CN112125374A - Method and device for preserving plasma activated water and method for preparing finished product - Google Patents
Method and device for preserving plasma activated water and method for preparing finished product Download PDFInfo
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- CN112125374A CN112125374A CN202010980261.XA CN202010980261A CN112125374A CN 112125374 A CN112125374 A CN 112125374A CN 202010980261 A CN202010980261 A CN 202010980261A CN 112125374 A CN112125374 A CN 112125374A
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- plasma
- activated water
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/4608—Treatment of water, waste water, or sewage by electrochemical methods using electrical discharges
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/22—Treatment of water, waste water, or sewage by freezing
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
Abstract
The invention provides a method and a device for preserving plasma activated water and a method for preparing a finished product. The preparation method of the plasma activated water finished product comprises the following steps: step 1) generating atmospheric pressure low-temperature plasma by using a plasma generation module with a surface discharge structure, and diffusing the plasma into a solution to be treated to form plasma activated water; the plasma generation module, the discharge gas and the solution to be treated are all in an environment lower than room temperature; and 2) rapidly cooling the formed plasma activated water by using liquid nitrogen to convert the plasma activated water into a frozen state, and storing the plasma activated water in a liquid nitrogen environment. The invention rapidly reduces the temperature of the activated water prepared in a low-temperature environment to-196 ℃ by using liquid nitrogen to form plasma activated ice (solid state), so that the short-life particles of the plasma activated water can maintain higher concentration for a longer time.
Description
Technical Field
The invention relates to the technical field of plasma, in particular to a preservation method of plasma activated water and a preparation method of a finished product.
Background
The atmospheric pressure low-temperature plasma activated water is activated water with low pH value and high oxidation-reduction potential, which is obtained by treating an aqueous solution by an atmospheric pressure low-temperature plasma device. The plasma generates a large amount of neutral reactive species, e.g., H, O, O, in the gas phase3、OH、NO、NO2、N2O、H2O2、N2O5When these gas phase particles come into contact with water, various liquid phase active particles containing hydrogen peroxide, superoxide anion, hydroxyl radical, NO radical, peroxynitrous acid, etc. are generated in the liquid phase, and the liquid phase active particles participate in numerous biochemical reactions, are indispensable participants in physiological processes, and have biomedical effects such as anticancer and sterilization. The active particles can effectively kill various microorganisms such as bacteria, fungi, viruses and the like; in the treatment of cancer, the plasma activating fluid can selectively induce apoptosis of cancer cells without destroying normal cell growth.
But because the life of the free radicals is short, the free radicals disappear in a certain time, so that the action effect of the plasma activated water is obviously weakened or even disappears along with the prolonging of the standing time. This phenomenon greatly affects the use of plasma activated water. Therefore, how to improve the survival life of the active radical particles in the plasma activated water, improve the storage time and develop efficient plasma activated water is one of the difficulties and hotspots of the current research.
Currently, researchers also propose that activated water can be obtained by performing plasma discharge in a temperature environment lower than room temperature, and the activated water can maintain a high active radical particle concentration in a short time; however, there is still a significant drop after one or two hours, and even if the addition of antifreeze continues to maintain or reduce the activated water to around 0 degrees, the half-life is usually no longer than 5 hours.
Disclosure of Invention
The purpose of the present invention is to improve the survival life of active radical particles in plasma-activated water, to improve the storage time, and to develop highly efficient plasma-activated water.
In order to achieve the above purpose, the invention provides the following technical scheme:
a preparation method of a finished product of plasma activated water comprises the following steps:
step 1) generating atmospheric pressure low-temperature plasma by using a plasma generation module with a surface discharge structure, and diffusing the plasma into a solution to be treated to form plasma activated water; the plasma generation module, the discharge gas and the solution to be treated are all in an environment lower than room temperature;
and 2) rapidly cooling the formed plasma activated water by using liquid nitrogen to convert the plasma activated water into a frozen state, and storing the plasma activated water in a liquid nitrogen environment.
Optionally, in the step 1), the ambient temperature of the plasma generation module, the discharge gas and the solution to be treated is controlled to be-25 ℃ to 10 ℃ all the time. Wherein the temperature can be reduced to below 0 ℃ by adding a small amount of antifreeze solution.
