CN114506907A - Active oxygen/active nitrogen enhanced oxidized electrolyzed water and preparation method and application thereof - Google Patents
Active oxygen/active nitrogen enhanced oxidized electrolyzed water and preparation method and application thereof Download PDFInfo
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- electrolyzed water
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 188
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 142
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 97
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 239000001301 oxygen Substances 0.000 title claims abstract description 91
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 31
- 230000004913 activation Effects 0.000 claims abstract description 29
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000460 chlorine Substances 0.000 claims abstract description 27
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 27
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 23
- 239000012159 carrier gas Substances 0.000 claims abstract description 21
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000011780 sodium chloride Substances 0.000 claims abstract description 15
- 239000003899 bactericide agent Substances 0.000 claims abstract description 12
- 239000003014 ion exchange membrane Substances 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000003792 electrolyte Substances 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- 230000003647 oxidation Effects 0.000 claims description 29
- 238000007254 oxidation reaction Methods 0.000 claims description 29
- 239000012528 membrane Substances 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 20
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 17
- 229910052719 titanium Inorganic materials 0.000 claims description 17
- 239000010936 titanium Substances 0.000 claims description 17
- 239000007789 gas Substances 0.000 claims description 15
- 230000033116 oxidation-reduction process Effects 0.000 claims description 13
- 238000005341 cation exchange Methods 0.000 claims description 9
- HTXDPTMKBJXEOW-UHFFFAOYSA-N dioxoiridium Chemical compound O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 claims description 9
- 229910000457 iridium oxide Inorganic materials 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 230000005284 excitation Effects 0.000 claims description 7
- 239000007921 spray Substances 0.000 claims description 7
- 230000002378 acidificating effect Effects 0.000 claims description 6
- 230000009467 reduction Effects 0.000 claims description 3
- 239000003011 anion exchange membrane Substances 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims description 2
- 150000002926 oxygen Chemical class 0.000 claims 6
- 230000001954 sterilising effect Effects 0.000 abstract description 17
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 11
- 238000001228 spectrum Methods 0.000 abstract 1
- 238000005507 spraying Methods 0.000 abstract 1
- 238000001994 activation Methods 0.000 description 26
- 210000004027 cell Anatomy 0.000 description 24
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 10
- 150000002500 ions Chemical class 0.000 description 10
- 230000001590 oxidative effect Effects 0.000 description 10
- 229910045601 alloy Inorganic materials 0.000 description 7
- 239000000956 alloy Substances 0.000 description 7
- 230000001580 bacterial effect Effects 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000000523 sample Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 229910002651 NO3 Inorganic materials 0.000 description 5
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 235000013305 food Nutrition 0.000 description 5
- -1 nitrate ions Chemical class 0.000 description 5
- 229940005654 nitrite ion Drugs 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 208000019331 Foodborne disease Diseases 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 244000063299 Bacillus subtilis Species 0.000 description 3
- 235000014469 Bacillus subtilis Nutrition 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 230000002147 killing effect Effects 0.000 description 3
- 230000000813 microbial effect Effects 0.000 description 3
- 239000008055 phosphate buffer solution Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 210000002421 cell wall Anatomy 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- OSVXSBDYLRYLIG-UHFFFAOYSA-N dioxidochlorine(.) Chemical compound O=Cl=O OSVXSBDYLRYLIG-UHFFFAOYSA-N 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 244000000010 microbial pathogen Species 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 2
- 235000019345 sodium thiosulphate Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 208000035143 Bacterial infection Diseases 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 239000004155 Chlorine dioxide Substances 0.000 description 1
- 229920002444 Exopolysaccharide Polymers 0.000 description 1
- MSFSPUZXLOGKHJ-UHFFFAOYSA-N Muraminsaeure Natural products OC(=O)C(C)OC1C(N)C(O)OC(CO)C1O MSFSPUZXLOGKHJ-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 108010013639 Peptidoglycan Proteins 0.000 description 1
- 239000005708 Sodium hypochlorite Substances 0.000 description 1
- 238000005349 anion exchange Methods 0.000 description 1
- 208000022362 bacterial infectious disease Diseases 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 230000019522 cellular metabolic process Effects 0.000 description 1
- 235000019398 chlorine dioxide Nutrition 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000000645 desinfectant Substances 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 244000078673 foodborn pathogen Species 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000005802 health problem Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000036542 oxidative stress Effects 0.000 description 1
- 239000002504 physiological saline solution Substances 0.000 description 1
- 238000000678 plasma activation Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000007845 reactive nitrogen species Substances 0.000 description 1
- 239000003642 reactive oxygen metabolite Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- 238000012414 sterilization procedure Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000002525 ultrasonication Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
