the low-temperature sterilization
device for liquid substances such as plant extracts based on graphene nano materials of
the present invention.
Figure 5 is a graph of GC-MS detection results of various amino acids in Fangchenggang
Camellia nitidissima extracts sterilized by traditional high temperature sterilization
technology; wherein, the high temperature sterilization is carried out at 121°C for 30min.
The principle of the low-temperature sterilization method for liquid substances such as
plant extracts based on graphene nano materials is as follows. Graphene is a two
dimensional carbon nanomaterial, and the diameter of carbon atoms composing graphene
is very small, and the diameter of bacteria is between 0.5 and 5 microns. When bacteria in
liquid substances such as plant extracts contact with carbon atoms in graphene, bacterial
cells will be split by carbon atoms with smaller diameters, which leads to the death of bacteria and achieves the sterilization effect. At the same time, the ultrasonic wave with the frequency of 20KHz-95KHz vibrates very fast and contains high energy, which can disrupt the normal metabolism of bacteria and play the role of sterilization. Graphene sterilization substances and ultrasonic can kill bacteria at normal temperature without high temperature and high pressure by using their own properties, thus preventing the heat-labile substances in the liquid to be sterilized from being destroyed, and making the plant extracts to be sterilized still rich in various nutrients after sterilization.
Furthermore, graphene oxide has a smaller diameter than graphene, and the surface has a
plurality of irregular columnar or needle-like protrusions, which is more conducive to
breaking bacterial cells. Fluorinated graphene contains carbon-fluorine bonds, which can
release a small amount of fluoride ions. Fluorine ions can inhibit the synthesis of
polysaccharide and lipoteichoic acid, which are important components of bacterial cell
wall and cell membrane, so fluorine ions can inhibit the reproduction of bacteria, and the
higher the concentration of fluoride ions, the more the number of bacteria decreases.
Fluorinated graphene oxide has the advantages of both fluorinated graphene and graphene
oxide and has a stronger sterilization ability.
The low-temperature sterilization method for liquid substances such as plant extracts
based on graphene nano materials comprises the following steps.
Si. Enabling a liquid to be sterilized to flow through the graphene sterilization substances
to obtain sterilized liquid.
Wherein, the graphene sterilization substance is one or more of graphene oxide,
fluorinated graphene, fluorinated graphene oxide and graphene composite sterilization
substances. Specifically, the graphene composite sterilization substance is any one or more of graphene oxide/silver nano particle composite, graphene oxide quantum dots/silver nano particle composite, graphene oxide/y-Fe203 nanocomposite, graphene oxide quantum dots/Fe304 composites, graphene oxide/cuprous oxide nanocomposite, zinc oxide/graphene oxide composite.
S2. Storing the sterilized liquid.
Introducing the sterilized liquid into a collection device for storage.
In the low-temperature sterilization method for liquid substances such as plant extracts
based on graphene nano materials, if the liquid to be sterilized is Theaceae plant extract,
the Theaceae extract needs to be obtained by a low-temperature extraction method. The
low-temperature extraction method is any one of supercritical fluid technology,
subcritical extraction technology, molecular distillation technology and low-temperature
dissolved matter extraction technology.
The following describes the specific structure of the low-temperature sterilization device
for liquid substances such as plant extracts based on graphene nano materials of the
present invention. Please refer to Fig. 1, which is a structural schematic diagram of the
low-temperature sterilization device for liquid substances such as plant extracts based on
graphene nano materials according to the present invention. The low-temperature
sterilization device for liquid substances such as plant extracts based on graphene nano
materials of the present invention sequentially comprises a pumping valve (10), a low
temperature sterilization unit (20) and a collection device (30) from front to back. The
pumping 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 collection device
(30) is used for collecting and storing sterilized liquid.
