CN111569683A - High-concentration long-acting ozone nano bubble aqueous solution and preparation method thereof - Google Patents
High-concentration long-acting ozone nano bubble aqueous solution and preparation method thereof Download PDFInfo
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/20—Mixing gases with liquids
- B01F23/23—Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/20—Mixing gases with liquids
- B01F23/23—Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids
- B01F23/235—Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids for making foam
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- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/20—Mixing gases with liquids
- B01F23/23—Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids
- B01F23/237—Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids characterised by the physical or chemical properties of gases or vapours introduced in the liquid media
- B01F23/2373—Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids characterised by the physical or chemical properties of gases or vapours introduced in the liquid media for obtaining fine bubbles, i.e. bubbles with a size below 100 µm
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/20—Mixing gases with liquids
- B01F23/23—Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids
- B01F23/237—Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids characterised by the physical or chemical properties of gases or vapours introduced in the liquid media
- B01F23/2376—Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids characterised by the physical or chemical properties of gases or vapours introduced in the liquid media characterised by the gas being introduced
- B01F23/23761—Aerating, i.e. introducing oxygen containing gas in liquids
- B01F23/237613—Ozone
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
- B01F2101/04—Mixing biocidal, pesticidal or herbicidal ingredients used in agriculture or horticulture, e.g. for spraying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
- B01F2101/2202—Mixing compositions or mixers in the medical or veterinary field
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
- B01F2101/24—Mixing of ingredients for cleaning compositions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
- B01F2101/48—Mixing water in water-taps with other ingredients, e.g. air, detergents or disinfectants
Abstract
A process for preparing the high-concentration long-acting aqueous solution of nano-class ozone bubbles features that the micro-bubble generator is used to prepare nano-class ozone bubbles in the aqueous solution containing bubble-holding agent, resulting in the ozone concentration higher than 129 × 108100mL of ozone nano-bubbles with the particle size of less than 500nm can be stably retained in the aqueous solution for a long time. The ozone concentration of the ozone nano bubble water solution is 18.5-63 mg/L, and the ozone concentration of the ozone nano bubble water solution can still be kept above 60% of the ozone concentration of the prepared ozone nano bubble water solution after being sealed and stored for three months at normal temperature in a shading mode. The ozone nano bubble water solution has higher sterilization capability than the existing ozone water. Can be applied to the fields of medical treatment, sanitation, industry, food processing, agriculture, breeding industry, fresh keeping, sterilization, decontamination, deodorization, washing, family personal and pets, etc.
Description
Technical Field
The invention relates to a high-concentration long-acting ozone nano bubble aqueous solution and a preparation method thereof, belonging to the technical field of preparation of preserving ozone nano bubbles.
Background
The water in which ozone gas is dissolved is called ozone water, and it is known that ozone water has a strong oxidizing ability as well as ozone gas, and is widely used in the fields of sterilization, disinfection, freshness preservation, deodorization, cleaning, decoloring, and the like. The ozone gas oxidizes respiratory tissues to cause damage to the body tissues, but the ozone water is harmless to the body tissues (except for the ozone gas dissipated in the air) and has no residue. The united states Food and Drug Administration (USA Food and Drug Administration) listed ozone water as a Food additive in 2001, and could be used for Food factory sterilization and Food sterilization. The decomposition speed of ozone in water is faster than that in air, the half-life period of ozone dissolved in water is 5-30 minutes, ozone can be recovered to oxygen (no residual property of ozone) within half an hour after the ozone is manufactured, namely, the ozone water has no long-acting property and storage property, the ozone water needs to be manufactured and used on site by a machine, the application of the ozone water is greatly limited, and the long-acting ozone water which can be stored for a long time and can be carried is not available at present, so the ozone water cannot be widely applied to various industries, particularly to the aspects of medical treatment, families and individuals.
Chinese patent CN106573805A discloses an ozone water and its manufacturing method. Ozone exists stably in water at a concentration of, for example, 1 to 50mg/L, and a half-life period of the ozone is, for example, 3 days or more at a temperature of 40 ℃ in a sealed container filled with the ozone under atmospheric pressure; further, for example, after filling the inside of a sealed container under atmospheric pressure and freezing and storing the container at a temperature of-20 ℃ for 1 month or more, the container is naturally thawed at normal temperature (25 ℃), and the ozone concentration before freezing can be maintained.
However, the ozone water prepared by the Chinese patent CN106573805A has low ozone concentration, the highest concentration is only 5mg/L in the embodiment, the half-life period is more than three days at the temperature of 40 ℃, and the storage time is short; although the freezing storage can be more than one month, the storage cost is high, and therefore the freezing storage cannot be commercialized, and the practicability is low.
Disclosure of Invention
The invention aims to provide a high-concentration long-acting ozone nano bubble aqueous solution. The ozone concentration is 18.5-63 mg/L, and after the ozone nano bubble water solution is sealed and protected from light for three months at normal temperature, the ozone concentration in the water solution can still keep more than 60% of the ozone concentration in the preparation process.
The ozone nano bubble water solution can be stored for more than three months at normal temperature and can become a widely used commodity.
The technical scheme of the invention is as follows:
the high-concentration long-acting ozone nano bubble water solution is obtained by generating ozone micro bubbles with the diameter of less than 60 mu m in the water solution dissolved with the bubble retention agent.
