CN110950306A - Method for generating singlet oxygen by activating peroxydisulfate through hydroxyl-rich metal oxide - Google Patents
Method for generating singlet oxygen by activating peroxydisulfate through hydroxyl-rich metal oxide Download PDFInfo
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- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 50
- 125000002887 hydroxy group Chemical group [H]O* 0.000 title claims abstract description 44
- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 42
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 42
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 title claims abstract description 35
- 230000003213 activating effect Effects 0.000 title claims abstract description 25
- 239000011259 mixed solution Substances 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 14
- 239000001257 hydrogen Substances 0.000 claims abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000000395 magnesium oxide Substances 0.000 claims description 14
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 14
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical group [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 14
- 150000003839 salts Chemical class 0.000 claims description 9
- DQYBDCGIPTYXML-UHFFFAOYSA-N ethoxyethane;hydrate Chemical compound O.CCOCC DQYBDCGIPTYXML-UHFFFAOYSA-N 0.000 claims description 7
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 4
- 239000000920 calcium hydroxide Substances 0.000 claims description 4
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 4
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 4
- 239000000347 magnesium hydroxide Substances 0.000 claims description 4
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 4
- 125000005385 peroxodisulfate group Chemical group 0.000 claims description 4
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 claims description 4
- 229940007718 zinc hydroxide Drugs 0.000 claims description 4
- 229910021511 zinc hydroxide Inorganic materials 0.000 claims description 4
- ZQXSFZAMFNRZOQ-UHFFFAOYSA-N 2-methylpropan-2-ol;hydrate Chemical compound O.CC(C)(C)O ZQXSFZAMFNRZOQ-UHFFFAOYSA-N 0.000 claims description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 3
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical group O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 claims description 3
- -1 hydrogen persulfate salt Chemical class 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 6
- 239000001301 oxygen Substances 0.000 abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 abstract description 6
- 239000003344 environmental pollutant Substances 0.000 abstract description 4
- 231100000719 pollutant Toxicity 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 9
- 239000000126 substance Substances 0.000 description 8
- 208000017983 photosensitivity disease Diseases 0.000 description 4
- 231100000434 photosensitization Toxicity 0.000 description 4
- 239000003504 photosensitizing agent Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 229910001882 dioxygen Inorganic materials 0.000 description 3
- 230000005281 excited state Effects 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000005283 ground state Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- HDMGAZBPFLDBCX-UHFFFAOYSA-M potassium;sulfooxy sulfate Chemical compound [K+].OS(=O)(=O)OOS([O-])(=O)=O HDMGAZBPFLDBCX-UHFFFAOYSA-M 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- AQRLNPVMDITEJU-UHFFFAOYSA-N triethylsilane Chemical compound CC[SiH](CC)CC AQRLNPVMDITEJU-UHFFFAOYSA-N 0.000 description 2
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000005708 Sodium hypochlorite Substances 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000001362 electron spin resonance spectrum Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000005298 paramagnetic effect Effects 0.000 description 1
- 150000004032 porphyrins Chemical class 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- WVMSIBFANXCZKT-UHFFFAOYSA-N triethyl(hydroxy)silane Chemical compound CC[Si](O)(CC)CC WVMSIBFANXCZKT-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/02—Preparation of oxygen
- C01B13/0203—Preparation of oxygen from 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to a method for activating peroxydisulfate by a hydroxyl-rich metal oxide to generate singlet oxygen, which comprises the steps of adding the hydroxyl-rich metal oxide and the peroxydisulfate into a solvent to obtain a mixed solution, stirring the mixed solution at the temperature of between 10 and 30 ℃ for reaction, wherein the mass concentration of the hydroxyl-rich metal oxide in the mixed solution is as follows: 0.1-2.0 g/L, wherein the concentration of the hydrogen persulfate in the mixed solution is as follows: 0.20 to 5.00 mmol/L. The method provided by the invention has the advantages that the generation of singlet oxygen is realized immediately after the reaction, no other active oxygen species are generated in the whole reaction process, the efficient and directional generation of the singlet oxygen is realized, the activity of the singlet oxygen is not affected at all, pollutants can be efficiently degraded, and the used activating agent is nontoxic and harmless.
Description
Technical Field
The invention relates to a method for generating singlet oxygen by activating peroxydisulfate with hydroxyl-rich metal oxide, belonging to the field of water treatment.
Background
Singlet oxygen (1O2) Is the lowest excited state of diatomic oxygen molecules, also called excited state oxygen molecules, and has different physical and chemical properties from diatomic oxygen molecules. Singlet oxygen is in a quantum state in which all electrons spin in pairs, is paramagnetic, is dynamically unstable at ambient temperature, and decays very slowly. The singlet oxygen has strong oxidability and good reactivity with organic compounds, and can be applied to organic synthesis and medicinesThe method comprises the following fields of synthesis, sterilization, disinfection, cancer treatment, environmental remediation, pollutant treatment and the like. Traces of singlet oxygen are present in the upper atmosphere and in polluted urban atmosphere, which contributes to the formation of nitrogen dioxide, which is harmful to the lungs.