The low-temperature sterilization unit (20) includes a first sterilization column (21), a
second sterilization column (22) and a sterilization pool (23). A first valve (24) is
arranged between the first sterilization column (21) and the second sterilization column
(22), a second valve (25) is arranged between the second sterilization column (22) and the
sterilization pool (23), and a third valve (26) is arranged between the sterilization pool
(23) and the collection device (30). The first valve (24), the second valve (25) and the
third valve (26) are responsible for controlling the liquid sterilized in the former part to
flow into the latter part, thus preventing the liquid from flowing into the next part after
insufficient sterilization in the previous part and preventing the liquid sterilized in the
next part from flowing back to the previous part.
The first sterilization column (21) is internally provided with a high-defect graphene
oxide screen (211) with 3-15 levels. The mesh number of the high-defect graphene oxide
screen (211) increases in turn along the direction of liquid flow, and the addition ratio of
high-defect graphene oxide in the high-defect graphene oxide screen is 5%-12.5%.
The second sterilization column (22) is filled with fluorinated graphene oxide (221), and
a 3-8-level laser-induced graphene screen (222) is arranged at the end close to the
sterilization pool (23). Please refer to Fig. 2, which is a picture of fluorinated graphene
oxide used in the present invention, wherein Fig. 2a is a physical picture of the
fluorinated graphene oxide, and Fig. 2b is a transmission electron microscope picture of
fluorinated graphene oxide. The fluorinated graphene oxide (221) is wrapped in
regenerated fibre cloth or glass fiber cloth with 100- 325 meshes, and the fluorine doping ratio in the fluorinated graphene oxide (221) is 0.25%-1.25%. The mesh number of the graphene sterilization grid (222) increases sequentially along the direction of liquid flow.
The sterilization pool (23) is filled with graphene sterilization substances (231) and
provided with an ultrasonic generator (232). The graphene sterilization substance (231) is
any one or more of graphene oxide/silver nano particle composite, graphene oxide
quantum dots/silver nano particle composite, graphene oxide/-Fe203 nanocomposite,
graphene oxide quantum dots/Fe304 composites, graphene oxide/cuprous oxide
nanocomposite, zinc oxide/graphene oxide composite. The frequency of the ultrasonic
waves generated by the ultrasonic generator (232) is 20Kz-95KHz, and the working
time is 15-30min.
The materials of the first sterilization column, the second sterilization column, the high
defect graphene oxide screen, the laser-induced graphene screen and the sterilization pool
are one of stainless steel, ceramics, glass, poly(vinylidene fluoride), poly tetra
fluoroethylene and poly(ether-ether-ketone). The pump in the pumping valve can be one
of peristaltic pump, plunger pump or 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 screen is provided with a protrusion device matched with the
longitudinal groove of the inner wall of the second sterilization column, which is
convenient for replacement and cleaning. The size of that high-defect graphene oxide
screen is match with the inner diameter of the first sterilization column, and the edge is
provided with a protrusion device matched with the longitudinal groove of the inner wall
of the first sterilization column, so that replacement and cleaning are convenient. In
addition, the high-defect graphene oxide screen can be prepared by directly forming a high-defect graphene oxide coating with a thickness of 0.01-0.8 m on screens with relevant sizes. The laser-induced graphene screen is prepared by forming a coating with a thickness of 0.01-0.8 m by coating laser-induced graphene nano materials on screens with relevant sizes. Specifically, the preparation method of the laser-induced graphene nano materials is as follows. Soaking 6H-SiC silicon carbide wafer in acetone, ultrasonicating for 15min to remove surface organic residues, and then irradiating the sample with a xenon chloride excimer laser with a wavelength of 308nm for 60 nanoseconds, wherein, the specific parameters of xenon chloride excimer laser are single pulse energy density 1.08J/cm 2, frequency 5Hz, pulse count 60, defocusing amount 3cm2
, facula area 0.45 cm2 and mask area 8mm2 . After laser irradiation, two layers of materials
are obtained, wherein the upper layer is polysilicon layer and the lower layer is laser
induced graphene layer. Then, 193nm argon-fluorine laser or (248nm krypton-fluorine
laser is irradiated for 60 nanoseconds, in which the frequency is 9Hz and the pulse count
is 60. Performing laser irradiation again to cause the silicon to sublimate, leaving only the
laser-induced graphene nano materials.