-
- 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
-
- 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
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
-
- 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
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
- C02F1/4674—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation with halogen or compound of halogens, e.g. chlorine, bromine
-
- 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
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/46—Apparatus for electrochemical processes
- C02F2201/461—Electrolysis apparatus
- C02F2201/46105—Details relating to the electrolytic devices
- C02F2201/46115—Electrolytic cell with membranes or diaphragms
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/46—Apparatus for electrochemical processes
- C02F2201/461—Electrolysis apparatus
- C02F2201/46105—Details relating to the electrolytic devices
- C02F2201/4612—Controlling or monitoring
- C02F2201/46125—Electrical variables
- C02F2201/4614—Current
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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
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/46—Apparatus for electrochemical processes
- C02F2201/461—Electrolysis apparatus
- C02F2201/46105—Details relating to the electrolytic devices
- C02F2201/4612—Controlling or monitoring
- C02F2201/4615—Time
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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
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/46—Apparatus for electrochemical processes
- C02F2201/461—Electrolysis apparatus
- C02F2201/46105—Details relating to the electrolytic devices
- C02F2201/4618—Supplying or removing reactants or electrolyte
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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
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/46—Apparatus for electrochemical processes
- C02F2201/461—Electrolysis apparatus
- C02F2201/46105—Details relating to the electrolytic devices
- C02F2201/4619—Supplying gas to the electrolyte
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/02—Temperature
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/04—Oxidation reduction potential [ORP]
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/06—Controlling or monitoring parameters in water treatment pH
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/29—Chlorine compounds
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical
Abstract
The invention belongs to the field of preparation of novel environment-friendly bactericides, and particularly relates to active oxygen/active nitrogen enhanced oxidized electrolyzed water as well as a preparation method and application thereof. The method comprises the following steps: in an ion exchange membrane electrolytic cell, a homogeneous ion exchange membrane is adopted to divide the electrolytic cell into an anode region and a cathode region; adding equal volume of sodium chloride aqueous solution as electrolyte in the anode region and the cathode region, and performing constant current electrolysis to obtain oxidized electrolyzed water in the anode region; adding the prepared oxidized electrolyzed water into an activation chamber, generating low-temperature plasma in a glow discharge mode by taking nitrogen and oxygen as carrier gas, spraying the low-temperature plasma into the oxidized electrolyzed water, and carrying out related chemical reaction with the oxidized electrolyzed water, thereby preparing the active oxygen/active nitrogen enhanced oxidized electrolyzed water high-efficiency bactericide rich in active chlorine, active oxygen and active nitrogen. The active oxygen/active nitrogen enhanced oxidized electrolyzed water has the advantages of high sterilization efficiency, broad sterilization spectrum, wide application range, convenient use and green and environment-friendly novel bactericide.
Description
Technical Field
The invention belongs to the field of preparation of novel environment-friendly bactericides, and particularly relates to active oxygen/active nitrogen enhanced oxidized electrolyzed water as well as a preparation method and application thereof.
Background
Food-borne diseases widely exist all over the world, the incidence rate of the food-borne diseases is the top of the overall incidence rate of various diseases, the food-borne diseases are the most prominent health problems in the world at present, and the food-borne diseases are directly related to the life safety and health of people. Statistically, more than 80% of bacterial infections are associated with bacterial biofilms in food processing equipment. Bacterial biofilms are multi-cellular complex microbial communities with three-dimensional self-assembled extracellular polymeric substance structures (exopolysaccharides, proteins, extracellular DNA, etc.). Biofilm cells are more resistant to bactericides than planktonic cells, and therefore they are extremely difficult to eliminate. Therefore, the research on the novel food sterilization technology which has wide adaptability, high efficiency, broad spectrum, safety, no residue and strong applicability has important strategic significance.
The oxidation electrolysis water bactericide is an electrochemical sterilization technology which is widely researched in recent years. The sterilization efficiency of the oxidation electrolysis water is superior to that of common food bactericides (sodium hypochlorite, ozone, chlorine dioxide and the like), and the oxidation electrolysis water is harmless to human bodies, has little environmental residue and is a safe disinfectant. However, the killing effect of the oxidation electrolysis water on the bacterial biofilm in the food processing equipment is far lower than that of the bacterial planktonic cells at present. This is because bacterial biofilms are a complex microbial community, and extracellular polymers secreted by microorganisms can protect internal cells, so that active chlorine bactericidal factors in the electrolyzed oxidizing water cannot easily permeate into the cells and complete sterilization.