The high-concentration long-acting ozone nano-bubble aqueous solution comprises a bubble retention agent, an electrolyte, a surfactant and a water-soluble polymer.
In the high-concentration long-acting ozone nano bubble aqueous solution, the electrolyte is an inorganic salt electrolyte.
In the high-concentration long-acting ozone nanobubble aqueous solution, the inorganic salt electrolyte is one or more of sodium chloride, magnesium chloride, potassium chloride, calcium chloride, ferric chloride, calcium silicate, calcium carbonate, ammonium chloride, ammonium carbonate, ammonium phosphate, sodium phosphate and magnesium phosphate, and the content of the inorganic salt electrolyte in the aqueous solution is 3 wt% -50 wt%.
In the high-concentration long-acting ozone nanobubble aqueous solution, the inorganic salt electrolyte is salt, including sea salt, well salt, rock salt, lake salt and crystal salt; or inorganic salt in seawater, concentrated seawater, underground brine, salt lake water and salt well water, and the content of the inorganic salt in the aqueous solution is 3 to 36 weight percent.
In the high-concentration long-acting ozone nano bubble aqueous solution, the inorganic salt electrolyte is bittern which comprises bittern, brine, bittern blocks, brine powder, bittern sheets, bittern crystals, rock bittern and well bittern, and the content of the inorganic salt electrolyte in the aqueous solution is 3-50 wt%.
In the high-concentration long-acting ozone nano bubble aqueous solution, the surfactant is one or more of a nonionic surfactant, a zwitterionic surfactant, an anionic surfactant, a cationic surfactant and a high molecular surfactant, and the content of the surfactant in the aqueous solution is 200ppm to 2000 ppm.
In the high-concentration long-acting ozone nanobubble aqueous solution, the surfactant is one or more of alkyl polyglycoside, sucrose fatty acid ester, sorbitol ester, polyoxyethylene sorbitan monooleate, sodium cocoamphoacetate, cocamidopropyl betaine and sodium lauryl sulfate.
In the high-concentration long-acting ozone nanobubble aqueous solution, the surfactant is one or two of alkyl polyglycoside and polyoxyethylene sorbitan monooleate.
The water-soluble polymer comprises natural water-soluble polymer, modified natural water-soluble polymer, synthetic water-soluble polymer and inorganic water-soluble polymer, and the content of the water-soluble polymer in the solution is 100ppm to 2000 ppm.
In the high-concentration long-acting ozone nano bubble aqueous solution, the water-soluble polymer is one or more of sodium alginate, sodium carboxymethyl starch, arabic gum, gelatin, hydroxypropyl methylcellulose, methyl cellulose, carboxymethyl cellulose, hydroxyethyl cellulose, polyacrylamide, polyacrylic acid and salts thereof, polyvinylpyrrolidone, polyvinyl alcohol, polyquaternary ammonium salt, magnesium aluminum silicate, magnesium lithium silicate and magnesium sodium silicate, and the content of the water-soluble polymer in the solution is 100ppm to 2000 ppm.
In the high-concentration long-acting ozone nano bubble aqueous solution, the water-soluble polymer is polyvinylpyrrolidone or polyvinyl alcohol, and one or two of the polyvinylpyrrolidone and the polyvinyl alcohol are used in combination.
The high-concentration long-acting ozone nano bubble water solution has the ozone nano bubble particle size of below 500nm, the average particle size of 300nm, the ozone concentration of 18.5-63 mg/L, and the number of the ozone nano bubbles exceeding 129 × 108One/100 mL.
In the high-concentration long-acting ozone nanobubble aqueous solution, one or more of an antibacterial agent, a pH adjuster, a dispersant, antibacterial metal ions, sugar, a stabilizer, a complexing agent, an emulsifier, an astringent, a binder, a dispersion aid, a fluidizing agent, a buffer, a perfume, a suspending agent, and vitamins are added.
The high-concentration long-acting ozone nano bubble aqueous solution is used for sterilization, disinfection, treatment of skin diseases, oral health care, deodorization, fresh keeping and cleaning.
In the preparation method of the high-concentration long-acting ozone nano bubble aqueous solution, the bubble retaining agent is added into water to be dissolved, and ozone micro bubbles with the diameter of less than 60 microns are generated in the obtained aqueous solution; under the action of the bubble retaining agent, the ozone microbubbles are shrunk in the aqueous solution to form ozone nanobubbles which are reserved in the aqueous solution.
In the preparation method of the high-concentration long-acting ozone nano-bubble aqueous solution, the surfactant and the water-soluble polymer are added into the seawater, the concentrated seawater, the underground brine, the salt lake water and the salt well water, ozone micro-bubbles with the diameter of less than 60 microns are generated in the aqueous solution, and the ozone micro-bubbles are shrunk to form ozone nano-bubbles in the aqueous solution and are remained in the aqueous solution.
In the preparation method of the high-concentration long-acting ozone nanobubble aqueous solution, the bubble retention agent is added into water to be dissolved, and microbubbles of air, oxygen, nitrogen, carbon monoxide gas, carbon dioxide gas, argon or hydrogen gas are generated in the aqueous solution to prepare nanobubble aqueous solutions of various gases such as air nanobubbles, oxygen nanobubbles, nitrogen nanobubbles, carbon monoxide nanobubbles, carbon dioxide nanobubbles, argon nanobubbles or hydrogen nanobubbles.