Alternatively, in step 2), the formed plasma activated water is transferred to a sealed container and then immediately placed in an insulated enclosure filled with liquid nitrogen.
Optionally, the solution to be treated is deionized water, ultrapure water, double distilled water, a NaOH solution, or ultrapure water containing ethanol.
A system for preparing plasma activated water comprises a high-voltage power supply, a cold plasma generation module adopting a creeping discharge structure and an activation liquid container containing a solution to be treated; the cold plasma generation module comprises an insulating dielectric plate for dielectric barrier discharge, a high-voltage electrode and a ground electrode with a grid structure, wherein the ground electrode is used as a cold plasma generation interface for creeping discharge, and a gas gap is formed between the ground electrode and the activation liquid container; the positive output end and the negative output end of the high-voltage power supply are respectively connected with a high-voltage electrode and a ground electrode of the cold plasma generation module, and the cold plasma is generated by exciting the cold plasma generation module to process the solution to be processed; it is characterized in that: the device also comprises a temperature adjusting device and a gas cooling pipe; the output end of the gas cooling pipe is positioned in the gas gap and used for introducing cooling gas; the temperature adjusting device is provided with an accommodating space, and the cold plasma generating module and the activating liquid container are both arranged in the accommodating space of the temperature adjusting device, so that the environment temperature is lower than the room temperature.
Optionally, the system further comprises a discharge space shell, the activating liquid container is fixedly arranged at the bottom inside the discharge space shell, and the cold plasma generating module is detachably, hermetically and fixedly covered at the upper end of the discharge space shell so that the discharge space is isolated from the outside air; the input end of the gas cooling pipe is connected with the working gas storage bottle, and the output end of the gas cooling pipe is connected with one side of the discharge space shell; the other side of the discharge space housing is used for discharging waste gas through an exhaust pipe, and an air valve is arranged on the exhaust pipe.
Here, the detachable sealing and fixing form is, for example, that a sealing ring is arranged at an upper end of the discharge space housing in a circle corresponding to a lower surface of the insulating medium plate of the cold plasma generation module near the edge, and the cold plasma generation module can be detachably sealed and fixed by pressing the sealing ring by self weight.
Optionally, the temperature adjusting device adopts a contact refrigerator, a groove is arranged on the upper surface of the temperature adjusting device to form the accommodating space, and cooling liquid is filled in the groove; the gas cooling tube has a portion bent and immersed in the cooling liquid, and the lower portion of the discharge space housing is also immersed in the cooling liquid.
Optionally, a temperature monitor (e.g., a thermocouple) is disposed within the cavity of the discharge space housing for feedback regulation of refrigeration during operation.
In addition, the cold plasma generation module can be formed by connecting one or more creeping discharge components in parallel; the high-voltage power supply adopts a high-voltage sine power supply or a high-voltage pulse power supply; the temperature adjusting device can also use an ice block cooling or air cooling radiator singly or in combination; the gas cooling tubes and other cooling system tubes may be embodied as helically wound metal tubing.
A method for preserving plasma activated water comprises rapidly cooling the plasma activated water with liquid nitrogen to obtain frozen state, and storing in liquid nitrogen environment.
The plasma activated water storage device comprises a heat preservation shell and a sealed container, wherein the sealed container is used for hermetically storing plasma activated water, liquid nitrogen is filled in the heat preservation shell, and the sealed container is completely placed in the liquid nitrogen environment.
The invention has the following beneficial effects:
the active particles can be greatly reduced in attenuation speed in the cooling process after the reaction is finished by rapidly cooling the prepared active water to-196 ℃ by using liquid nitrogen to form plasma activated ice (solid state). Under the same discharge conditions, the prepared plasma activated water can be stored in liquid nitrogen at-196 ℃ for a longer time, and the particle concentration is still kept at a considerable level within about 24 h.
In the preparation process, heat exchange between the outside air and the discharge space is avoided as much as possible, and the working gas, the discharge device and the activation liquid are all subjected to cooling treatment, so that the quenching rate of active free radicals generated by plasma activation in the solution is greatly reduced, and higher particle concentration is maintained; meanwhile, the reaction rate of a metal electrode and oxygen in the plasma discharge device is reduced, the insulating medium layer is prevented from being deformed due to heat accumulated in the discharge process, the service life of the device can be obviously prolonged, and the discharge form of the plasma device is more stable.