In summary, food-borne pathogens that persist in food processing facilities grow primarily as biofilms. The biological envelope cells have strong resistance to the bactericide, and a novel bactericide which is efficient and environment-friendly is not available at present.
Disclosure of Invention
The invention aims to solve the problems and obtain enhanced oxidized electrolyzed water with certain active chlorine content and certain active oxygen/active nitrogen content by increasing the active oxygen and active nitrogen content of the oxidized electrolyzed water. The active oxygen/active nitrogen enhanced oxidized electrolyzed water has high-efficiency bactericidal effect on pathogenic microorganism envelopes.
In order to achieve the above object, a first aspect of the present invention provides a method for producing active oxygen/active nitrogen enhanced oxidized electrolyzed water, the method comprising:
s1: preparation of oxidized electrolyzed water: in an ion exchange membrane electrolytic cell, a homogeneous ion exchange membrane is adopted to divide the electrolytic cell into a cathode area and an anode area; respectively adding sodium chloride aqueous solution as electrolyte in a cathode area and an anode area, and performing constant current electrolysis to obtain acidic oxidation electrolyzed water in the anode area and alkaline reduction electrolyzed water in the cathode area;
s2: preparing active oxygen/active nitrogen enhanced oxidation electrolyzed water: placing the oxidized electrolyzed water prepared in the step S1 in an activation chamber, and placing a plasma generator spray head above or below the oxidized electrolyzed water solution; taking a carrier gas containing nitrogen and oxygen as an excitation gas source, and generating low-temperature plasma in a glow discharge mode; and the active oxygen/active nitrogen enhanced oxidized electrolyzed water rich in active chlorine, active oxygen and active nitrogen is obtained by injecting the active oxygen/active nitrogen enhanced oxidized electrolyzed water into oxidized electrolyzed water and carrying out chemical reaction with the oxidized electrolyzed water.
According to the invention, the obtained active oxygen/active nitrogen enhanced oxidation electrolyzed water has acidity, and can influence the normal physiological metabolism of cells to inactivate the cells. Meanwhile, the active oxygen/active nitrogen enhanced oxidation electrolyzed water also has higher oxidizability, and can carry out oxidation damage on cells. The active oxygen/active nitrogen enhanced oxidation electrolyzed water contains active chlorine, active oxygen and active nitrogen, wherein the active oxygen/active nitrogen is favorable for oxidizing and destroying extracellular polymers of bacterial biofilm, cell walls of bacteria can be weakened through reaction with carbon-hydrogen bonds, intramolecular bonds of peptidoglycan can be destroyed to cause cell wall rupture, the oxidative stress of microbial cell membranes is caused, the surface structure and the chemical state of the bacteria are changed, and therefore the active chlorine can smoothly permeate into cells to cause DNA decomposition, protein destruction and other internal component damage.
Preferably, in step S1, the anode is a titanium-based iridium oxide composite electrode, and the cathode is a titanium plate electrode.
The current can be better adjusted by controlling the distance between the cathode plate and the anode plate. Preferably, the distance between the cathode plate and the anode plate is 0.5-5 cm, preferably 1-3 cm.
Preferably, in step S1, the homogeneous ion exchange membrane is a homogeneous cation exchange membrane or a homogeneous anion exchange membrane. Preferably a cation exchange membrane is used.
The concentration of sodium chloride is too low to generate effective chlorine with certain concentration through electrolysis; the concentration of sodium chloride is too high, and the content of residual chloride ions in the solution after electrolysis is too high. By controlling the concentration of the sodium chloride aqueous solution, the influence of the concentration of the sodium chloride on the content of the available chlorine is avoided. Preferably, in step S1, the concentration of the aqueous solution of sodium chloride is 0.5-5 g/L, more preferably 1-3 g/L.
Preferably, in step S1, the constant current density of the constant current electrolysis is 1-10 mA/cm2More preferably 2 to 7mA/cm2。
Preferably, in step S1, the electrolysis time is 1-60 min, more preferably 10-30 min.