The invention relates to a preparation principle of ozone nano bubbles and an ozone nano bubble aqueous solution
Definition of Nanobubble Water
Bubbles with a diameter in the range of 1 μm to 100 μm are called Micro bubbles (Micro bubbles), while bubbles with a diameter smaller than 1 μm are called ultra fine bubbles (Nano bubbles), also called Nano bubbles (Nano bubbles), and the water in which Nano bubbles remain is Nano bubble water.
Apparatus for producing microbubbles
The micro-bubble manufacturing method mainly includes two types, i.e., a pressurized gas dissolving method and a two-phase flow rotating method. The pressurizing and air dissolving mode is widely applied due to the simple structure of the equipment, low energy consumption and large amount of generated bubbles.
Micro bubble forming principle by pressurized gas dissolving mode
The gas-liquid mixing pump stirs, mixes and dissolves gas in liquid (water), high pressure is formed in the pressure gas dissolving tank through circulating water flow, so that the gas is supersaturated and dissolved in the pressure gas dissolving tank, when the gas dissolving liquid in the supersaturated state passes through a releaser arranged on the water tank, the gas dissolving liquid returns to the normal pressure state from the high pressure state, the pressure is released, the supersaturated gas dissolved in the water is gushed out into the water in the form of micro-bubbles, and a large amount of micro-bubbles with different sizes below 60 mu m are formed in the water.
Micro-bubbles with different sizes below 60 mu m are formed in water, and the micro-bubbles with the sizes more than 50 mu m rise to the water surface to be broken under the action of buoyancy; the micro bubbles smaller than 50 μm are rapidly reduced due to the action of surface tension and finally disappear in water; and in the rising process, a large number of micro bubbles are combined into large bubbles continuously, and the large bubbles rise to the water surface to be broken. Microbubbles generally remain in the water for less than 3 minutes.
The principle of the present invention for forming nano bubbles
The aqueous solution of the present invention has dissolved therein a bubble-retaining agent comprising an electrolyte, a surfactant and a water-soluble polymer, wherein the electrolyte is present in the aqueous solution in the form of positive and negative ions. The gas-liquid interface of the general bubble has the characteristic of negative electricity, in the process of rapidly reducing the micro-bubble with the diameter less than 50 microns, negative ions on the gas-liquid interface and positive ions attracted to the vicinity of the gas-liquid interface by the electrostatic attraction of the negative ions are simultaneously and rapidly concentrated in high concentration, when the micro-bubble is reduced to 50 nm-500 nm, the attraction between the positive ions and the negative ions reaches a balance under the action of electrostatic coulomb force, an electronic shell consisting of concentrated ions is formed at the periphery of the bubble, the electronic shell prevents the gas in the bubble from being released into an aqueous solution, the gas in the bubble is not released into the aqueous solution any more, the bubble is not reduced any more and is not disappeared, and thus, the nano-bubble wrapped by the electronic shell is formed. The nano bubbles are extremely tiny and are not influenced by buoyancy and gravity, so that the nano bubbles do not float and sink, and only do irregular swinging (Brownian motion) in the aqueous solution, so that the nano bubbles can be remained in the aqueous solution for a long time.
The surfactant functions to reduce the surface tension of the bubbles, maintain the spherical shape of the bubbles, prevent coalescence between the bubbles, and reduce the rising speed of the bubbles. The surfactant prevents the merging of bubbles, so that the generated microbubbles with the diameter of less than 50 mu m can be almost changed into nanobubbles to be reserved in the aqueous solution, and the generated nanobubbles are huge in quantity.
The water-soluble polymer has a long-branched-chain or dendritic multi-branched-chain structure with most linear molecules, forms a three-dimensional cross-linked network structure in an aqueous solution, and can wrap nano bubbles in the three-dimensional cross-linked network structure so as to enable the nano bubbles to be more stably retained in the aqueous solution for a long time.
The invention uses the above-mentioned pressurized gas-dissolving type microbubble generating device and ozone gas generator, in the water solution dissolved with bubble retention agent, produce a large amount of ozone microbubbles circularly, wherein a large amount of ozone microbubbles with a diameter of less than 50 μm, under the action of ion and surfactant, the bubbles do not meet and continuously shrink to form ozone nanobubbles wrapped by the electronic shell, and produce and retain more than 1 hundred million/mL ozone nanobubbles in the water solution, thus produce high concentration ozone nanobubble water solution.
As mentioned above, ozone gas can not escape from the nano bubbles with the electronic shell, the nano bubbles wrapped by the electronic shell can be remained in the aqueous solution for a long time, and the water-soluble polymer forms a three-dimensional cross-linked network structure in the aqueous solution, so that the nano bubbles are covered in the three-dimensional network structure, and the ozone nano bubbles are remained in the aqueous solution for a long time more stably. Thus, the long-acting ozone nano bubble water solution is produced.
The invention selects electrolyte, surfactant and water-soluble polymer as bubble retention agent, which can store the ozone nano bubble water solution for a long time, compared with the patent document, the prepared ozone has high concentration which can reach 70mg/L, the ozone concentration can still keep more than 60% of the prepared ozone after being stored for three months in a sealed and light-proof way at normal temperature, the storage life can reach more than three months, and the possibility of preparing the consumption product for commercial sale is provided.