Due to the high forbidden resistance of transition, the light absorption of the diatomic oxygen molecule in the ground state is impossible to directly generate singlet oxygen; singlet oxygen can be obtained by photosensitization methods, microwave discharge methods and chemical methods.
The photosensitization method is that the photosensitizer transits to an excited state under the condition of illumination, and then transfers energy to ground state oxygen molecules to form singlet oxygen. However, the method currently has the following problems: 1. the photosensitizer used generally is a toxic and harmful substance (such as porphyrin photosensitizer with high toxicity), so the application of the method in the fields of biomedicine, water treatment and the like is limited; 2. the photosensitizer used in the method is generally a water-soluble substance, which is not beneficial to subsequent separation; 3. when singlet oxygen is generated, the method is often accompanied with the generation of other active oxygen species (such as superoxide radical, hydroxyl radical and the like), and the singlet oxygen cannot be efficiently and directionally generated.
One commonly used chemical method is to decompose triethylsilyl hydroxide generated in situ from triethylsilane and ozone, further decomposing to obtain singlet oxygen, and the other is to react hydrogen peroxide with sodium hypochlorite in water. The prior common preparation method has the problems of inconvenient transportation of raw materials, high cost, inconvenient use, incapability of on-site preparation and the like.
Aiming at the defects of the existing photosensitization method and chemical method, a method which has low cost, convenient transportation and use, high efficiency, no toxicity and no harm and can generate singlet oxygen is needed to be developed.
Disclosure of Invention
Aiming at the defects of the existing photosensitization method and chemical method, the invention provides a method for generating singlet oxygen by activating peroxydisulfate with hydroxyl-rich metal oxide.
The invention achieves the following aims:
1. can quickly and efficiently generate singlet oxygen, does not generate other active oxygen species when generating the singlet oxygen, and can generate directionally.
2. The used activating agent is non-toxic and harmless, has no secondary pollution in reaction, low cost, convenient transportation and use and convenient subsequent separation.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
a method for activating a hydrogen persulfate salt to generate singlet oxygen by a hydroxyl-rich metal oxide, comprising the steps of:
adding the hydroxyl-rich metal oxide and hydrogen persulfate into a solvent to obtain a mixed solution, and stirring the mixed solution at the temperature of between 10 and 30 ℃ for reaction, wherein the mass concentration of the hydroxyl-rich metal oxide in the mixed solution is as follows: 0.1-2.0 g/L, wherein the concentration of the hydrogen persulfate in the mixed solution is as follows: 0.20 to 5.00 mmol/L.
Preferably, according to the present invention, the hydroxyl-rich metal oxide is magnesium oxide, magnesium hydroxide, calcium hydroxide, aluminum hydroxide or zinc hydroxide.
Most preferably, the hydroxyl-rich metal oxide is magnesium oxide.
According to the invention, the preferred peroxodisulfate is oxone complex salt or sodium peroxodisulfate complex salt.
More preferably, the peroxodisulfate is a oxone complex salt.
According to the invention, the mixed solution preferably contains the following hydroxyl-rich metal oxides in mass concentration: 0.1-1.0 g/L, wherein the concentration of the hydrogen persulfate in the mixed solution is as follows: 0.20 to 4.00 mmol/L.
Further preferably, the mass concentration of the hydroxyl-rich metal oxide in the mixed solution is as follows: 0.4-1.0 g/L, wherein the concentration of the hydrogen persulfate in the mixed solution is as follows: 0.50 to 3.00 mmol/L.
According to the invention, the solvent is preferably water, alcohol-water or ether-water; the alcohol-water is methanol-water, ethanol-water or tert-butanol-water, and the ether-water is diethyl ether-water.
According to the present invention, the concentration of the alcohol or ether in the mixed solution is preferably: 200-5000 mmol/L.
Most preferably, the solvent is water.
In the invention, the reaction temperature is preferably 20-30 ℃.
In the present invention, the pH of the mixed solution is preferably 3.0 to 11.0.
More preferably, the pH of the mixed solution is 3.0 to 9.0.
Preferably, the reaction time is as follows: 0.5-2 h.
The invention preferably adopts a technical scheme that a method for generating singlet oxygen by activating peroxydisulfate with hydroxyl-rich metal oxide comprises the following steps:
adding the hydroxyl-rich metal oxide and the hydrogen persulfate into a water solvent, and stirring at 20-30 ℃ for reaction, wherein the pH of a reaction solution is 3.0-9.0, and the mass concentration of the hydroxyl-rich metal oxide in a mixed solution is as follows: 0.4-1.0 g/L, wherein the concentration of the hydrogen persulfate in the mixed solution is as follows: 0.50 to 3.00 mmol/L.