Under the conditions of constant current density and electrolysis time of constant current electrolysis, the content of available chlorine can be more effectively influenced, and the available chlorine with the content of 10-200 mg/L is generated.
According to the invention, the acidic electrolyzed oxidizing water obtained by the method meets the condition that the oxidation-reduction potential value is more than or equal to 1100 mV.
According to the invention, the acidic oxidation electrolyzed water obtained by the method meets the requirement that the effective chlorine content is 10-200 mg/L.
According to the invention, the acidic electrolyzed oxidizing water obtained by the method meets the condition that the pH value is less than or equal to 3.00.
Preferably, in step S2, the volume ratio of nitrogen to oxygen in the carrier gas is (2-4): 1.
the pressure of the carrier gas is within a certain range to perform plasma discharge. The carrier gas pressure is too low to generate plasma; too high carrier gas pressure affects discharge efficiency, resulting in a large amount of carrier gas not being ionized. Preferably, in step S2, the pressure of the carrier gas is 0.1 to 0.3MPa, more preferably 0.12 to 0.16 MPa.
The discharge current affects the plasma generation efficiency. When the discharge current is too low, sufficient plasma cannot be generated. The discharge current is too high and the energy consumption is increased. Preferably, in step S2, the glow discharge current is 2.00 to 4.00A, more preferably 3.00 to 3.50A.
The activation time will affect the amount of reactive oxygen species and reactive nitrogen species generated. Preferably, in step S2, the activation time is 0.5 to 60min, and more preferably 1 to 20 min.
Preferably, in step S2, the activated volume is 50-200 mL.
Preferably, in step S2, the low-temperature plasma activation may be performed by discharging on water or discharging under water.
Preferably, in step S2, the distance between the plasma jet probe and the liquid is 50-80 mm (water activation) or 10-20 mm (underwater activation).
A second aspect of the present invention provides active oxygen/active nitrogen-enhanced oxidized electrolyzed water obtained by the above-described method for producing active oxygen/active nitrogen-enhanced oxidized electrolyzed water.
According to the invention, the pH value of the active oxygen/active nitrogen enhanced oxidation electrolyzed water obtained by the method is less than or equal to 2.50. The reduction of pH is beneficial to improving the bactericidal activity. After activation, the pH will be further lowered.
According to the invention, the active chlorine content of the active oxygen/active nitrogen enhanced oxidized electrolyzed water obtained by the method is 10-200 mg/L.
According to the invention, the active oxygen content of the active oxygen/active nitrogen enhanced oxidized electrolyzed water obtained by the method is 10-200 mg/L.
According to the invention, the active nitrogen content of the active oxygen/active nitrogen enhanced oxidized electrolyzed water obtained by the method is 10-200 mg/L.
The third aspect of the invention provides the use of the active oxygen/active nitrogen enhanced oxidized electrolyzed water in the preparation of a bactericide.
The technical scheme of the invention has the following beneficial effects:
(1) the active oxygen/active nitrogen enhanced oxidation electrolyzed water high-efficiency bactericide rich in active chlorine, active oxygen and active nitrogen and having high-efficiency sterilization efficiency on pathogenic microorganism envelopes is prepared by the method.
(2) The active oxygen/active nitrogen enhanced oxidized electrolyzed water has the characteristics of safety, environmental protection, no toxicity, no environmental pollution and the like, and has wide applicability.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the following describes preferred embodiments of the present invention, it should be understood that the present invention may be embodied in various forms and should not be limited by the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
In the following examples and comparative examples, cation exchange membranes used in ion exchange membrane cells were purchased from Hangzhou environmental protection technologies, Inc. model number HoCEM Grion 0011T; the anode adopts a titanium-based iridium oxide alloy electrode, and the preparation method is shown in patent number ZL 201410452379.X invention patent example 1, wherein the molar ratio of platinum to iridium is 1: 1. The plasma generator adopts a low-temperature plasma machine produced by Shenzhen Hongshenge electronic technology Limited.
In various embodiments of the present invention, the entire electrolysis reaction is dynamically performed.
Example 1
S1: preparation of oxidized electrolyzed water: in the ion membrane electrolytic cell, a cation exchange membrane is adopted to divide the ion membrane electrolytic cell into a cathode area and an anode area, a titanium-based iridium oxide alloy electrode is adopted as an anode, a titanium plate electrode is adopted as a cathode, the distance between a cathode plate and an anode plate is 2cm, and the effective area of the electrode is 75cm2. 400mL of NaCl solution with a concentration of 1g/L was added as electrolyte in the cathode and anode regions, respectively. During the electrolysis, the current density is 4.5mA/cm2Electrolyzing for 3min to obtain oxidized electrolyzed water in the anode region. Through detection, the pH value of the electrolyzed oxidizing water is 2.95, the oxidation-reduction potential value is 1125mV, and the available chlorine is 18.06 mg/L.