The half-life period of the short-life particles of the plasma activated water is prolonged by 15-50 times compared with that of the short-life particles of the plasma activated water stored at room temperature, so that the short-life particles of the plasma activated water can still maintain higher concentration within 24 hours.
Drawings
Fig. 1 is a schematic structural view of a system for preparing plasma-activated water according to an embodiment of the present invention. In the figure, 1-high voltage power supply; 2-a cold plasma generation module; 201-ground electrode; 3-activating liquid container; 4-a discharge space housing; 5-a temperature regulating device; 6-cooling liquid; 7-gas cooling pipes; 8-a thermocouple; 9-a thermometer; 10-an oscilloscope; 11-a high voltage probe; 12-Current Probe.
FIG. 2 is a statistical graph of the change in the concentration of short-lived reactive species in plasma-activated water generated at room temperature (25 ℃) under different storage temperature conditions.
FIG. 3 is a statistical graph of the change in the concentration of short-lived active species in plasma-activated water generated at low temperature (10 ℃ C.) under different storage temperature conditions.
Detailed Description
The present application will be described in further detail below by way of examples with reference to the accompanying drawings. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
As shown in fig. 1, a cold plasma generation module 2 adopting a creeping discharge structure is assembled with an activation liquid container 3 containing a solution to be treated, and a cold plasma generation interface is formed and has a gas gap; the high-voltage electrode and the ground electrode are respectively connected to two sides of the insulating dielectric plate to form the cold plasma generation module for dielectric barrier discharge. Generally, air is used as a discharge gas (working gas) to generate ozone, hydrogen peroxide, nitric acid and nitrous acid particles, but other common plasma working gases can also be adopted; the solution to be treated is deionized water, ultrapure water, double distilled water, NaOH solution or ultrapure water containing ethanol.
The distance between the solution to be treated and the atmospheric pressure cold plasma generation module can be properly adjusted, and is preferably 12 mm.
The material of the dielectric barrier discharge insulating dielectric plate can be selected according to the requirement, and the embodiment adopts an epoxy resin material.
The power supply of the atmospheric pressure cold plasma generation module can select a high-voltage sine power supply or a high-voltage pulse power supply.
The atmospheric pressure cold plasma generation module can be formed by connecting one or more creeping discharge assemblies in parallel.
The activating liquid container 3 is fixedly arranged at the bottom in a discharge space shell 4, and the cold plasma generating module 2 is detachably, hermetically and fixedly covered at the upper end of the discharge space shell 4, so that the discharge space is isolated from the outside air; the input end of the gas cooling pipe 7 is connected with the working gas storage bottle, and the output end is connected with one side of the discharge space shell; the other side of the discharge space housing is used for discharging waste gas through an exhaust pipe, and an air valve is arranged on the exhaust pipe. The temperature adjusting device 5 adopts a contact refrigerator, a groove is arranged on the upper surface of the temperature adjusting device to form an accommodating space, and cooling liquid 6 is filled in the groove; the gas cooling tube has a portion bent and immersed in the cooling liquid, and the lower portion of the discharge space housing is also immersed in the cooling liquid. Different environmental temperatures can be adjusted through the operation panel of the temperature adjusting device.
Starting the high-voltage power supply 1, opening the working gas storage cylinder, cooling the working gas, and then feeding the working gas into the discharge space, wherein under the excitation of the high-voltage power supply, the plasma generating module generates plasma on the surface of one side of the ground electrode 201, so that the solution to be treated is indirectly treated, and plasma activated water is obtained.
In order to ensure the cooling effect of the device, a temperature monitor (such as a thermocouple 8) is arranged in the device, the temperature of the discharge space and the temperature of the plasma activated water are monitored in real time, and the temperature adjusting device carries out corresponding feedback adjustment according to the temperature monitor, so that the stability of the temperature of the discharge space and the temperature of the plasma activated water is ensured.