The application method of the device for low-temperature sterilization of liquid
substances such as plant extracts based on graphene nano materials of the present
invention is as follows. The liquid to be sterilized is pumped into the first sterilization
column (21) by using the pumping valve (10), and the liquid to be sterilized sequentially
flows through several levels of high-defect graphene oxide screens (211) inside the first
sterilization column (21) for the first sterilization to obtain the first sterilized liquid. The
first sterilized liquid flows into the second sterilization column (22) through the first
valve (24), and then flows through the fluorinated graphene oxide (221) and the 3-8-level graphene sterilization grid (222) for secondary sterilization to obtain the second sterilized liquid. The liquid after secondary sterilization flows into the sterilization pool (23) through the second valve (25) and further flows through the graphene sterilization substances (231) and is sterilized for 15-30min by ultrasonic at 20KHz-95KHz to obtain the liquid after tertiary sterilization. The liquid sterilized for the third time is guided into the collection device through the third valve (26) and the guide pipe, and inert gas is introduced for seal and store.
The low-temperature sterilization device for liquid substances such as plant extracts
based on graphene nano materials of the present invention also has various variations. For
example, the sterilization screen is not limited to the shape of the screen but can also be a
structure with meshes such as a sterilization grid and a sterilization permeable membrane.
The sterilization screen is not only a high-defect graphene oxide screen and a laser
induced graphene screen, but also a fluorinated graphene screen and the like. The level
number of the high-defect graphene oxide screen can be any level, more than 3-15 levels.
Similarly, the number of levels of the laser-induced graphene screen can be any level, not
only 3-8 levels.
Embodiment 1
In this embodiment, taking Fangchenggang Camellia nitidissima as an example, the low
temperature sterilization method for liquid substances such as Fangchenggang Camellia
nitidissima Chi extracts based on graphene nano materials and the use method of the
device are specifically explained. Please refer to Fig. 3, which is a flow chart of low
temperature sterilization of Fangchenggang Camellia nitidissima extracts based on
graphene nano materials in this embodiment.
Pretreatment
The flowers of Fangchenggang Camellia nitidissima Chi are cleaned, crushed and
ground, and then extracted by supercritical C02 low temperature extraction process to
obtain the flower extracts of Camellia nitidissima Chi waiting for sterilization.
Si. Carrying out low-temperature sterilization on liquid to be sterilized by graphene
sterilization substances and ultrasonic waves to obtain sterilized liquid
Introducing the pretreated extracts to be sterilized into the pumping valve (10), which
pumps the extracts to be sterilized into the first sterilization column (21), and the extracts
to be sterilized sequentially flows through the eight-level high-defect graphene oxide
screen (211) made of poly tetra fluoroethylene inside the first sterilization column (21) to
obtain the first sterilized Camellia nitidissima Chi extracts, wherein the grid mesh
numbers of the eight-level high-defect graphene oxide screen are 20 meshes, 60 meshes,
170 meshes, 400 meshes, 650 meshes, 1100 meshes and 200 meshes from front to back.