S2: preparing active oxygen/active nitrogen enhanced oxidation electrolyzed water: placing the oxidized electrolyzed water prepared in the step S1 in an activation chamber, and placing a plasma generator spray head above or below the oxidized electrolyzed water solution; taking a carrier gas containing nitrogen and oxygen as an excitation gas source, and generating low-temperature plasma in a glow discharge mode; and the active oxygen/active nitrogen enhanced oxidized electrolyzed water rich in active chlorine, active oxygen and active nitrogen is obtained by injecting the active oxygen/active nitrogen enhanced oxidized electrolyzed water into oxidized electrolyzed water and carrying out chemical reaction with the oxidized electrolyzed water.
The activation conditions were: the gas source type is mixed gas of nitrogen and oxygen with a ratio of 4:1, the pressure value of carrier gas is about 0.13MPa, the discharge current is 3.04A, the activation volume is 50mL, the distance between a plasma jet probe and liquid is 80mm (on water), and the activation time is 3 min. The pH value of the prepared active oxygen/active nitrogen enhanced oxidation electrolyzed water is 2.41; the oxidation-reduction potential value is 609 mV; the concentration of the hydrogen peroxide is 47.66 mg/L; the concentration of nitrate ions is 71.38 mg/L; the nitrite ion concentration was 48.57 mg/L.
Test example 1: sterilizing effect of active oxygen/active nitrogen enhanced oxidation electrolyzed water
And (3) washing the bacillus subtilis biofilm stainless steel sheet cultured for more than 7 days with a PBS (phosphate buffer solution) solution for 2-3 times. And (3) putting the stainless steel sheet into 10mL of active oxygen/active nitrogen enhanced oxidation electrolyzed water, and treating for 10 s. The stainless steel sheet was taken out and placed in a PE tube containing 10mL of 0.5% sodium thiosulfate solution (neutralizer) and allowed to stand for 10min, and the stainless steel sheet was transferred into 10mL of sterilized physiological saline and subjected to ultrasonication for 15min (100W, 25 ℃). After gradient dilution, a proper gradient is selected for plate culture, and counting is carried out after 24h of culture at 37 ℃. In the control group, a Bacillus subtilis biofilm stainless steel sheet cultured for more than 7 days is taken, washed with PBS solution for 2-3 times, put into 10mL sterilized normal saline, and subjected to ultrasonic treatment for 15min (100W, 25 ℃)After gradient dilution, a proper gradient is selected for plate culture, and counting is carried out after 24h of culture at 37 ℃. The calculated killing logarithm value is 1.76log10 CFU。
Example 2
S1: preparation of oxidized electrolyzed water: in the ion membrane electrolytic cell, a cation exchange membrane is adopted to divide the ion membrane electrolytic cell into a cathode area and an anode area, a titanium-based iridium oxide alloy electrode is adopted as an anode, a titanium plate electrode is adopted as a cathode, the distance between a cathode plate and an anode plate is 4cm, and the effective area of the electrode is 75cm2. 400mL of NaCl solution with the concentration of 2g/L is respectively added in the cathode area and the anode area to be used as electrolyte. During the electrolysis, the current density is 4.5mA/cm2Electrolyzing for 15min to obtain oxidized electrolyzed water in the anode area. Through detection, the pH value of the electrolyzed oxidizing water is 2.69, the oxidation-reduction potential value is 1171mV, and the available chlorine is 84.04 mg/L.
S2: preparing active oxygen/active nitrogen enhanced oxidation electrolyzed water: placing the oxidized electrolyzed water prepared in the step S1 in an activation chamber, and placing a plasma generator spray head above or below the oxidized electrolyzed water solution; taking a carrier gas containing nitrogen and oxygen as an excitation gas source, and generating low-temperature plasma in a glow discharge mode; and the active oxygen/active nitrogen enhanced oxidized electrolyzed water rich in active chlorine, active oxygen and active nitrogen is obtained by injecting the active oxygen/active nitrogen enhanced oxidized electrolyzed water into oxidized electrolyzed water and carrying out chemical reaction with the oxidized electrolyzed water.
