CN110918009B - Aerogel material, preparation method thereof, catalyst, sulfonamide wastewater degradation method and application - Google Patents
Aerogel material, preparation method thereof, catalyst, sulfonamide wastewater degradation method and application Download PDFInfo
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- 239000002351 wastewater Substances 0.000 title claims abstract description 74
- 229940124530 sulfonamide Drugs 0.000 title claims abstract description 70
- 150000003456 sulfonamides Chemical class 0.000 title claims abstract description 70
- 239000004964 aerogel Substances 0.000 title claims abstract description 69
- 239000000463 material Substances 0.000 title claims abstract description 69
- 239000003054 catalyst Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000006731 degradation reaction Methods 0.000 title abstract description 19
- 230000015556 catabolic process Effects 0.000 title abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 96
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 73
- 239000007864 aqueous solution Substances 0.000 claims abstract description 45
- 239000006185 dispersion Substances 0.000 claims abstract description 39
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 22
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000000017 hydrogel Substances 0.000 claims description 84
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 46
- 238000003756 stirring Methods 0.000 claims description 40
- 239000008367 deionised water Substances 0.000 claims description 39
- 229910021641 deionized water Inorganic materials 0.000 claims description 39
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 23
- 238000002156 mixing Methods 0.000 claims description 22
- 238000004108 freeze drying Methods 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 18
- 230000000593 degrading effect Effects 0.000 claims description 17
- 239000012286 potassium permanganate Substances 0.000 claims description 15
- 238000000502 dialysis Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 13
- FHHJDRFHHWUPDG-UHFFFAOYSA-L peroxysulfate(2-) Chemical compound [O-]OS([O-])(=O)=O FHHJDRFHHWUPDG-UHFFFAOYSA-L 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000005273 aeration Methods 0.000 claims description 10
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- 238000004140 cleaning Methods 0.000 claims description 6
- 238000007710 freezing Methods 0.000 claims 1
- 230000008014 freezing Effects 0.000 claims 1
- 238000007789 sealing Methods 0.000 claims 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 abstract description 15
- 230000003647 oxidation Effects 0.000 abstract description 9
- 230000008901 benefit Effects 0.000 abstract description 5
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- 231100000956 nontoxicity Toxicity 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 30
- 238000006243 chemical reaction Methods 0.000 description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 14
- 238000003760 magnetic stirring Methods 0.000 description 12
- 239000011148 porous material Substances 0.000 description 9
- 239000005457 ice water Substances 0.000 description 6
- HDMGAZBPFLDBCX-UHFFFAOYSA-M potassium;sulfooxy sulfate Chemical compound [K+].OS(=O)(=O)OOS([O-])(=O)=O HDMGAZBPFLDBCX-UHFFFAOYSA-M 0.000 description 6
- 239000013049 sediment Substances 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
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- 230000007547 defect Effects 0.000 description 3
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- 239000002689 soil Substances 0.000 description 3
- WMPXPUYPYQKQCX-UHFFFAOYSA-N Sulfamonomethoxine Chemical compound C1=NC(OC)=CC(NS(=O)(=O)C=2C=CC(N)=CC=2)=N1 WMPXPUYPYQKQCX-UHFFFAOYSA-N 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
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- 238000012986 modification Methods 0.000 description 2
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- 150000003839 salts Chemical class 0.000 description 2
- 229950003874 sulfamonomethoxine Drugs 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 239000012425 OXONE® Substances 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 229940124599 anti-inflammatory drug Drugs 0.000 description 1
- 229940124350 antibacterial drug Drugs 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- LFINSDKRYHNMRB-UHFFFAOYSA-N diazanium;oxido sulfate Chemical compound [NH4+].[NH4+].[O-]OS([O-])(=O)=O LFINSDKRYHNMRB-UHFFFAOYSA-N 0.000 description 1
- YMGGAHMANIOXGP-UHFFFAOYSA-L disodium;oxido sulfate Chemical compound [Na+].[Na+].[O-]OS([O-])(=O)=O YMGGAHMANIOXGP-UHFFFAOYSA-L 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002065 inelastic X-ray scattering Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- HJKYXKSLRZKNSI-UHFFFAOYSA-I pentapotassium;hydrogen sulfate;oxido sulfate;sulfuric acid Chemical compound [K+].[K+].[K+].[K+].[K+].OS([O-])(=O)=O.[O-]S([O-])(=O)=O.OS(=O)(=O)O[O-].OS(=O)(=O)O[O-] HJKYXKSLRZKNSI-UHFFFAOYSA-I 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- GPTONYMQFTZPKC-UHFFFAOYSA-N sulfamethoxydiazine Chemical compound N1=CC(OC)=CN=C1NS(=O)(=O)C1=CC=C(N)C=C1 GPTONYMQFTZPKC-UHFFFAOYSA-N 0.000 description 1
- 229960002229 sulfametoxydiazine Drugs 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
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Abstract
The invention relates to the field of chemical industry, and particularly discloses an aerogel material, a preparation method thereof, a catalyst, a sulfonamide wastewater degradation method and application, wherein the aerogel material comprises the following raw materials: graphene oxide aqueous dispersion and hydrazine hydrate aqueous solution. The aerogel material provided by the embodiment of the invention can efficiently activate persulfate to degrade sulfonamide wastewater, so that an oxidation system formed by the aerogel material and persulfate can effectively degrade sulfonamide wastewater, can be recycled through simple extrusion, avoids secondary pollution to the environment, has the advantages of stability, high efficiency, low cost, no toxicity and the like, and solves the problem that the existing persulfate oxidation method adopts a powdered carbon material as a catalyst, and cannot recycle the catalyst.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to an aerogel material, a preparation method thereof, a catalyst, a sulfonamide wastewater degradation method and application.