After the plasma activation is finished, the activated water is transferred into a storage vessel (a sealed container) from an activated liquid container, then liquid nitrogen is rapidly frozen and cooled, the temperature of the liquid nitrogen is lowered to-196 ℃ under normal pressure, and the plasma activated solution is stored in the liquid nitrogen in a sealed manner. The sealed container can be prepared into different shapes, and is convenient for storing and transporting activated ice made of activated water. The transfer process should also be as rapid as possible, and the specific transfer method is not limited, for example, the activating liquid container can be directly taken out from the discharge space housing, the activating water in the activating liquid container can be poured into the sealed container, or a suction pipe can be additionally arranged to be inserted into the activating liquid container through the side wall of the discharge space housing, so that the activating water can be directly taken out and transferred into the sealed container without removing the cold plasma generation module at the upper end of the discharge space housing.
After the discharge is finished, if the temperature is reduced at normal temperature or slowly, active particles with biological effect in the plasma activation solution are attenuated quickly, and the short-life active free radicals in the solution can be preserved to the maximum extent by utilizing the quick temperature reduction of liquid nitrogen. The method can prolong the half-life of the active particles with short service life by 15-50 times, and can prolong the half-life to nearly 24 hours at most.
Example one
The discharge device activates the deionized water at room temperature (25 ℃) for 3 min. After the discharge is finished, the activated water is quickly subpackaged and stored under different temperature conditions. The results of the short-lived active particle concentration after thawing to room temperature before detection are shown in FIG. 2. It can be seen that the short-lived particle half-life of plasma-activated water under liquid nitrogen storage conditions is significantly extended relative to other storage conditions.
Specifically, the relationship between the active particle concentration and the storage temperature is obvious in the first 4 to 6 hours (the active particle concentration is inversely proportional to the storage temperature); however, after 10 hours, the active particle concentrations at room temperature, -4 ℃, -20 ℃ and-80 ℃ had not differed much, while the active particles were still maintained at higher concentrations, at least 2 times greater than the former, under liquid nitrogen storage conditions. According to analysis, on one hand, if the temperature is reduced at normal temperature or slowly, the free radicals and the active particles still participate in the chemical reaction in the solution at a high reaction rate, so that a large amount of active species are consumed, and the active particles can be greatly reduced in decay rate after the reaction is finished due to the fact that the active species are transferred to a liquid nitrogen environment for rapid temperature reduction; on the other hand, the frozen state is also advantageous for delaying the decay of active particles compared to the liquid state.
Example two
And starting the temperature adjusting device, activating the deionized water by the discharging device under a low-temperature condition (10 ℃), and simultaneously keeping the discharging gas and the solution to be treated at room temperature for 3 min. After the discharge is finished, the activated water is quickly subpackaged and stored at different temperature conditions. When the sample is thawed to room temperature before detection, the active particle concentration result is shown in fig. 3, and it can be seen that the short-lifetime particle half-life of the plasma activated water under the liquid nitrogen preservation condition is obviously prolonged compared with that under other preservation conditions.
Comparing fig. 2 and fig. 3, it can also be seen that, under the same storage conditions, the lower the ambient temperature for preparing the activation solution, the higher the concentration of the generated short-lived active particles (the higher the generation efficiency of the active particles in the plasma activation solution), and that the active particles are maintained at a higher concentration, particularly under the liquid nitrogen storage conditions, which is significantly better than that under other conditions.
Claims (10)
1. A method for preparing a finished product of plasma activated water is characterized by comprising the following steps:
step 1) generating atmospheric pressure low-temperature plasma by using a plasma generation module with a surface discharge structure, and diffusing the plasma into a solution to be treated to form plasma activated water; the plasma generation module, the discharge gas and the solution to be treated are all in an environment lower than room temperature;
and 2) rapidly cooling the formed plasma activated water by using liquid nitrogen to convert the plasma activated water into a frozen state, and storing the plasma activated water in a liquid nitrogen environment.
2. The method for preparing a finished product of plasma activated water as claimed in claim 1, wherein in the step 1), the environment temperature of the plasma generation module, the discharge gas and the solution to be treated is controlled to be-25 ℃ to 10 ℃ all the time.
3. The method for producing a finished product of plasma-activated water according to claim 1 or 2, wherein in step 2), the formed plasma-activated water is transferred to a sealed container and then immediately placed in a thermal insulation case filled with liquid nitrogen.
4. The method for preparing a finished product of plasma activated water as claimed in claim 1, wherein the solution to be treated is deionized water, ultrapure water, double distilled water, NaOH solution or ultrapure water containing ethanol.