The activation conditions were: the air source type is compressed air, the pressure value of carrier gas is about 0.15MPa, the discharge current is 3.04A, the activation volume is 200mL, the distance between a plasma jet probe and liquid is 80mm (on water), and the activation time is 10 min. The pH value of the prepared active oxygen/active nitrogen enhanced oxidation electrolyzed water is 2.22; the oxidation-reduction potential value is 653 mV; the concentration of hydrogen peroxide is 22.39 mg/L; the concentration of nitrate ions is 53.93 mg/L; the nitrite ion concentration was 13.76 mg/L.
Test example 2: sterilizing effect of active oxygen/active nitrogen enhanced oxidized electrolyzed water
The sterilization process was the same as in example 1, and the calculated kill log was 1.50log10 CFU。
Example 3
S1: preparation of oxidized electrolyzed water: in the ion membrane electrolytic cell, a cation exchange membrane is adopted to divide the ion membrane electrolytic cell into a cathode area and an anode area, a titanium-based iridium oxide alloy electrode is adopted as an anode, a titanium plate electrode is adopted as a cathode, the distance between a cathode plate and an anode plate is 2cm, and the effective area of the electrode is 75cm2. 400mL of NaCl solution with the concentration of 5g/L is respectively added in the cathode area and the anode area to be used as electrolyte. During the electrolysis, the current density is 7.0mA/cm2Electrolyzing for 30min to obtain oxidized electrolyzed water in the anode area. Through detection, the pH value of the electrolyzed oxidizing water is 2.33, the oxidation-reduction potential value is 1192mV, and the available chlorine is 145.83 mg/L.
S2: preparing active oxygen/active nitrogen enhanced oxidation electrolyzed water: placing the oxidized electrolyzed water prepared in the step S1 in an activation chamber, and placing a plasma generator spray head above or below the oxidized electrolyzed water solution; taking a carrier gas containing nitrogen and oxygen as an excitation gas source, and generating low-temperature plasma in a glow discharge mode; and the active oxygen/active nitrogen enhanced oxidized electrolyzed water rich in active chlorine, active oxygen and active nitrogen is obtained by injecting the active oxygen/active nitrogen enhanced oxidized electrolyzed water into oxidized electrolyzed water and carrying out chemical reaction with the oxidized electrolyzed water.
The activation conditions were: the gas source type is a mixed gas of nitrogen and oxygen with a 2:1 ratio, the pressure value of carrier gas is about 0.20MPa, the current is 3.50A, the activation volume is 200mL, the distance between a plasma jet probe and liquid is 50mm (on water), and the activation time is 20 min. The pH value of the prepared active oxygen/active nitrogen enhanced oxidation electrolyzed water is 2.41; the oxidation-reduction potential value is 637 mV; the concentration of the hydrogen peroxide is 116.16 mg/L; the concentration of nitrate ions is 140.79 mg/L; the nitrite ion concentration was 134.93 mg/L.
Test example 3: sterilizing effect of active oxygen/active nitrogen enhanced oxidized electrolyzed water
The sterilization process was the same as in example 1, and the calculated kill log was 2.87log10 CFU。
Example 4
S1: preparation of oxidized electrolyzed water: in an ion-exchange membrane cell, anion exchange is usedThe membrane-ion membrane electrolytic cell is divided into a cathode area and an anode area, wherein the anode adopts a titanium-based iridium oxide alloy electrode, the cathode adopts a titanium plate electrode, the distance between a cathode plate and an anode plate is 2cm, and the effective area of the electrode is 75cm2. 400mL of NaCl solution with a concentration of 1g/L was added as electrolyte in the cathode and anode regions, respectively. During the electrolysis, the current density is 4.5mA/cm2Electrolyzing for 8min to obtain oxidized electrolyzed water in the anode area. Through detection, the pH value of the electrolyzed oxidizing water is 2.83, the oxidation-reduction potential value is 1152mV, and the available chlorine is 45.83 mg/L.
S2: preparing active oxygen/active nitrogen enhanced oxidation electrolyzed water: placing the oxidized electrolyzed water prepared in the step S1 in an activation chamber, and placing a plasma generator spray head above or below the oxidized electrolyzed water solution; taking a carrier gas containing nitrogen and oxygen as an excitation gas source, and generating low-temperature plasma in a glow discharge mode; and the active oxygen/active nitrogen enhanced oxidized electrolyzed water rich in active chlorine, active oxygen and active nitrogen is obtained by injecting the active oxygen/active nitrogen enhanced oxidized electrolyzed water into oxidized electrolyzed water and carrying out chemical reaction with the oxidized electrolyzed water.