Background
Sulfonamides are a class of artificially synthesized broad-spectrum antibacterial and anti-inflammatory drugs commonly used in modern medicine. The sulfonamide wastewater generated in the sulfonamide production process is typical organic wastewater which is difficult to biodegrade, and the removal effect is not ideal by adopting a conventional biological treatment method.
At present, an activated persulfate oxidation method based on a sulfate radical oxidation principle is increasingly applied to the aspect of degrading organic pollutants (particularly to the aspect of degrading sulfonamide wastewater) due to the advantages of economy, high efficiency, environmental friendliness, safety, stability and the like. In general, the activated persulfate oxidation process requires the use of a catalyst to activate persulfate, which in turn generates a large amount of sulfate radicals to completely oxidize organic pollutants in water to water, carbon dioxide and inorganic salts.
When a catalyst is used to activate persulfate, a powdered carbon material is generally used as the catalyst, which has the advantage of being environmentally friendly. However, the conventional powdered carbon material has a defect of easy loss, and cannot realize the recycling of the catalyst.
Disclosure of Invention
The embodiment of the invention aims to provide an aerogel material, a preparation method thereof, a catalyst, a sulfonamide wastewater degradation method and application, and aims to solve the problem that the existing activated persulfate oxidation method provided in the background art adopts a powdered carbon material as the catalyst, and the catalyst cannot be recycled.
In order to achieve the purpose, the invention provides the following technical scheme:
an aerogel material comprises the following raw materials in parts by weight: 29-31 parts of graphene oxide aqueous dispersion and 0.10-0.15 part of hydrazine hydrate aqueous solution, wherein the mass fraction of the hydrazine hydrate aqueous solution is 0-50%, and the concentration of the graphene oxide aqueous dispersion is 3-5 mg/mL.
Preferably, the concentration of the graphene oxide aqueous dispersion is 4 mg/mL.
As a further scheme of the invention: the graphene oxide in the graphene oxide aqueous dispersion comprises the following raw materials in parts by weight: 3-5 parts of graphite powder, 45-55 parts of sulfuric acid aqueous solution, 8-10 parts of potassium permanganate, 38-42 parts of hydrogen peroxide and 450 parts of deionized water, wherein the mass fraction of the sulfuric acid aqueous solution is not less than 70%.
Preferably, the mass fraction of the aqueous sulfuric acid solution is 85%.
As a still further scheme of the invention: the preparation method of the graphene oxide in the graphene oxide aqueous dispersion liquid comprises the following steps: weighing graphite powder according to a proportion, slowly adding the graphite powder into a sulfuric acid aqueous solution for mixing, slowly adding potassium permanganate, stirring at 58-62 ℃, then heating to 95-97 ℃, adding one fourth of deionized water in the total amount of the deionized water for mixing, continuously stirring for 50min, cooling to room temperature, placing on a magnetic stirrer for stirring, adding hydrogen peroxide for oxidation reaction, then adding the rest deionized water for terminating the reaction, and then sequentially centrifuging, cleaning and drying to obtain the catalyst.