The addition proportion of high-defect graphene oxide in the high defect graphene oxide
screen is 6%. The first valve (24) is opened, and the once sterilized flower extracts of
Camellia nitidissima Chi enters a second sterilization column (22) made of ceramic
material to further inactivate the residual bacteria in the extracts. In the second
sterilization column (22), the extract first flows through fluorinated graphene oxide (221)
wrapped by glass fiber cloth with mesh number of 170 meshes, and the fluorine doping
ratio of the fluorinated graphene oxide is 1.1%. Then the extract flows through a five
level laser-induced graphene sterilization grid (222) to obtain the twice sterilized flower
extracts of Camellia nitidissima Chi. And the grid meshes of the five-level laser-induced
graphene sterilization grid are 10 meshes, 35 meshes, 100 meshes, 200 meshes and 325 meshes from front to back in turn. Opening the second valve (25), the twice sterilized flower extract of Camellia nitidissima Chi flows into the sterilization pool (23) filled with graphene oxide/silver nano particle composite as graphene sterilization substance (231), and at the same time, the ultrasonic generator in the sterilization pool (23) emits ultrasonic wave with frequency of 60KHz to assist sterilization for 20min, thus obtaining the third sterilized flower extracts of Camellia nitidissima Chi.
S2. Storing sterilized liquid.
Open the third valve (26), so that the flower extracts of Camellia nitidissima Chi, which
is sterilized by the sterilization pool (23) and sterilized for three times, is guided into the
collection device (30) through the pipeline, filled with inert gas, and then sealed and
stored for subsequent product development and production.
The eight-level high-defect graphene oxide sterilization screen (211) in this embodiment
can be prepared by directly forming a high-defect graphene oxide coating with a
thickness of 0.1 m on screens of relevant sizes, while the high-defect graphene oxide
coating level is prepared by hydrogen plasma acting on graphene oxide, and graphene
oxide is obtained by Hummers method. The laser-induced graphene sterilization grid
(222) is prepared by using silver oxide-laser-induced graphene nanocomposite to form a
0.08km nano coating on the ceramic surface.
Effect detection
The Camellia nitidissima Chi extract obtained by pretreatment is evenly divided into two
groups, wherein one group is subjected to low-temperature sterilization by the low
temperature sterilization device for liquid substances such as plant extracts based on
graphene nano materials; the other group is subjected to traditional high temperature sterilization technology (treatment at 121°C for 30min) for high temperature sterilization.
Then, CC-MS is used to detect amino acids in the sterilized extracts of Camellia
nitidissima Chi.
Please refer to Fig. 4, which is a GC-MS detection result diagram of various amino acids
in Camellia nitidissima Chi extracts after being sterilized by the low-temperature
sterilization device of plant extracts and other liquid substances based on graphene nano
materials of the present invention. It can be seen from Fig. 4 that 17 kinds of amino acid
active ingredients including Ala, Gly, Thr, Ser, Val, Leu, Ile, Cys, Pro, Met, Asp, Phe,
Glu, Lys, Tyr, His and Arg can be detected from the sterilized Camellia nitidissima Chi
extracts after low-temperature sterilization by using the graphene nanotechnology-based
low-temperature sterilization device of the present invention, wherein Thr, Val, Leu, Ile,
Met, Phe and Lys are seven human essential amino acids (EAAs).
Please refer to Fig. 5, which is the GC-MS detection result of various amino acids in
Camellia nitidissima Chi extracts after being sterilized by traditional high temperature
sterilization technology (treated at 121°C for 30min). It can be seen from Fig. 5 that 14
kinds of amino acid active ingredients, including Ala, Gly, Thr, Ser, Val, Leu, Ile, Pro,
Asp, Phe, Glu, Lys, His and Arg can be detected from the sterilized Camellia nitidissima
Chi extracts after high temperature sterilization by traditional high temperature
sterilization technology. Wherein, there are six EAAs of Thr, Val, Leu, Ile, Phe and Lys.
Compared with Fig 4, Cys, Met and Tyr are missing, indicating that these three amino
acids are completely destroyed after high temperature sterilization. The peak values of the
remaining 14 amino acids are relatively low, which indicates that these 14 amino acids
also had partial degradation loss after high temperature sterilization. At the same time, there are many impurity peaks in Fig. 5, which are presumed to be the decomposition of nutritional components of amino acids destroyed by heat into other non-nutritional components.