The activation conditions were: the gas source type is mixed gas of nitrogen and oxygen with a ratio of 4:1, the pressure value of carrier gas is about 0.13MPa, the current is 3.04A, the activation volume is 200mL, the distance between a plasma jet probe and liquid is 20mm (underwater), and the activation time is 3 min. The pH value of the prepared active oxygen/active nitrogen enhanced oxidation electrolyzed water is 2.41; the oxidation-reduction potential value is 637 mV; the concentration of hydrogen peroxide is 16.16 mg/L; the concentration of nitrate ions is 40.79 mg/L; the nitrite ion concentration was 34.93 mg/L.
Test example 4: sterilizing effect of active oxygen/active nitrogen enhanced oxidized electrolyzed water
The sterilization process was the same as in example 1, and the calculated kill log was 1.48log10 CFU。
Example 5
S1: preparation of oxidized electrolyzed water: in the ion membrane electrolytic cell, a cation exchange membrane is adopted to divide the ion membrane electrolytic cell into a cathode area and an anode area, a titanium-based iridium oxide alloy electrode is adopted as an anode, a titanium plate electrode is adopted as a cathode, a cathode plate and an anode plateThe distance between the anode plates is 2cm, and the effective area of the electrode is 75cm2. 400mL of NaCl solution with a concentration of 1g/L was added as electrolyte in the cathode and anode regions, respectively. During the electrolysis, the current density is 4.5mA/cm2Electrolyzing for 3min to obtain oxidized electrolyzed water in the anode region. Through detection, the pH value of the electrolyzed oxidizing water is 2.95, the oxidation-reduction potential value is 1125mV, and the available chlorine is 18.06 mg/L.
S2: preparing active oxygen/active nitrogen enhanced oxidation electrolyzed water: placing the oxidized electrolyzed water prepared in the step S1 in an activation chamber, and placing a plasma generator spray head above or below the oxidized electrolyzed water solution; taking a carrier gas containing nitrogen and oxygen as an excitation gas source, and generating low-temperature plasma in a glow discharge mode; and the active oxygen/active nitrogen enhanced oxidized electrolyzed water rich in active chlorine, active oxygen and active nitrogen is obtained by injecting the active oxygen/active nitrogen enhanced oxidized electrolyzed water into oxidized electrolyzed water and carrying out chemical reaction with the oxidized electrolyzed water.
The activation conditions were: the gas source type is mixed gas of nitrogen and oxygen with a ratio of 4:1, the pressure value of carrier gas is about 0.13MPa, the discharge current is 3.04A, the activation volume is 50mL, the distance between a plasma jet probe and liquid is 80mm (on water), and the activation time is 3 min. The pH value of the prepared active oxygen/active nitrogen enhanced oxidation electrolyzed water is 2.41; the oxidation-reduction potential value is 609 mV; the concentration of the hydrogen peroxide is 47.66 mg/L; the concentration of nitrate ions is 71.38 mg/L; the nitrite ion concentration was 48.57 mg/L.
Test example 5: sterilizing effect of active oxygen/active nitrogen enhanced oxidized electrolyzed water
1ml of the colony is taken and the concentration is 105CFU/mL of Bacillus subtilis suspension, 9mL of active oxygen/active nitrogen enhanced oxidation electrolysis water is added, and the sterilization effect is 10 s. Then, 1mL of the above mixed solution was removed, and 9mL of a 0.5% sodium thiosulfate solution was added to neutralize the solution for 10 min. Taking 0.1mL for plate counting culture; culturing at 36 + -1 deg.C for 24 h. The log of killing log value obtained by calculation is 2.03log10 CFU。
Comparative example 1
In the ion membrane electrolytic cell, a cation exchange membrane is adopted to divide the ion membrane electrolytic cell into a cathode area and an anode area,the anode adopts a titanium-based iridium oxide alloy electrode, the cathode adopts a titanium plate electrode, the distance between a cathode plate and an anode plate is 2cm, and the effective area of the electrode is 75cm2. 400mL of NaCl solution with a concentration of 1g/L was added as an electrolyte in the cathode and anode regions. During the electrolysis, the current density is 4.5mA/cm2Electrolyzing for 5min to obtain oxidized electrolyzed water in the anode region. The pH value of the electrolyzed oxidizing water is detected to be 2.93, the oxidation-reduction potential value is 1129mV, and the available chlorine is 19.61 mg/L.