Preferably, the preparation method of the graphene oxide in the graphene oxide aqueous dispersion comprises the following steps: weighing graphite powder according to a proportion, slowly adding the graphite powder into a sulfuric acid aqueous solution for mixing, slowly adding potassium permanganate, stirring at 60 ℃, heating to 96 ℃, adding one fourth of deionized water in the total amount of the deionized water for mixing, continuously stirring for 50min, cooling to room temperature, placing on a magnetic stirrer for stirring, adding hydrogen peroxide for oxidation reaction, adding the rest of deionized water for terminating the reaction, and then sequentially centrifuging, cleaning and drying to obtain the graphite powder.
Preferably, the centrifugation is to centrifuge the mixture after the termination reaction for 10min at 4000 r/min; and the cleaning is to wash the graphene oxide with hydrochloric acid solution for 5min, then centrifuge the graphene oxide for 10min at 4000r/min, then wash the graphene oxide with ethanol solution for 10min, then centrifuge the graphene oxide for 10min at 4000r/min, and collect the earthy yellow deposit, wherein the drying is to dry the earthy yellow deposit in vacuum at 80 ℃ for 12h to obtain the graphene oxide.
Another object of an embodiment of the present invention is to provide a method for preparing an aerogel material, including the following steps:
weighing graphene oxide aqueous dispersion according to the weight parts, mixing the graphene oxide aqueous dispersion with a hydrazine hydrate aqueous solution, keeping the mixture at the temperature of 190-210 ℃ for 2-4h, and cooling the mixture to room temperature to obtain hydrogel;
dialyzing the hydrogel to obtain the dialyzed hydrogel;
and (3) freeze-drying the dialyzed hydrogel to obtain the hydrogel.
As a still further scheme of the invention: and the dialysis is to seal the hydrogel in a dialysis bag, then place the hydrogel in deionized water, stand the hydrogel for 7 to 9 hours and take the hydrogel out.
As a still further scheme of the invention: and the dialysis is to seal the hydrogel in a dialysis bag, then place the hydrogel in deionized water for standing for 8 hours, take out the hydrogel and replace the hydrogel again, and repeat the dialysis three times until no impurity ions are separated out.
As a still further scheme of the invention: the freeze drying is to freeze the dialyzed hydrogel at a temperature of between 10 ℃ below zero and 50 ℃ below zero and then dry the dialyzed hydrogel at a pressure of between 1.3 and 13 Pa.
As a still further scheme of the invention: the freeze drying is to place the dialyzed hydrogel in a cold trap of a freeze dryer, pre-freeze the hydrogel for 3 hours at-50 ℃, then place the hydrogel on a tray above the freeze dryer, and freeze-dry the hydrogel for 24 hours under 3Pa, so that the original pore structure of the hydrogel can be maintained.
Another object of the embodiments of the present invention is to provide an aerogel material prepared by the method for preparing an aerogel material.
The embodiment of the invention also aims to provide an application of the aerogel material in degrading sulfonamide wastewater.
It is another object of embodiments of the present invention to provide a catalyst, partially or wholly comprising the aerogel material described above.
Another object of the embodiments of the present invention is to provide a method for degrading sulfonamide wastewater, which comprises the following steps: mixing the sulfonamide wastewater to be degraded with the catalyst, and then adding peroxymonosulfate for aeration.
Preferably, the concentration of the sulfonamide wastewater is 15mg/L, the sulfonamide wastewater to be degraded is mixed with the catalyst, the catalyst is placed in a proper amount of the sulfonamide wastewater, so that the sulfonamide wastewater overflows over the catalyst, and then the mixture is placed for 40 min.
As a still further scheme of the invention: the peroxymonosulfate may be any of potassium hydrogen persulfate, potassium monopersulfate, sodium monopersulfate, ammonium peroxymonosulfate, or sodium peroxymonosulfate.
Preferably, the peroxymonosulfate is potassium hydrogen persulfate, and of course, the peroxymonosulfate can be replaced by peroxydisulfate to degrade the sulfonamide wastewater according to requirements.
The amount of the potassium hydrogen persulfate can be selected according to needs, and in general, excessive potassium hydrogen persulfate is added, the potassium hydrogen persulfate is activated by the catalyst to generate a large amount of sulfate radicals, and then organic pollutants in the water body are thoroughly oxidized into carbon dioxide, water and inorganic salts.