The ozone nanobubbles and the ozone nanobubble aqueous solution of the invention act
The nano bubbles have the characteristics of killing bacteria and inactivating viruses, so that the nano bubbles in the ozone nano bubble water solution have a powerful sterilization effect besides the ozone gas. When the electronic shell of the nano-bubble contacts bacteria or viruses, the charges escape, the electronic shell at the periphery of the nano-bubble is easily cracked, the bubble disappears instantly, and the disappearance of the bubble is caused by the rapid reduction of the bubble. The internal pressure of the bubble is inversely proportional to the diameter of the bubble, and when the bubble is rapidly contracted, the internal pressure of the bubble rises rapidly, and as a result of this very rapid velocity, when the bubble disappears, a high-temperature and high-pressure limit reaction field (hot spot) is generated, which is extremely minute but powerful, and which forcedly decomposes gas molecules and peripheral water molecules inside the bubble to generate OH, a substance called hydroxyl radical, english being hydroxyyradic. This OH is the most reactive active species in the radical, has the strongest oxidizing power, is higher than ozone, and decomposes chemical substances, and is a strong oxidizing agent. The surface of the bacteria is directly oxidized by ozone released when the ozone nano bubbles disappear and a large number of hydroxyl radicals generated by decomposition, and under the action of the double strong oxidation, bacterial cytoplasm agglutinates to cause outer membrane obstruction and cell nucleus condensation, and finally the bacterial cytoplasm is broken into fragments to die.
As described above, the aqueous ozone nanobubble solution of the present invention has both strong oxidation effects of ozone and hydroxyl radicals, and has stronger sterilization ability and stronger cleaning, decontamination, decoloring, etc. ability than the existing ozone water. The ozone nanobubble aqueous solution does not cause the generation of drug resistant bacteria.
The nano bubbles in the ozone nano bubble water solution have the functions of improving the physiological activity of the biological tissues and repairing the biological tissues. When the nano bubbles are formed, an electric field is generated around the nano bubbles, and the electric field has the effects of promoting physiological activity, accelerating metabolism, improving immunity and promoting the growth of body tissues.
The nano bubbles in the ozone nano bubble water solution have extremely high permeability. Because the diameter of the nano bubbles is smaller than that of cells and bacteria, the nano bubbles can permeate into the lower surface of the skin and the mucous membrane to kill bacteria, fungi and viruses under the skin and in the mucous membrane, so the ozone nano bubble aqueous solution is a brand-new non-medicine type sterilization therapeutic agent which is extremely effective in treating beriberi, dermatophytosis, gynecological diseases, oral diseases, urinary infection, rhinitis and the like.
The permeability of the nano bubbles also enables the nano bubbles to have high stripping performance, so the nano bubbles can be used for cleaning industrial processing parts and the like; it can also be used for cleaning cultured Concha Ostreae and killing bacteria and virus in Concha Ostreae.
Safety of ozone nanobubble aqueous solution
The ozone nano bubble water solution is nontoxic and harmless to body tissues and is extremely safe.
The ozone nano bubble water solution has no irritation to body tissues, particularly to body mucosa. Because the ozone in the aqueous solution of the ozone nano-bubbles is not dissolved in the aqueous solution but is completely wrapped in the nano-bubbles in the aqueous solution, and a layer of electronic shell is arranged outside the nano-bubbles to tightly wrap the nano-bubbles, the ozone gas cannot easily escape from the nano-bubbles, and the ozone cannot escape from the aqueous solution to the air. When the high concentration ozone nano bubble water solution is opened under the atmospheric pressure, only the ozone gas with the concentration of about 0.05ppm is released, and the ozone smell in the air can not be smelled. The concentration of the ozone gas which affects the living body tissue is 0.15ppm according to the national safety standard of China. The ozone gas with a concentration of 0.05ppm does not oxidize biological tissues, particularly biological mucous membranes, and does not irritate the biological tissues such as eyes, nose, throat, etc., so the ozone nanobubble aqueous solution is extremely safe.
Detailed Description
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
The invention is realized by the following steps:
the high-concentration long-acting ozone nano bubble water solution is obtained by generating ozone micro bubbles with the diameter of less than 60 mu m in the water solution dissolved with the bubble retention agent.
The high-concentration long-acting ozone nano-bubble aqueous solution comprises a bubble retention agent, an electrolyte, a surfactant and a water-soluble polymer.
The electrolyte is an inorganic salt electrolyte.
The inorganic salt electrolyte is one or more of sodium chloride, magnesium chloride, potassium chloride, calcium chloride, ferric chloride, calcium silicate, calcium carbonate, ammonium chloride, ammonium carbonate, ammonium phosphate, sodium phosphate and magnesium phosphate, and the content of the inorganic salt electrolyte in the aqueous solution is 3-50 wt%.
The inorganic salt electrolyte can adopt inorganic salt with single component, and also can adopt salt consisting of inorganic salts with multiple components, including sea salt, well salt, rock salt, lake salt and crystal salt; or the inorganic salt in the seawater, the concentrated seawater, the underground brine, the salt lake water and the salt well water, the content of the inorganic salt in the water solution is 3 to 36 weight percent.
The inorganic salt electrolyte can also be bittern, including bittern, bittern blocks, bittern powder, bittern sheets, bittern crystals, rock bittern and well bittern, and the content of the inorganic salt electrolyte in the aqueous solution is 3-50 wt%.
The surfactant is one or more of nonionic surfactant, zwitterionic surfactant, anionic surfactant, cationic surfactant and high molecular surfactant, and the content of the surfactant in the aqueous solution is 200-2000 ppm.