It can be seen that, compared with the traditional high-temperature sterilization
technology, the low-temperature sterilization technology based on graphene
nanomaterials can more effectively preserve the nutrient components in liquid species
from decomposition, so that liquid substances have richer nutrition.
Embodiment 2
In this embodiment, taking Camellia fascicularis as an example, the low-temperature
sterilization method for liquid substances such as Camelliafascicularisextracts based on
graphene nano materials and the use method of the device are specifically explained.
Pretreatment
The leaves of Camelliafascicularis are cleaned, crushed and ground, and then extracted
by molecular distillation extraction process to obtain the leaf extracts of Camellia
fasciculariswaiting for sterilization.
Si. Carrying out low-temperature sterilization on liquid to be sterilized by sterilization
substances and ultrasonic waves to obtain sterilized liquid
Introducing the pretreated extracts to be sterilized into the pumping valve (10), which
pumps the extracts to be sterilized into the first sterilization column (21) made of ceramic
material, and the extracts to be sterilized sequentially flows through the six-level high
defect graphene oxide screen (211) made of poly(ether-ether-ketone) inside the first
sterilization column (21) to obtain the first sterilized Camelliafascicularis extracts,
wherein the grid mesh numbers of the six-level high-defect graphene oxide screen are 50 meshes, 120 meshes, 325 meshes, 540 meshes, 900 meshes and 1600 meshes from front to back. The addition proportion of high-defect graphene oxide in the high defect graphene oxide screen is 10%. The first valve (24) is opened, and the once sterilized leaf extracts of Camellia fascicularis enter a second sterilization column (22) made of ceramic material to further inactivate the residual bacteria in the extracts. In the second sterilization column (22), the extract first flows through fluorinated graphene oxide (221) wrapped by glass fiber cloth with mesh number of 120 meshes, and the fluorine doping ratio of the fluorinated graphene oxide is 0.5%. Then the extract flows through a four level laser-induced graphene sterilization grid (222) to obtain the twice sterilized leaf extracts of Camellia fascicularis. And the grid meshes of the four-level laser-induced graphene sterilization grid can be 20 meshes, 80 meshes, 170 meshes and 400 meshes from front to back in turn. Opening the second valve (25), the twice sterilized leaf extract of Camellia fascicularis flows into the sterilization pool (23) filled with graphene oxide/y-Fe203 nanocomposite as graphene sterilization substance (231), and at the same time, the ultrasonic generator in the sterilization pool (23) emits ultrasonic wave with frequency of 45KHz to assist sterilization for 30min, thus obtaining the third sterilized leaf extracts of Camelliafascicularis.
S2. Storing sterilized liquid.
Open the third valve (26), so that the leaf extracts of Camelliafascicularis , which is
sterilized by the sterilization pool (23) and sterilized for three times, is guided into the
collection device (30) through the pipeline, filled with inert gas, and then sealed and
stored for subsequent product development and production.
The six-level high-defect graphene oxide sterilization screen (211) in this embodiment
can be prepared by directly forming a high-defect graphene oxide coating with a
thickness of 0.02tm on screens of relevant sizes. And the high-defect graphene oxide is
obtained by the action of excessive strong oxides (KMnO4, H2SO4, H202, etc.) on
graphene oxide, while the graphene oxide is obtained by improved Hummers method.
The laser-induced graphene sterilization grid (222) is prepared by zinc oxide-laser
induced graphene nanocomposite to form a 0.05tm nano coating on the surface of
poly(ether-ether-ketone) polymer materials.