The embodiment of the invention also aims to provide an application of the method for degrading the sulfonamide wastewater in organic pollutant treatment. The organic pollutants to be degraded are mixed with the catalyst, and then the peroxymonosulfate is added, so that the catalyst can efficiently catalyze the peroxymonosulfate to be degraded under natural aeration, has the advantages of stability, high efficiency, low cost, no toxicity and the like, and can be applied to the degradation of the organic pollutants difficult to biodegrade.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides an aerogel material, which can effectively activate persulfate to degrade sulfonamide wastewater, so that an oxidation system formed by the aerogel material and the persulfate can effectively degrade the sulfonamide wastewater, can realize recycling through simple extrusion, avoids secondary pollution to the environment, has the advantages of stability, high efficiency, low cost, no toxicity and the like, can be applied to degradation of organic pollutants difficult to biodegrade, solves the problem that the existing persulfate activation oxidation method adopts a powdered carbon material as a catalyst, cannot realize recycling of the catalyst, and has wide market prospect.
Drawings
FIG. 1 is an X-ray diffraction pattern of an aerogel material provided by an embodiment of the present invention.
Fig. 2 is a raman spectrum of an aerogel material according to an embodiment of the present invention.
FIG. 3 is a Fourier transform infrared spectrum of an aerogel material according to an embodiment of the present invention.
Detailed Description
The invention is described in further detail below with reference to the figures and the specific embodiments. The following examples will aid those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any manner. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the concept of the invention. All falling within the scope of the invention.
Example 1
The specific preparation method of the aerogel material comprises the following steps:
dispersing graphene oxide in 30mL of deionized water to obtain graphene oxide aqueous dispersion with the concentration of 4mg/mL, then adding 0.12mL of deionized water, stirring and dispersing uniformly, transferring to a hydrothermal kettle, moving the hydrothermal kettle to an oven, keeping the temperature of the oven at 200 ℃ for 3 hours, then cooling to room temperature to obtain hydrogel, and carrying out dialysis treatment and freeze drying to obtain an aerogel material; the step of freeze drying is to place the dialyzed hydrogel in a cold trap of a freeze dryer, pre-freeze the hydrogel for 3 hours at-50 ℃, then place the hydrogel on a tray above the freeze dryer, and freeze-dry the hydrogel for 24 hours under 3Pa, so that the original pore structure of the hydrogel can be maintained.
In this embodiment, the method for preparing graphene oxide in the graphene oxide aqueous dispersion liquid includes: under the condition of ice-water bath, 4g of graphite powder is slowly added into 50mL of sulfuric acid aqueous solution under magnetic stirring, the mass fraction of the sulfuric acid aqueous solution is 98%, after the magnetic stirring is carried out for 20min, 9g of potassium permanganate is slowly added, after the stirring is continued for 1h, the solution is dark green, then the temperature is slowly increased to 60 ℃, the stirring is continued for 1h until the solution is slightly viscous, then the temperature is increased to 96 ℃, 100mL of deionized water is added, the stirring is continued for 50min, after the solution is cooled to the room temperature, the solution is placed on a magnetic stirrer to be stirred, 40mL of hydrogen peroxide is added, 300mL of deionized water is added to terminate the reaction, the mixture after the termination of the reaction is centrifuged for 10min under the condition of 4000r/min, the mixture is pickled for 5min with hydrochloric acid solution, then is centrifuged for 10min under the condition of 4000r/min, then is alcohol-washed for 10min with ethanol solution, then is centrifuged for 10min under the condition of 4000r/min, and the yellowish soil sediment is collected, and (3) drying for 12h at 80 ℃ in vacuum to obtain the graphene oxide.
In this embodiment, the aerogel material is applied to degradation of sulfonamide wastewater.
In this embodiment, a catalyst comprises, in part or in whole, an aerogel material as described above.
In this embodiment, a method for degrading sulfonamide wastewater includes the following steps: mixing the sulfonamide wastewater to be degraded with the catalyst, and then adding peroxymonosulfate for aeration. The concentration of the sulfonamide wastewater is 15mg/L, the sulfonamide wastewater to be degraded is mixed with the catalyst, the catalyst is placed in a proper amount of the sulfonamide wastewater, so that the sulfonamide wastewater overflows the catalyst, and then the mixture is placed for 40 min.