Preferably, the surfactant is one or more of alkyl polyglycoside, sucrose fatty acid ester, sorbitol ester, polyoxyethylene sorbitan monooleate, sodium cocoamphoacetate, cocamidopropyl betaine, and sodium lauryl sulfate.
More preferably, the surfactant is one or a mixture of alkyl polyglycoside and polyoxyethylene sorbitan monooleate.
The water-soluble polymer comprises natural water-soluble polymer, modified natural water-soluble polymer, synthetic water-soluble polymer and inorganic water-soluble polymer, wherein the content of the water-soluble polymer in the solution is 100 ppm-2000 ppm.
Preferably, the water-soluble polymer is one or more of sodium alginate, sodium carboxymethyl starch, Arabic gum, gelatin, hydroxypropyl methylcellulose, carboxymethylcellulose, hydroxyethyl cellulose, polyacrylamide, polyacrylic acid and salts thereof, polyvinylpyrrolidone, polyvinyl alcohol, polyquaternium, magnesium aluminum silicate, magnesium lithium silicate and sodium magnesium silicate, and the content of the water-soluble polymer in the solution is 100ppm to 2000 ppm.
More preferably, the water-soluble polymer is polyvinylpyrrolidone or polyvinyl alcohol, and one or a mixture of two of them is used.
The particle size of the ozone nano bubbles is below 500nm, the average particle size is 300nm, the ozone concentration is 18.5-63 mg/L, and the number of the ozone nano bubbles exceeds 129 × 108One/100 mL.
The solution is added with one or more of an antibacterial agent, a pH regulator, a dispersing agent, antibacterial metal ions, sugar, a stabilizer, a complexing agent, an emulsifier, an astringent, a binding agent, a dispersing auxiliary agent, a fluidizing agent, a buffering agent, a spice, a suspending agent and vitamins to prepare products with different effects and different functions, and the products are used in the fields of sterilization, disinfection, skin disease treatment, oral health care, deodorization, fresh keeping, cleaning and the like.
The preparation method of the high-concentration long-acting ozone nano bubble water solution comprises the steps of adding the bubble retention agent into water for dissolving, and generating ozone micro bubbles with the diameter of less than 60 mu m in the obtained water solution; under the action of the bubble retaining agent, the ozone microbubbles are shrunk in the aqueous solution to form ozone nanobubbles which are reserved in the aqueous solution.
The surfactant and the water-soluble polymer can be added into the seawater, the concentrated seawater, the underground brine, the salt lake water and the salt well water, ozone microbubbles with the diameter of less than 60 mu m are generated in the aqueous solution, and the ozone microbubbles are shrunk to form ozone nanobubbles and are remained in the aqueous solution.
According to the technical scheme of the invention, the bubble holding agent can be added into water to be dissolved, and air, oxygen, nitrogen, carbon monoxide gas, carbon dioxide gas, argon or hydrogen microbubbles are generated in the obtained aqueous solution to prepare the nanobubble aqueous solution of various gases such as air nanobubbles, oxygen nanobubbles, nitrogen nanobubbles, carbon monoxide nanobubbles, carbon dioxide nanobubbles, argon nanobubbles or hydrogen nanobubbles.
How to prepare the invention is described below by combining specific mixture ratio
Example 1
Using machines
Using a pressurized dissolved air type microbubble generator (made by environmental protection technologies Co., Ltd., Yixing, Jiangsu) with a flow rate of 2m3/h。
An ozone gas generator (model HY-YW-060, manufactured by Ottoman, Sichuan) was used in an amount of 60g/h, and medical oxygen was used as a gas source of the ozone gas generator.
Aqueous solution
Solid bittern, alkyl polyglycoside and polyvinyl alcohol were respectively put into water and dissolved with stirring as shown in table 1, and the conductivity of the aqueous solution after dissolution was 56ms/cm and the pH was adjusted to 5.0 (measured using an IP67 multifunctional waterproof handheld pH/conductivity/salinity/solubility meter manufactured by taiwan AZ Instrument corp.).
TABLE 1 composition of aqueous solution
| Composition of aqueous solution | Amount of the composition used | Content (wt.) |
| Water (W) | 19 liters of water | |
| Solid bittern | 1kg | 5wt％ |
| Alkyl polyglycosides | 28.59 | 1500ppm |
| Polyvinyl alcohol | 199 | 1000ppm |
Manufacturing operating conditions
Pressure of the pressurized dissolved air tank: 0.4 to 0.5MPa
The temperature of the aqueous solution in the operation is kept between 1 and 8 DEG C
Ozone gas generator oxygen inlet flow: 2 to 3L/min
Ozone gas generator ozone gas generation amount: 1 to 2L/min
Vacuum negative pressure: 0.015 to 0.03MPa below zero
Production of ozone nanobubble aqueous solution
Pouring the prepared aqueous solution into a water tank of a pressurized dissolved air type micro-bubble generating device, starting the pressurized dissolved air type micro-bubble generating device and an ozone gas generating machine, and circularly operating for 45 minutes to prepare the ozone nano-bubble aqueous solution.
Measuring ozone concentration of ozone nanobubble aqueous solution
The aqueous solution of ozone nanobubbles was sampled from a beaker and measured with an electrode type ozone detector (LEANLEAU DOZ30 pen ozone tester) to show that the concentration of ozone was 0 mg/L.