In addition to the Camelliafascicularisin this embodiment and Fangchenggang Camellia
nitidissima in the Embodiment 1, it can also be Camellia euphlebia, Camellia
longruiensis, Camellia tunghinensis, Camellia microcarpa and its varieties, Camellia
achrysantha, Camellia pubipetala, Camellia impressinervis, Camellia leptopetala,
Camellia parvipetala, Camellia ptilosperma, Camellia multipetala, Camellia multipetala
S. Y. Liang et C. Z. Deng, Camellia limonia, Camellia flava (Pitard) Sealy, Camellia
chrysanthoides, Camellia xiashiensis Liang, Camellia nitidissima form. longistyla,
Camellia long-zhouensis, Camellia wumingensis, Canlellia pingguoensis, Camellia
pinggaoensis Fang var. terminalis S.Y.Liang, Camellia micrantha, Camellia
longgangensis, Camellia parvifolia, Camellia fusuiensis, Camellia tianeensis, Camellia
favida Chang var. polypetala (Li et He)S. Y. Lang, Camellia flavida, Camellia
fascicularis Chang, Camellia multipetala Lianget Deng var. patens (Liang et Mo)S.Y.
Liang, Camellia bobaiensis , Camellia aurea Chang, Camelliagrandis (Lianget Mo)
Chang et S. Y. Liang, Camellia szechuanensis S.Y.Liang et Y.C.Yang, Camellia huana
T. L. Ming et W. J. Zhang, Camelliafascicularis, Camellia liberofilamenta Chang et C.
H. Yang, Camellia vietnam tonkinensis, Camellia amplexicaulis, Camellia
cucphuongensis, Camellia crassiphylla, Camellia tamdaoensis, Camellia Hu longus and
Camellia Luteopallida (T.Q.T.Nguyen&Luu), Camellia bugiamapensis
(Orel,Curry,Luu&Q.D.)andCamelliacapitata(Orel,Curry&Luu,sp.nov.).
Embodiment 3
In this embodiment, taking Luokeng Alpine ancient tree tea as an example, the low
temperature sterilization method for liquid substances such as Luokeng Alpine ancient
tree tea extracts based on graphene nano materials and the use method of the device are
specifically explained.
Pretreatment
The leaves of Luokeng Alpine ancient tree tea are cleaned, crushed and ground, and then
extracted by molecular distillation extraction process to obtain the leaf extracts of
Luokeng Alpine ancient tree tea waiting for sterilization.
Si. Carrying out low-temperature sterilization on liquid to be sterilized by sterilization
substances and ultrasonic waves to obtain sterilized liquid
Introducing the pretreated extracts to be sterilized into the pumping valve (10), which
pumps the extracts to be sterilized into the first sterilization column (21) made of
stainless steel, and the extracts to be sterilized sequentially flows through the seven-level
high-defect graphene oxide screen (211) made of poly(vinylidene fluoride) inside the first
sterilization column (21) to obtain the first sterilized Luokeng Alpine ancient tree tea
extracts, wherein the grid mesh numbers of the six-level high-defect graphene oxide
screen are 20 meshes, 60 meshes, 150 meshes, 325 meshes, 650 meshes 1100 meshes and
2000 meshes from front to back. The addition proportion of high-defect graphene oxide in the high defect graphene oxide screen is 12.5%. The first valve (24) is opened, and the once sterilized leaf extracts of Luokeng Alpine ancient tree tea enter a second sterilization column (22) made of tempered glass to further inactivate the residual bacteria in the extracts. In the second sterilization column (22), the extract first flows through fluorinated graphene oxide (221) wrapped by glass fiber cloth with mesh number of 120 meshes, and the fluorine doping ratio of the fluorinated graphene oxide is 0.75%. Then the extract flows through a four-level laser-induced graphene sterilization grid (222) to obtain the twice sterilized leaf extracts of Luokeng Alpine ancient tree tea. And the grid meshes of the four-level laser-induced graphene sterilization grid can be 50 meshes, 200 meshes, 325 meshes and 650 meshes from front to back in turn. Opening the second valve (25), the twice sterilized leaf extract of Luokeng Alpine ancient tree tea flows into the sterilization pool (23) filled with graphene oxide/Fe304 nanocomposite as graphene sterilization substance (231), and at the same time, the ultrasonic generator in the sterilization pool (23) emits ultrasonic wave with frequency of 45KHz to assist sterilization for 10min, thus obtaining the third sterilized leaf extracts of Luokeng Alpine ancient tree tea.