Example 2
An aerogel material is prepared by the following specific steps:
dispersing graphene oxide in 30mL of deionized water to obtain graphene oxide aqueous dispersion with the concentration of 4mg/mL, then adding 0.12mL of hydrazine hydrate aqueous solution with the mass fraction of 10%, uniformly stirring and dispersing, transferring to a hydrothermal kettle, moving the hydrothermal kettle to an oven, keeping the hydrothermal kettle at 200 ℃ for 3 hours, then cooling to room temperature to obtain hydrogel, and carrying out dialysis treatment and freeze drying to obtain an aerogel material; the freeze drying is to place the dialyzed hydrogel in a cold trap of a freeze dryer, pre-freeze the hydrogel for 3 hours at-50 ℃, then place the hydrogel on a tray above the freeze dryer, and freeze-dry the hydrogel for 24 hours under 3Pa, so that the original pore structure of the hydrogel can be maintained.
In this embodiment, the preparation method of graphene oxide in the graphene oxide aqueous dispersion liquid is: under the condition of ice-water bath, 4g of graphite powder is slowly added into 50mL of sulfuric acid aqueous solution under magnetic stirring, the mass fraction of the sulfuric acid aqueous solution is 98%, after the magnetic stirring is carried out for 20min, 9g of potassium permanganate is slowly added, after the stirring is continued for 1h, the solution is dark green, then the temperature is slowly increased to 60 ℃, the stirring is continued for 1h until the solution is slightly viscous, then the temperature is increased to 96 ℃, 100mL of deionized water is added, the stirring is continued for 50min, after the solution is cooled to the room temperature, the solution is placed on a magnetic stirrer to be stirred, 40mL of hydrogen peroxide is added, 300mL of deionized water is added to terminate the reaction, the mixture after the termination of the reaction is centrifuged for 10min under the condition of 4000r/min, the mixture is pickled for 5min with hydrochloric acid solution, then is centrifuged for 10min under the condition of 4000r/min, then is alcohol-washed for 10min with ethanol solution, then is centrifuged for 10min under the condition of 4000r/min, and the yellowish soil sediment is collected, and (3) drying for 12h at 80 ℃ in vacuum to obtain the graphene oxide.
In this embodiment, the aerogel material is applied to degradation of sulfonamide wastewater.
In this embodiment, a catalyst comprises a portion or all of the aerogel material described above.
In this embodiment, a method for degrading sulfonamide wastewater includes the following steps: mixing the sulfonamide wastewater to be degraded with the catalyst, and then adding peroxymonosulfate for aeration. The concentration of the sulfonamide wastewater is 15mg/L, the sulfonamide wastewater to be degraded is mixed with the catalyst, the catalyst is placed in a proper amount of the sulfonamide wastewater, so that the sulfonamide wastewater overflows over the catalyst, and then the mixture is placed for 40 min.
Example 3
An aerogel material is prepared by the following specific steps:
dispersing graphene oxide in 30mL of deionized water to obtain graphene oxide aqueous dispersion with the concentration of 4mg/mL, then adding 0.12mL of hydrazine hydrate aqueous solution with the mass fraction of 20%, uniformly stirring and dispersing, transferring to a hydrothermal kettle, moving the hydrothermal kettle to an oven, keeping the hydrothermal kettle at 200 ℃ for 3 hours, then cooling to room temperature to obtain hydrogel, and carrying out dialysis treatment and freeze drying to obtain an aerogel material; the step of freeze drying is to place the dialyzed hydrogel in a cold trap of a freeze dryer, pre-freeze the hydrogel for 3 hours at-50 ℃, then place the hydrogel on a tray above the freeze dryer, and freeze-dry the hydrogel for 24 hours under 3Pa, so that the original pore structure of the hydrogel can be maintained.
In this embodiment, the preparation method of graphene oxide in the graphene oxide aqueous dispersion liquid is: under the condition of ice-water bath, slowly adding 4g of graphite powder into 50mL of sulfuric acid aqueous solution under magnetic stirring, wherein the mass fraction of the sulfuric acid aqueous solution is 98%, after magnetic stirring for 20min, slowly adding 9g of potassium permanganate, continuously stirring for 1h to obtain a dark green solution, then slowly heating to 60 ℃, continuously stirring for 1h to obtain a slightly viscous solution, then heating to 96 ℃, adding 100mL of deionized water, further continuously stirring for 50min, cooling to room temperature, placing on a magnetic stirrer, stirring, adding 40mL of hydrogen peroxide, then adding 300mL of deionized water to terminate the reaction, then centrifuging the mixture after terminating the reaction for 10min under the condition of 4000r/min, washing with hydrochloric acid for 5min, then centrifuging for 10min under the condition of 4000r/min, then washing with ethanol solution for 10min, then centrifuging for 10min under the condition of 4000r/min, and collecting earthy yellow sediments, and (3) drying for 12h at 80 ℃ in vacuum to obtain the graphene oxide.