The principle of the hydroxyl-rich metal oxide activating the peroxydisulfate to generate singlet oxygen is as follows:
the hydroxyl-rich metal oxide is added into water, water molecules and the metal oxide are subjected to matching copolymerization, a large amount of hydroxyl is generated on the surface of the oxide, hydroxyl induces the peroxydisulfate to form a diepoxy intermediate, the diepoxy intermediate can be decomposed automatically to generate singlet oxygen, the generated singlet oxygen degrades pollutants to achieve the purpose of removing pollution, and the released hydroxyl-rich oxide continuously catalyzes the peroxydisulfate to realize the circulating catalysis effect.
The raw materials and equipment used in the invention are all the prior art.
The invention has the following advantages:
1. according to the method, the generation of singlet oxygen is immediately started at the beginning of the reaction, and no other active oxygen species are generated in the whole reaction process, so that the efficient and directional generation of the singlet oxygen is realized;
2. when the singlet oxygen is generated, the method does not need to add any toxic and harmful substance, and the whole reaction process is green and environment-friendly, so the method can be popularized and used in the fields of biomedicine, water purification and the like.
3. The method has the advantages of cheap and easily obtained raw materials, convenient transportation, mild reaction process, high efficiency, no secondary pollution in reaction, low toxicity and wide pH range. The method can play an important role in the field of environmental management.
Drawings
FIG. 1 is a singlet oxygen ESR spectrum measured in application test example 1.
FIG. 2 is a graph showing the effect of singlet oxygen generated by various metal oxides rich in hydroxyl groups on the degradation of bisphenol A in Experimental example 2.
Detailed Description
The present invention is further illustrated by, but is not limited to, the following specific examples.
The raw materials used in the following examples are all commercially available products and were analytically pure.
Example 1:
a method for activating hydrogen persulfate to generate singlet oxygen by using a hydroxyl-rich metal oxide comprises the following steps:
0.5g of magnesium oxide and 0.21g of potassium hydrogen persulfate composite salt are weighed and dispersed in 1L of water to obtain a mixed solution, the mixed solution is stirred and reacted for 1h at the temperature of 25 ℃, sampling and filtering are carried out, a TEMP probe ESR is used for detection, and singlet oxygen is generated in the reaction solution.
Example 2:
the method for activating a persulfate to produce singlet oxygen with a metal oxide rich in hydroxyl groups as described in example 1, except that: sodium peroxodisulfate is used instead of oxone.
Example 3:
the method for activating a persulfate to produce singlet oxygen with a metal oxide rich in hydroxyl groups as described in example 1, except that: magnesium hydroxide is used instead of magnesium oxide.
Example 4:
the method for activating a persulfate to produce singlet oxygen with a metal oxide rich in hydroxyl groups as described in example 1, except that: calcium hydroxide was used instead of magnesium oxide.
Example 5:
the method for activating a persulfate to produce singlet oxygen with a metal oxide rich in hydroxyl groups as described in example 1, except that: aluminum hydroxide was used instead of magnesium oxide.
Example 6:
the method for activating a persulfate to produce singlet oxygen with a metal oxide rich in hydroxyl groups as described in example 1, except that: zinc hydroxide was used instead of magnesium oxide.
Example 7:
the method for activating a persulfate to produce singlet oxygen with a metal oxide rich in hydroxyl groups as described in example 1, except that: ethanol-water was used instead of water.
Example 8:
the method for activating a persulfate to produce singlet oxygen with a metal oxide rich in hydroxyl groups as described in example 1, except that: methanol-water was used instead of water.
Example 9:
the method for activating a persulfate to produce singlet oxygen with a metal oxide rich in hydroxyl groups as described in example 1, except that: ether-water was used instead of water.
Example 10:
the method for activating a persulfate to produce singlet oxygen with a metal oxide rich in hydroxyl groups as described in example 1, except that: tert-butanol-water was used instead of water.
Example 11:
the method for activating a persulfate to produce singlet oxygen with a metal oxide rich in hydroxyl groups as described in example 1, except that: 0.40g of magnesium oxide and 0.10g of oxone complex salt were weighed out and dispersed in 1L of water.
Example 12:
the method for activating a persulfate to produce singlet oxygen with a metal oxide rich in hydroxyl groups as described in example 1, except that: 0.60g of magnesium oxide and 0.15g of oxone complex salt were weighed out and dispersed in 1L of water.
Example 13:
the method for activating a persulfate to produce singlet oxygen with a metal oxide rich in hydroxyl groups as described in example 1, except that: 0.80g of magnesium oxide and 0.26g of oxone complex salt were weighed out and dispersed in 1L of water.