Diluting the sampled ozone nano bubble aqueous solution by 50 times with purified water, pouring 10mL into a detection dish of an intelligent portable ozone detector, respectively sucking 1mL of DPD ozone detection reagent A, 0.5mL of DPD ozone detection reagent B and DPD ozone detection reagent C by a dropper, dripping into the detection dish containing the ozone nano bubble aqueous solution diluted by 50 times, and then putting the detection dish into the intelligent portable ozone detector (model Y-615, manufactured by Hangzhou Qinwei instruments Co., Ltd.), wherein the ozone concentration of the ozone nano bubble aqueous solution is 0.506mg/L, and the actual concentration is 0.506 × 50 ═ 25.3 mg/L.
Measuring the quantity and the particle diameter of ozone nano bubbles
The ozone nanobubble aqueous solution was sampled, and the amount of nanobubbles was measured to be 1.51 × 10 using a nanosight NS500 nm measuring instrument from nanosight, Inc. of UK8ge/mL, nanobubble average particle size is 298 nm.
Examples 2 to 10
Examples 2 to 10 were prepared in the same manner as in example 1 except that the materials added to the aqueous solution were different and the percentage contents were different, as shown in Table 2.
Table 2 shows the additive materials and percentage contents thereof, the production time and the nanobubble measurement data at the time of production in examples 1 to 10.
TABLE 2
Table 3 shows the ozone concentration when the aqueous solution of ozone nanobubble of examples 1 to 10 was prepared and the ozone concentration at each storage time period, and all data were measured by using an intelligent portable ozone detector (model Y-615, manufactured by hangzhou chenille instrument ltd).
Table 3 ozone concentration units: mg/L storage conditions: sealing in glass bottle, and storing at room temperature in dark place
| Examples | At the time of manufacture | After 1 month | After 2 months | After 3 months |
| 1 | 25.3 | 23.5 | 19.6 | 15.4 |
| 2 | 36.7 | 34 | 29.5 | 26 |
| 3 | 45 | 41.6 | 38.1 | 28.2 |
| 4 | 53 | 50.3 | 46 | 39.1 |
| 5 | 58.3 | 55 | 51.2 | 47 |
| 6 | 63 | 60.1 | 57 | 53.5 |
| 7 | 18.5 | 16.6 | 13 | 11.6 |
| 8 | 26 | 21.4 | 18 | 16.7 |
| 9 | 38 | 33.6 | 27.4 | 23.1 |
| 10 | 41.5 | 38 | 35.9 | 27 |
Comparative example 1
The aqueous solution of ozone nanobubbles prepared using 5 wt% bittern without addition of alkyl polyglycoside and polyvinyl alcohol as in example 1 had an ozone concentration of 5.7mg/L, and after three days of storage at room temperature in the dark, the ozone concentration was measured to be 0 mg/L.
Comparative example 2
Ozone water was prepared in the same manner as in example 1 in water to which no bubble retention agent was added.
During the operation of the machine, the highest ozone concentration was measured to be 7mg/L using an electrode type ozone measuring instrument (using a LEANEAU DOZ30 pen ozone tester), 2mg/L after the machine was stopped, and 0mg/L after ten minutes of the machine was stopped.
Analysis of results of examples and comparative examples
1. From the above example 1, it can be seen that the concentration of ozone was not detected when the aqueous ozone nanobubble solution of the present invention was measured by an electrode type ozone meter, indicating that all ozone gas was wrapped in nanobubbles and not dissolved in water.
2. From examples 1 to 10, it is understood that the number of nanobubbles and the ozone concentration increase as the inorganic salt content in the aqueous solution increases.
3. It is clear from the above examples 1 to 10 that the bittern generates ozone nanobubbles more than sodium chloride at the same content and has a high concentration. The bittern consists of a plurality of components, and the sodium chloride is a single component, which shows that the more the inorganic salt component is, the more the ozone nano-bubbles are produced, and the higher the concentration is.
4. From examples 1 to 10, it is clear that the ozone concentration of the produced ozone nanobubble aqueous solution is high because the number of generated nanobubbles exceeds 1.29 hundred million/mL and the number of nanobubbles is large by adding the bubble-retaining agent to water.
5. The nanobubbles of examples 1-10 were all extremely small, with an average particle size below 300nm, and therefore they were able to remain in the aqueous ozone nanobubble solution for a long time; through a preservation experiment (table 3), the ozone concentration of the ozone nano bubble water solution is reduced very slowly, after three months of preservation, the ozone concentration is kept to be more than 60% of the ozone concentration during preparation, the aim of keeping the ozone concentration for a long time (namely, long-acting property and long-term preservation property) is achieved, the minimum ozone concentration after three months of preservation is still 11.6mg/L which is nearly three times of the minimum sterilization concentration of 4mg/L of ozone water, and the ozone nano bubble water solution still has extremely high sterilization capacity.
6. From the above comparative example 1, it is understood that the aqueous ozone nanobubble solution prepared by adding only the inorganic salt, but not the surfactant and the water-soluble polymer has a shelf life of three days or less and no preservability.
7. As is clear from comparative example 2, the ozone water produced without adding the bubble retention agent had an ozone half-life of 10 minutes or less.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Main use in industry
The ozone nano bubble water solution prepared by the invention is filled into a sealed container, can be carried, transported and stored, and can be widely applied to various industries, particularly to the aspects of medical treatment, families and individuals.