In this embodiment, the aerogel material is applied to degradation of sulfonamide wastewater.
In this embodiment, a catalyst comprises a portion or all of the aerogel material described above.
In this embodiment, a method for degrading sulfonamide wastewater includes the following steps: mixing the sulfonamide wastewater to be degraded with the catalyst, and then adding peroxymonosulfate for aeration. The concentration of the sulfonamide wastewater is 15mg/L, the sulfonamide wastewater to be degraded is mixed with the catalyst, the catalyst is placed in a proper amount of the sulfonamide wastewater, so that the sulfonamide wastewater overflows the catalyst, and then the mixture is placed for 40 min.
Example 4
An aerogel material is prepared by the following specific steps:
dispersing graphene oxide in 30mL of deionized water to obtain graphene oxide aqueous dispersion with the concentration of 4mg/mL, then adding 0.12mL of hydrazine hydrate aqueous solution with the mass fraction of 30%, uniformly stirring and dispersing, transferring to a hydrothermal kettle, moving the hydrothermal kettle to an oven, keeping the hydrothermal kettle at 200 ℃ for 3 hours, then cooling to room temperature to obtain hydrogel, and carrying out dialysis treatment and freeze drying to obtain an aerogel material; the freeze drying is to place the dialyzed hydrogel in a cold trap of a freeze dryer, pre-freeze the hydrogel for 3 hours at-50 ℃, then place the hydrogel on a tray above the freeze dryer, and freeze-dry the hydrogel for 24 hours under 3Pa, so that the original pore structure of the hydrogel can be maintained.
In this embodiment, the method for preparing graphene oxide in the graphene oxide aqueous dispersion liquid includes: under the condition of ice-water bath, 4g of graphite powder is slowly added into 50mL of sulfuric acid aqueous solution under magnetic stirring, the mass fraction of the sulfuric acid aqueous solution is 98%, after the magnetic stirring is carried out for 20min, 9g of potassium permanganate is slowly added, after the stirring is continued for 1h, the solution is dark green, then the temperature is slowly increased to 60 ℃, the stirring is continued for 1h until the solution is slightly viscous, then the temperature is increased to 96 ℃, 100mL of deionized water is added, the stirring is continued for 50min, after the solution is cooled to the room temperature, the solution is placed on a magnetic stirrer to be stirred, 40mL of hydrogen peroxide is added, 300mL of deionized water is added to terminate the reaction, the mixture after the termination of the reaction is centrifuged for 10min under the condition of 4000r/min, the mixture is pickled for 5min with hydrochloric acid solution, then is centrifuged for 10min under the condition of 4000r/min, then is alcohol-washed for 10min with ethanol solution, then is centrifuged for 10min under the condition of 4000r/min, and the yellowish soil sediment is collected, and (3) drying for 12h at 80 ℃ in vacuum to obtain the graphene oxide.
In this embodiment, the aerogel material is applied to degradation of sulfonamide wastewater.
In this embodiment, a catalyst comprises, in part or in whole, an aerogel material as described above.
In this embodiment, a method for degrading sulfonamide wastewater includes the following steps: mixing the sulfonamide wastewater to be degraded with the catalyst, and then adding peroxymonosulfate for aeration. The concentration of the sulfonamide wastewater is 15mg/L, the sulfonamide wastewater to be degraded is mixed with the catalyst, the catalyst is placed in a proper amount of the sulfonamide wastewater, so that the sulfonamide wastewater overflows over the catalyst, and then the mixture is placed for 40 min.
Example 5
An aerogel material is prepared by the following specific steps:
dispersing graphene oxide in 30mL of deionized water to obtain graphene oxide aqueous dispersion with the concentration of 4mg/mL, then adding 0.12mL of 40% hydrazine hydrate aqueous solution by mass fraction, uniformly stirring and dispersing, transferring to a hydrothermal kettle, moving the hydrothermal kettle to an oven, keeping the hydrothermal kettle at 200 ℃ for 3 hours, then cooling to room temperature to obtain hydrogel, and carrying out dialysis treatment and freeze drying to obtain an aerogel material; the step of freeze drying is to place the dialyzed hydrogel in a cold trap of a freeze dryer, pre-freeze the hydrogel for 3 hours at-50 ℃, then place the hydrogel on a tray above the freeze dryer, and freeze-dry the hydrogel for 24 hours under 3Pa, so that the original pore structure of the hydrogel can be maintained.