5. A system for preparing plasma activated water comprises a high-voltage power supply, a cold plasma generation module adopting a creeping discharge structure and an activation liquid container containing a solution to be treated; the cold plasma generation module comprises an insulating dielectric plate for dielectric barrier discharge, a high-voltage electrode and a ground electrode with a grid structure, wherein the ground electrode is used as a cold plasma generation interface for creeping discharge, and a gas gap is formed between the ground electrode and the activation liquid container; the positive output end and the negative output end of the high-voltage power supply are respectively connected with a high-voltage electrode and a ground electrode of the cold plasma generation module, and the cold plasma is generated by exciting the cold plasma generation module to process the solution to be processed;
the method is characterized in that: the device also comprises a temperature adjusting device and a gas cooling pipe; the output end of the gas cooling pipe is positioned in the gas gap and used for introducing cooling gas; the temperature adjusting device is provided with an accommodating space, and the cold plasma generating module and the activating liquid container are both arranged in the accommodating space of the temperature adjusting device, so that the environment temperature is lower than the room temperature.
6. The system for preparing plasma-activated water according to claim 5, wherein: the cold plasma generating module is detachably, hermetically and fixedly covered at the upper end of the discharge space shell, so that the discharge space is isolated from the outside air; the input end of the gas cooling pipe is connected with the working gas storage bottle, and the output end of the gas cooling pipe is connected with one side of the discharge space shell; the other side of the discharge space housing is used for discharging waste gas through an exhaust pipe, and an air valve is arranged on the exhaust pipe.
7. The system for preparing plasma-activated water according to claim 6, wherein: the temperature adjusting device adopts a contact refrigerator, a groove is formed in the upper surface of the temperature adjusting device to form the accommodating space, and cooling liquid is filled in the groove; the gas cooling tube has a portion bent and immersed in the cooling liquid, and the lower portion of the discharge space housing is also immersed in the cooling liquid.
8. The system for preparing plasma-activated water according to claim 6, wherein: and a temperature monitor is arranged in the cavity of the discharge space shell and used for feedback regulation and refrigeration in the working process.
9. A method for preserving plasma activated water is characterized in that the prepared plasma activated water is rapidly cooled by liquid nitrogen to be converted into a frozen state and is stored in a liquid nitrogen environment.
10. The device for preserving the plasma activated water is characterized by comprising a heat preservation shell and a sealed container, wherein the sealed container is used for hermetically storing the plasma activated water, liquid nitrogen is filled in the heat preservation shell, and the sealed container is completely placed in the liquid nitrogen environment.
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| CN202010962018 | 2020-09-14 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112972723A (en) * | 2021-02-24 | 2021-06-18 | 西安交通大学 | Discharge plasma disinfection device combining nitrogen oxide mode and ozone mode |
| CN113511706A (en) * | 2021-05-10 | 2021-10-19 | 北京农学院 | Device and method for preparing activated ice by air plasma |
| CN113717409A (en) * | 2021-08-20 | 2021-11-30 | 西安交通大学 | Injectable plasma activated hydrogel and preparation method thereof |
| RU2804982C1 (en) * | 2023-04-13 | 2023-10-09 | федеральное государственное автономное образовательное учреждение высшего образования "Казанский (Приволжский) федеральный университет" (ФГАОУ ВО КФУ) | Device for disinfection of wastewater with cold atmospheric air plasma and method of its use |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112972723A (en) * | 2021-02-24 | 2021-06-18 | 西安交通大学 | Discharge plasma disinfection device combining nitrogen oxide mode and ozone mode |
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| CN113511706A (en) * | 2021-05-10 | 2021-10-19 | 北京农学院 | Device and method for preparing activated ice by air plasma |
| CN113717409A (en) * | 2021-08-20 | 2021-11-30 | 西安交通大学 | Injectable plasma activated hydrogel and preparation method thereof |
| RU2804982C1 (en) * | 2023-04-13 | 2023-10-09 | федеральное государственное автономное образовательное учреждение высшего образования "Казанский (Приволжский) федеральный университет" (ФГАОУ ВО КФУ) | Device for disinfection of wastewater with cold atmospheric air plasma and method of its use |
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