Medical field
Cleaning and sterilizing medical instruments.
Can be used as dental water to replace the existing normal saline.
The nanometer bubble has permeability, and can improve tissue physiological activity, tissue repair function and antibacterial function, and can be used for treating loempe, tinea, gynecological diseases, urinary infection, osteomyelitis, rhinitis, oral diseases, ulcer, gangrene, decubital ulcer, wound, etc.
The animal is treated by common medicaments, the animal licks the medicaments to cause injury to the animal, and the animal licks the ozone nano bubble water solution without any problem.
The bath lotion can be used as bath lotion for pets, and has effects in preventing and treating animal skin tinea, removing odor from animal body, and making hair bright and soft.
Sterilizing and deodorizing environment
Can be used for sterilizing and deodorizing the environments of hospitals, public places, hotels, restaurants, retirees, families, farms and the like; can be used for cleaning and disinfecting household appliances such as desks, air conditioners, refrigerators, chopping boards and the like.
The field of food
Cleaning, deodorizing and preserving meat fish.
Cleaning and sterilizing food processing machinery, production line, ground, etc.
Sterilizing and preserving processed vegetables and fruits.
Removing residual pesticide on vegetables and fruits.
Field of agricultural breeding industry
Can be used for sterilizing hydroponics culture implement and seed.
Sterilizing the culture water.
Field of industry
The surface modification of metal processing parts, plastics and the like can increase the firmness of the electroplated layer.
For processing and manufacturing products
Disinfectant paper towels, wet tissues and portable hand-washing disinfectant.
Ozone toothpaste, beauty cream, beauty mask, etc.
Ozone sterilizing wound ointment and wound plaster.
Personal area of family
Can be used as collutory and tooth brushing liquid for preventing and treating oral diseases and whitening teeth.
Can be used as nasal wash for preventing and treating rhinitis.
It can be used for cleaning and sterilizing skin and genitals.
Used for washing.
It can be used for cleaning toilet, deodorizing, and removing dirt.
Is used for bathing with ozone nano bubble water solution.
Safety test
The concentration of ozone gas released into the air by the ozone nanobubble aqueous solution was measured to confirm the safety of water dissolution of the ozone nanobubbles.
2L of the aqueous ozone nanobubble solution of example 2 was poured into an open pan, heated to 72 ℃ and during the heating process, the concentration of ozone gas was measured at a level of 0.5m vertically above the pan, and the measured value was found to be below 0.05ppm and below 0.15ppm, which is the national ozone safety standard, confirming that the ozone gas released from the aqueous ozone nanobubble solution is safe to human body.
Confirmation of non-toxicity of ozone nanobubble aqueous solution
When the aqueous solution of ozone nanobubbles of 36.7mg/L in example 2 was orally administered to mice at 2000mg/kg for 14 consecutive days, no abnormality was observed in mice, and no abnormality was observed in any tissue during dissection, confirming that the aqueous solution of ozone nanobubbles was safe to the body and non-toxic.
Tissue cell safety test
The ozone nano-bubble aqueous solution and the disinfectant Chlorhexidine (Chlorhexidine) in the example 2 are used for a survival rate comparison test of oral epithelial cells and oral mucosa cells of a human body, the oral epithelial cells and the oral mucosa cells are respectively put into the ozone nano-bubble aqueous solution and the disinfectant Chlorhexidine in the example 2 for soaking, the survival rate of the cells of the Chlorhexidine is 50%, the oral epithelium is 10.8 hours, and the oral mucosa is 8.4 hours; the 50% survival rate of the cells of the ozone nanobubble aqueous solution of example 2 was over 24 hours, and it was confirmed that the ozone nanobubble aqueous solution was non-toxic and safe to human tissues.
Table 4 shows the results of a 50% survival comparison test of oral epithelial cells and oral mucosal cells using the aqueous ozone nanobubble solution of example 2 (ozone concentration of 36.7mg/L) and chlorhexidine.
TABLE 4
| Half-minus time of viable cell number (ET)50) | Oral epithelial cells | Oral mucosa |
| Example 2 aqueous ozone nanobubble solution | Over 24 hours | Over 24 hours |
| Dichlorobiguanide hexanes | 10.8 hours | 8.4 hours |
Sterilization test
In order to verify the sterilization effect of the ozone nanobubble aqueous solution on pathogenic bacteria, the soaking sterilization test of escherichia coli was performed by using the ozone nanobubble aqueous solution of example 2, and the sterilization test results were as follows:
the average bacteria content is about 35 after soaking for 30 seconds.
The average bacteria content is about 10 after soaking for 60 seconds.
Soaking for 180 seconds, and the average bacteria content is about 0.
The sterilization test result shows that the ozone nano bubble water solution has strong sterilization effect on pathogenic bacteria.
Claims (18)
1. A high-concentration long-acting ozone nano bubble aqueous solution is characterized in that: is obtained by generating ozone microbubbles having a size of 60 μm or less in an aqueous solution in which a bubble-retaining agent is dissolved.
2. The high concentration long acting ozone nanobubble aqueous solution of claim 1, characterized by: the bubble retention agent is composed of an electrolyte, a surfactant and a water-soluble polymer.
3. The high concentration long acting ozone nanobubble aqueous solution of claim 2, characterized by: the electrolyte is an inorganic salt electrolyte.