In this embodiment, the method for preparing graphene oxide in the graphene oxide aqueous dispersion liquid includes: under the condition of ice-water bath, slowly adding 4g of graphite powder into 50mL of sulfuric acid aqueous solution under magnetic stirring, wherein the mass fraction of the sulfuric acid aqueous solution is 98%, after magnetic stirring for 20min, slowly adding 9g of potassium permanganate, continuously stirring for 1h to obtain a dark green solution, then slowly heating to 60 ℃, continuously stirring for 1h to obtain a slightly viscous solution, then heating to 96 ℃, adding 100mL of deionized water, further continuously stirring for 50min, cooling to room temperature, placing on a magnetic stirrer, stirring, adding 40mL of hydrogen peroxide, then adding 300mL of deionized water to terminate the reaction, then centrifuging the mixture after terminating the reaction for 10min under the condition of 4000r/min, washing with hydrochloric acid for 5min, then centrifuging for 10min under the condition of 4000r/min, then washing with ethanol solution for 10min, then centrifuging for 10min under the condition of 4000r/min, and collecting earthy yellow sediments, and (3) drying for 12h at 80 ℃ in vacuum to obtain the graphene oxide.
In this embodiment, the aerogel material is applied to degradation of sulfonamide wastewater.
In this embodiment, a catalyst comprises a portion or all of the aerogel material described above.
In this embodiment, a method for degrading sulfonamide wastewater includes the following steps: mixing the sulfonamide wastewater to be degraded with the catalyst, and then adding peroxymonosulfate for aeration. The concentration of the sulfonamide wastewater is 15mg/L, the sulfonamide wastewater to be degraded is mixed with the catalyst, the catalyst is placed in a proper amount of the sulfonamide wastewater, so that the sulfonamide wastewater overflows over the catalyst, and then the mixture is placed for 40 min.
Example 6
An aerogel material is prepared by the following specific steps:
dispersing graphene oxide in 30mL of deionized water to obtain graphene oxide aqueous dispersion with the concentration of 4mg/mL, then adding 0.12mL of hydrazine hydrate aqueous solution with the mass fraction of 50%, uniformly stirring and dispersing, transferring to a hydrothermal kettle, moving the hydrothermal kettle to an oven, keeping the hydrothermal kettle at 200 ℃ for 3 hours, then cooling to room temperature to obtain hydrogel, and carrying out dialysis treatment and freeze drying to obtain an aerogel material; the freeze drying is to place the dialyzed hydrogel in a cold trap of a freeze dryer, pre-freeze the hydrogel for 3 hours at-50 ℃, then place the hydrogel on a tray above the freeze dryer, and freeze-dry the hydrogel for 24 hours under 3Pa, so that the original pore structure of the hydrogel can be maintained.
In this embodiment, the method for preparing graphene oxide in the graphene oxide aqueous dispersion liquid includes: under the condition of ice-water bath, slowly adding 4g of graphite powder into 50mL of sulfuric acid aqueous solution under magnetic stirring, wherein the mass fraction of the sulfuric acid aqueous solution is 98%, after magnetic stirring for 20min, slowly adding 9g of potassium permanganate, continuously stirring for 1h to obtain a dark green solution, then slowly heating to 60 ℃, continuously stirring for 1h to obtain a slightly viscous solution, then heating to 96 ℃, adding 100mL of deionized water, further continuously stirring for 50min, cooling to room temperature, placing on a magnetic stirrer, stirring, adding 40mL of hydrogen peroxide, then adding 300mL of deionized water to terminate the reaction, then centrifuging the mixture after terminating the reaction for 10min under the condition of 4000r/min, washing with hydrochloric acid for 5min, then centrifuging for 10min under the condition of 4000r/min, then washing with ethanol solution for 10min, then centrifuging for 10min under the condition of 4000r/min, and collecting earthy yellow sediments, and (3) drying for 12h at 80 ℃ in vacuum to obtain the graphene oxide.
In this embodiment, the aerogel material is applied to degradation of sulfonamide wastewater.
In this embodiment, a catalyst comprises a portion or all of the aerogel material described above.
In this embodiment, a method for degrading sulfonamide wastewater includes the following steps: mixing the sulfonamide wastewater to be degraded with the catalyst, and then adding peroxymonosulfate for aeration. The concentration of the sulfonamide wastewater is 15mg/L, the sulfonamide wastewater to be degraded is mixed with the catalyst, the catalyst is placed in a proper amount of the sulfonamide wastewater, so that the sulfonamide wastewater overflows the catalyst, and then the mixture is placed for 40 min.