Test example 6: sterilizing effect of oxidized electrolyzed water
The sterilization procedure was the same as in example 1, with a calculated inhibition of 38.44%, expressed as log kill log 0.2110 CFU。
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.
Claims (10)
1. A method for preparing active oxygen/active nitrogen enhanced oxidized electrolyzed water is characterized by comprising the following steps:
s1: preparation of oxidized electrolyzed water: in an ion exchange membrane electrolytic cell, a homogeneous ion exchange membrane is adopted to divide the electrolytic cell into a cathode area and an anode area; respectively adding sodium chloride aqueous solution as electrolyte in a cathode area and an anode area, and performing constant current electrolysis to obtain acidic oxidation electrolyzed water in the anode area and alkaline reduction electrolyzed water in the cathode area;
s2: preparing active oxygen/active nitrogen enhanced oxidation electrolyzed water: placing the oxidized electrolyzed water prepared in the step S1 in an activation chamber, and placing a plasma generator spray head above or below the oxidized electrolyzed water solution; taking a carrier gas containing nitrogen and oxygen as an excitation gas source, and generating low-temperature plasma in a glow discharge mode; and the active oxygen/active nitrogen enhanced oxidized electrolyzed water rich in active chlorine, active oxygen and active nitrogen is obtained by injecting the active oxygen/active nitrogen enhanced oxidized electrolyzed water into oxidized electrolyzed water and carrying out chemical reaction with the oxidized electrolyzed water.
2. The method of producing activated oxygen/activated nitrogen enhanced oxygenated electrolyzed water as claimed in claim 1, wherein in step S1,
the anode adopts a titanium-based iridium oxide composite electrode, and the cathode adopts a titanium plate electrode;
the distance between the cathode plate and the anode plate is 0.5-5 cm;
the homogeneous phase ion exchange membrane is a homogeneous phase cation exchange membrane or a homogeneous phase anion exchange membrane.
3. The method for producing activated oxygen/activated nitrogen enhanced oxidized electrolyzed water according to claim 1, wherein in step S1, the concentration of the aqueous sodium chloride solution is 0.5 to 5 g/L.
4. The method for producing activated oxygen/activated nitrogen enhanced oxidized electrolyzed water according to claim 1, wherein in step S1, the constant current density of constant current electrolysis is 1 to 10mA/cm2The electrolysis time is 1-60 min.
5. The method for producing activated oxygen/activated nitrogen enhanced oxidized electrolyzed water according to claim 1, wherein in step S1, the obtained acidic oxidized electrolyzed water satisfies:
the oxidation-reduction potential value is more than or equal to 1100 mV;
the content of available chlorine is 10-200 mg/L;
the pH value is less than or equal to 3.00.
6. The method for producing activated oxygen/activated nitrogen enhanced oxidized electrolyzed water according to claim 1, wherein in step S2,
the volume ratio of nitrogen to oxygen in the carrier gas is (2-4): 1;
the pressure of the carrier gas is 0.1-0.3 MPa.
7. The method for producing activated oxygen/activated nitrogen enhanced oxidized electrolyzed water according to claim 1, wherein in step S2,
the current of glow discharge is 2.00-4.00A;
the activation time is 0.5-60 min.
8. The active oxygen/active nitrogen-enhanced oxidized electrolyzed water obtained by the method for producing active oxygen/active nitrogen-enhanced oxidized electrolyzed water according to any one of claims 1 to 7.
9. The active oxygen/active nitrogen enhanced oxygenated electrolyzed water of claim 8,
the pH value of the active oxygen/active nitrogen enhanced oxidation electrolyzed water is less than or equal to 2.50;
the active chlorine content of the active oxygen/active nitrogen enhanced oxidized electrolyzed water is 10-200 mg/L;
the active oxygen content of the active oxygen/active nitrogen enhanced oxidized electrolyzed water is 10-200 mg/L;
the active nitrogen content of the active oxygen/active nitrogen enhanced oxidized electrolyzed water is 10-200 mg/L.
10. Use of the active oxygen/active nitrogen enhanced oxidized electrolyzed water according to claim 8 or 9 for producing a bactericide.
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