Example 14:
the method for activating a persulfate to produce singlet oxygen with a metal oxide rich in hydroxyl groups as described in example 1, except that: 0.95g of magnesium oxide and 0.35g of oxone complex salt were weighed out and dispersed in 1L of water.
Application test example 1:
the reaction solutions of examples 1, 3, 4, 5 and 6 were filtered, and singlet oxygen in the filtered reaction solutions was detected with a TEMP probe ESR, and the detection results are shown in fig. 1.
Application test example 2:
preparing simulated wastewater of 10mg/L bisphenol A by taking bisphenol A as a model pollutant, respectively weighing 50mg of magnesium oxide, magnesium hydroxide, calcium hydroxide, aluminum hydroxide, zinc hydroxide and 9.22mg of potassium hydrogen persulfate, dispersing in 50mL of the simulated wastewater, sampling 2mL of the wastewater every 10 minutes, filtering, quenching the sample with 0.5mL of ethanol, detecting the concentration of the bisphenol A in the sample by a liquid phase, reacting for 1h, and degrading as shown in figure 2.
An experimental instrument: high Performance Liquid Chromatography (HPLC), model ELITE P1201, instrument equipped with a diode array detector and a C18 reverse phase column (5 μm, 4.6mm 150mm), mobile phase methanol/water (70: 30, v/v), flow rate 1mL/min, column temperature 40 ℃, BPA detection wavelength 278 nm.
Claims (10)
1. A method for activating a hydrogen persulfate salt to generate singlet oxygen by a hydroxyl-rich metal oxide, comprising the steps of:
adding the hydroxyl-rich metal oxide and hydrogen persulfate into a solvent to obtain a mixed solution, and stirring the mixed solution at the temperature of between 10 and 30 ℃ for reaction, wherein the mass concentration of the hydroxyl-rich metal oxide in the mixed solution is as follows: 0.1-2.0 g/L, wherein the concentration of the hydrogen persulfate in the mixed solution is as follows: 0.20 to 5.00 mmol/L.
2. The method of producing singlet oxygen according to claim 1, wherein the hydroxyl-rich metal oxide is magnesium oxide, magnesium hydroxide, calcium hydroxide, aluminum hydroxide, or zinc hydroxide.
3. The method of producing singlet oxygen according to claim 1, wherein the hydroxyl-rich metal oxide is magnesium oxide.
4. The method for producing singlet oxygen according to claim 1, wherein the peroxodisulfate is oxone or oxone.
5. The method for producing singlet oxygen according to claim 1, wherein the peroxodisulfate salt is oxone complex salt.
6. The method of producing singlet oxygen according to claim 1, wherein the mixed liquor contains the following hydroxyl-rich metal oxides in mass concentration: 0.1-1.0 g/L, wherein the concentration of the hydrogen persulfate in the mixed solution is as follows: 0.20 to 4.00 mmol/L.
7. The method of producing singlet oxygen according to claim 1, wherein the mixed liquor contains the following hydroxyl-rich metal oxides in mass concentration: 0.4-1.0 g/L, wherein the concentration of the hydrogen persulfate in the mixed solution is as follows: 0.50 to 3.00 mmol/L.
8. The method for generating singlet oxygen according to claim 1, wherein the solvent is water, alcohol-water or ether-water; the alcohol-water is methanol-water, ethanol-water or tert-butanol-water, and the ether-water is diethyl ether-water.
9. The method for generating singlet oxygen according to claim 1, wherein the solvent is water.
10. The method for generating singlet oxygen according to claim 1, wherein the reaction temperature is 20 ℃ to 30 ℃, the pH of the mixed solution is 3.0 to 11.0, and the reaction time is: 0.5-2 h.
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Cited By (2)
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| CN115606604A (en) * | 2022-09-29 | 2023-01-17 | 中邦(成都)电器有限公司 | Method for using inorganic disinfectant |
| KR20230047239A (en) * | 2021-09-30 | 2023-04-07 | 한국전력공사 | A composition for oxygen carrier material, oxygen carrier using the same and manufacturing method thereof |
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2019
- 2019-12-13 CN CN201911281268.6A patent/CN110950306A/en active Pending
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20230047239A (en) * | 2021-09-30 | 2023-04-07 | 한국전력공사 | A composition for oxygen carrier material, oxygen carrier using the same and manufacturing method thereof |
| KR102574042B1 (en) | 2021-09-30 | 2023-09-07 | 한국전력공사 | A composition for oxygen carrier material, oxygen carrier using the same and manufacturing method thereof |
| CN115606604A (en) * | 2022-09-29 | 2023-01-17 | 中邦(成都)电器有限公司 | Method for using inorganic disinfectant |
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