S2. Storing sterilized liquid.
Open the third valve (26), so that the leaf extracts of Luokeng Alpine ancient tree tea ,
which is sterilized by the sterilization pool (23) and sterilized for three times, is guided
into the collection device (30) through the pipeline, filled with inert gas, and then sealed
and stored for subsequent product development and production.
The six-level high-defect graphene oxide sterilization screen (211) in this embodiment
can be prepared by directly forming a high-defect graphene oxide coating with a thickness of 0.35um on screens of relevant sizes. And the high-defect graphene oxide is obtained by three-dimensional assembly of graphene. The laser-induced graphene sterilization grid (222) is prepared by zinc oxide-laser-induced graphene nanocomposite to form a 0.015m nano coating on the ceramic surface.
In addition to Luokeng Alpine ancient tree tea in this embodiment, it can also be
Biluochun Tea, Xinyang Maojian Tea, West Lake Longjing Tea, Junshan Yinzhen Tea,
Huangshan Maofeng Tea, Wuyi Rock Tea, Keemun Black Tea, Duyun Maojian Tea,
Tieguanyin, Lu'an Guapian Tea, Fenghuang Dancong, Luokeng Ancient Tree Tea,
Lushan Yunwu Tea, Yingde Black Tea, Lingyun Pekoe Tea, Anhua Black Tea, Yunnan
Pu-erh Tea and Wuyi Dahongpao Tea, Fujian Yinzhen Tea and Suzhou Jasmine Tea and
so on.
Compared with the prior art, the method for low-temperature sterilization of liquid
substances such as plant extracts based on graphene nano materials in the invention uses
graphene oxide, fluorinated graphene and fluorinated graphene oxide with stronger
sterilization function after improvement to perform liquid sterilization together with
ultrasonic waves, so that the sterilization of liquid substances such as plant extracts can
be efficiently completed at normal temperature without high temperature, thus avoiding
the degradation of heat-labile substances in the liquid, thereby maximally retaining
nutritional or medicinal effective components in the liquid substances such as plant
extracts. Meanwhile, the low-temperature sterilization device for liquid substances such
as plant extracts based on graphene nano materials has simple overall structure, simple
and easy manufacturing, installation and operation, and is easy to popularize.
The above is only a preferred embodiment of the present invention, and is not intended to
limit the present invention. Any modifications, equivalent substitutions and
improvements made within the spirit and principles of the present invention should be
included in the protection scope of the present invention.
Claims (10)
1. A low-temperature sterilization method for liquid substances such as Theaceae plant
extracts based on graphene nano materials, characterized in that it comprises the
following steps of enabling liquid waiting for sterilization to flow through graphene
sterilization substances to obtain sterilized liquid and store the sterilized liquid.
Wherein, the graphene sterilization substance is one or more of graphene oxide,
fluorinated graphene, fluorinated graphene oxide and functionalized graphene
nanocomposite sterilization substances. Specifically, the graphene composite sterilization
substance is any one or more of graphene oxide/silver nano particle composite, graphene
oxide quantum dots/silver nano particle composite, graphene oxide/y-Fe203
nanocomposite, graphene oxide quantum dots/Fe304 composites, graphene oxide/cuprous
oxide nanocomposite, zinc oxide/graphene oxide composite.
2. The low-temperature sterilization method for liquid substances such as Theaceae plant
extracts based on graphene nano materials as stated in Claim 1, characterized in that the
liquid to be sterilized is also sterilized by ultrasonic waves with a frequency of 20KHz
KHz.