4. The high concentration long acting ozone nanobubble aqueous solution of claim 3, wherein: the inorganic salt electrolyte is one or more of sodium chloride, magnesium chloride, potassium chloride, calcium chloride, ferric chloride, calcium silicate, calcium carbonate, ammonium chloride, ammonium carbonate, ammonium phosphate, sodium phosphate and magnesium phosphate, and the content of the inorganic salt electrolyte in the aqueous solution is 3-50 wt%.
5. The high concentration long acting ozone nanobubble aqueous solution of claim 3, wherein: the inorganic salt electrolyte is salt, including sea salt, well salt, rock salt, lake salt and crystal salt; or inorganic salt in seawater, concentrated seawater, underground brine, salt lake water and salt well water, and the content of the inorganic salt in the aqueous solution is 3 to 36 weight percent.
6. The high concentration long acting ozone nanobubble aqueous solution of claim 3, wherein: the inorganic salt electrolyte is bittern comprising bittern, bittern block, bittern powder, bittern slice, bittern crystal, rock bittern and well bittern, and has content of 3-50 wt% in water solution.
7. The high concentration long acting ozone nanobubble aqueous solution of claim 2, characterized by: the surfactant is one or more of nonionic surfactant, zwitterionic surfactant, anionic surfactant, cationic surfactant and high molecular surfactant, and the content of the surfactant in the aqueous solution is 200-2000 ppm.
8. The high concentration long acting ozone nanobubble aqueous solution of claim 7, wherein: the surfactant is one or more of alkyl polyglycoside, sucrose fatty acid ester, sorbitol ester, polyoxyethylene sorbitan monooleate, sodium cocoyl amphoacetate, cocamidopropyl betaine and sodium lauryl sulfate.
9. The high concentration long acting ozone nanobubble aqueous solution of claim 8, wherein: the surfactant is alkyl polyglycoside and polyoxyethylene sorbitan monooleate, and one or two of the surfactants are mixed for use.
10. The high concentration long acting ozone nanobubble aqueous solution of claim 2, characterized by: the water-soluble polymer comprises natural water-soluble polymer, modified natural water-soluble polymer, synthetic water-soluble polymer and inorganic water-soluble polymer, wherein the content of the water-soluble polymer in the solution is 100 ppm-2000 ppm.
11. The high concentration long acting ozone nanobubble aqueous solution of claim 10, wherein: the water-soluble polymer is one or more than two of sodium alginate, sodium carboxymethyl starch, Arabic gum, gelatin, hydroxypropyl methylcellulose, carboxymethyl cellulose, hydroxyethyl cellulose, polyacrylamide, polyacrylic acid and salts thereof, polyvinylpyrrolidone, polyvinyl alcohol, polyquaternium, magnesium aluminum silicate, lithium magnesium silicate and sodium magnesium silicate, and the content of the water-soluble polymer in the solution is 100 ppm-2000 ppm.
12. The high concentration long acting ozone nanobubble aqueous solution of claim 11, wherein: the water-soluble polymer is polyvinylpyrrolidone and polyvinyl alcohol, and one or two of the polyvinylpyrrolidone and the polyvinyl alcohol are used in a mixed way.
13. The high-concentration long-acting ozone nanobubble aqueous solution of claim 1, wherein the particle size of the ozone nanobubbles is below 500nm, the average particle size is 300nm, the ozone concentration is 18.5-63 mg/L, and the number of the ozone nanobubbles exceeds 129 × 108One/100 mL.
14. The high concentration long acting ozone nanobubble aqueous solution of claim 1, characterized by: the solution is added with one or more of antibacterial agent, pH regulator, dispersant, antibacterial metal ion, sugar, stabilizer, complexing agent, emulsifier, astringent, binder, dispersion adjuvant, fluidizing agent, buffer, perfume, suspending agent, and vitamins.
15. The high concentration long acting ozone nanobubble aqueous solution of claim 1, characterized by: the aqueous solution is used for sterilization, disinfection, treatment of skin diseases, oral health care, deodorization, fresh keeping and cleaning.
16. The method for preparing a high-concentration long-acting ozone nanobubble aqueous solution according to any one of claims 1 to 15, characterized in that: adding the bubble retention agent into water for dissolving, and generating ozone microbubbles with the diameter of less than 60 microns in the obtained aqueous solution; under the action of the bubble retaining agent, the ozone microbubbles are shrunk in the aqueous solution to form ozone nanobubbles which are reserved in the aqueous solution.
17. The method of preparing a high concentration long acting ozone nanobubble aqueous solution of claim 16, wherein: adding the surfactant and the water-soluble polymer into the seawater, the concentrated seawater, the underground brine, the salt lake water and the salt well water, generating ozone microbubbles with the diameter of less than 60 mu m in the aqueous solution, and reducing the ozone microbubbles in the aqueous solution to form ozone nanobubbles to be remained in the aqueous solution.
18. The method of preparing a high concentration long acting ozone nanobubble aqueous solution of claim 16, wherein: and adding the bubble retention agent into water for dissolving, and generating micro bubbles of air, oxygen, nitrogen, carbon monoxide gas, carbon dioxide gas, argon or hydrogen in the obtained aqueous solution to prepare nano bubble aqueous solution of various gases such as air nano bubbles, oxygen nano bubbles, nitrogen nano bubbles, carbon monoxide nano bubbles, carbon dioxide nano bubbles, argon nano bubbles or hydrogen nano bubbles.
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