3. A low-temperature sterilization device for liquid substances such as Theaceae plant
extracts based on graphene nano materials, characterized by comprising a pumping valve,
a low-temperature sterilization unit and a collection device. The pumping valve presses
the liquid to be sterilized into the low-temperature sterilization unit; the low-temperature
sterilization unit performs low-temperature sterilization on the liquid to be sterilized to
obtain sterilized liquid; the collection device collects and stores sterilized liquid; the
low-temperature sterilization unit is provided with graphene sterilization substances.
Wherein, the graphene sterilization substance is one or more of graphene oxide,
fluorinated graphene, fluorinated graphene oxide and graphene composite sterilization
substances. Specifically, the graphene composite sterilization substance is any one or
more of graphene oxide/silver nano particle composite, graphene oxide quantum
dots/silver nano particle composite, graphene oxide/y-Fe203 nanocomposite, graphene
oxide quantum dots/Fe304 composites, graphene oxide/cuprous oxide nanocomposite,
zinc oxide/graphene oxide composite.
4. The low-temperature sterilization device for liquid substances such as plant extracts
based on graphene nano materials as stated in Claim 3, characterized in that the low
temperature sterilization unit comprises a sterilization column, and several levels of
sterilization screens are arranged inside the sterilization column along the liquid flow
direction, and the surface of the sterilization screen is coated with the graphene
sterilization substance.
5. The low-temperature sterilization device for liquid substances such as Theaceae plant
extracts based on graphene nano materials as stated in Claim 4, characterized in that a
sterilization bag is also arranged inside the sterilization column, and the sterilization bag
is located between the sterilization screens at adjacent levels. The sterilization bag is
wrapped with the graphene sterilization substance, and meshes are arranged on the
sterilization bag.
6. The low-temperature sterilization device for liquid substances such as Theaceae plant
extracts based on graphene nano materials as stated in Claim 4, characterized in that the
sterilization screen is a high-defect graphene oxide screen and/or a laser-induced
graphene screen.
7. The low-temperature sterilization device for liquid substances such as Theaceae plant
extracts based on graphene nano materials as stated in Claim 6, characterized in that the
mesh number of the high-defect graphene oxide screen is sequentially increased along the
liquid flow direction, and the mesh number of the laser-induced graphene screen is
sequentially increased along the liquid flow direction.
8. The low-temperature sterilization device for liquid substances such as Theaceae plant
extracts based on graphene nano materials as stated in any one of Claim 6 or 7,
characterized in that the low-temperature sterilization unit further comprises a
sterilization pool, and the sterilization pool is located between the sterilization column
and the collection device. The graphene sterilization substance is placed inside the
sterilization pool, and an ultrasonic generator is arranged.
9. The low-temperature sterilization device for liquid substances such as Theaceae plant
extracts based on graphene nano materials as stated in Claim 8, characterized in that the
graphene sterilization substance in the sterilization bag is fluorinated graphene oxide. The
graphene sterilization substance in the sterilization pool is the graphene composite
sterilization substances. Specifically, the graphene composite sterilization substance is
any one or more of graphene oxide/silver nano particle composite, graphene oxide
quantum dots/silver nano particle composite, graphene oxide/-Fe203 nanocomposite,
graphene oxide quantum dots/Fe304 composites, graphene oxide/cuprous oxide
nanocomposite, zinc oxide/graphene oxide composite. The ultrasonic generator emits
ultrasonic waves with a frequency of 20kHz-95kHz.
10. The low-temperature sterilization device for liquid substances such as Theaceae plant
extracts based on graphene nano materials as stated in Claim 9, characterized in that the sterilization column comprises a first sterilization column and a second sterilization column. Several levels of high-defect graphene oxide screens are arranged inside the first sterilization column and the sterilization bag and several levels of laser-induced graphene screens are arranged inside the second sterilization column, which are sequentially the sterilization bag and several levels of laser-induced graphene screens along the liquid flow direction. Valves are respectively arranged among the first sterilization column, the second sterilization column, the sterilization pool and the collection device.
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