Example 7
An aerogel material comprises the following raw materials in parts by weight: 29g of graphene oxide aqueous dispersion and 0.10g of hydrazine hydrate aqueous solution, wherein the mass fraction of the hydrazine hydrate aqueous solution is 50%, and the concentration of the graphene oxide aqueous dispersion is 3 mg/mL.
The graphene oxide in the graphene oxide aqueous dispersion comprises the following raw materials: 3g of graphite powder, 45g of sulfuric acid aqueous solution, 8g of potassium permanganate, 38g of hydrogen peroxide and 350g of deionized water, wherein the mass fraction of the sulfuric acid aqueous solution is 98%. The preparation method of the graphene oxide in the graphene oxide aqueous dispersion comprises the following steps: weighing graphite powder according to a proportion, slowly adding the graphite powder into a sulfuric acid aqueous solution for mixing, slowly adding potassium permanganate, stirring at 58 ℃, then heating to 95 ℃, adding one fourth of deionized water in the total amount of the deionized water for mixing, continuing stirring for 50min, cooling to room temperature, placing on a magnetic stirrer for stirring, adding hydrogen peroxide for oxidation reaction, then adding the rest of deionized water to stop the reaction, and then sequentially centrifuging, cleaning and drying to obtain the graphite powder.
A method of preparing an aerogel material, comprising the steps of:
weighing graphene oxide aqueous dispersion according to a proportion, mixing the graphene oxide aqueous dispersion with a hydrazine hydrate aqueous solution, keeping the mixture at 190 ℃ for 2 hours, and cooling the mixture to room temperature to obtain hydrogel;
dialyzing the hydrogel to obtain the dialyzed hydrogel;
and (3) freeze-drying the dialyzed hydrogel to obtain the hydrogel. And the freeze drying is to place the dialyzed hydrogel in a cold trap of a freeze dryer, pre-freeze the hydrogel for 3 hours at-50 ℃, then place the hydrogel on a tray above the freeze dryer, and freeze-dry the hydrogel for 24 hours under 3 Pa.
Example 8
An aerogel material comprises the following raw materials in parts by weight: 31g of graphene oxide aqueous dispersion and 0.15g of hydrazine hydrate aqueous solution, wherein the mass fraction of the hydrazine hydrate aqueous solution is 50%, and the concentration of the graphene oxide aqueous dispersion is 5 mg/mL.
The graphene oxide in the graphene oxide aqueous dispersion comprises the following raw materials: 5g of graphite powder, 55g of sulfuric acid aqueous solution, 10g of potassium permanganate, 42g of hydrogen peroxide and 450g of deionized water, wherein the mass fraction of the sulfuric acid aqueous solution is 98%. The preparation method of the graphene oxide in the graphene oxide aqueous dispersion comprises the following steps: weighing graphite powder according to a proportion, slowly adding the graphite powder into a sulfuric acid aqueous solution for mixing, slowly adding potassium permanganate, stirring at 62 ℃, heating to 97 ℃, adding one fourth of deionized water in the total amount of the deionized water for mixing, continuously stirring for 50min, cooling to room temperature, placing on a magnetic stirrer for stirring, adding hydrogen peroxide for oxidation reaction, adding the rest deionized water for stopping reaction, and sequentially centrifuging, cleaning and drying to obtain the graphite powder.
A method of preparing an aerogel material, comprising the steps of:
weighing graphene oxide aqueous dispersion and hydrazine hydrate aqueous solution according to a proportion, mixing, keeping at 210 ℃ for 4h, and cooling to room temperature to obtain hydrogel;
dialyzing the hydrogel to obtain the dialyzed hydrogel;
and (3) freeze-drying the dialyzed hydrogel to obtain the hydrogel. And the step of freeze drying is to place the dialyzed hydrogel in a cold trap of a freeze dryer, pre-freeze the hydrogel for 3 hours at-50 ℃, then place the hydrogel on a tray above the freeze dryer, and freeze-dry the hydrogel for 24 hours under 3 Pa.
Example 9
The aerogel materials prepared in examples 1 and 5 were characterized by X-ray diffraction, raman spectroscopy, and infrared spectroscopy, which were methods known in the art, and the results are shown in fig. 1-3, wherein fig. 1 is an X-ray diffraction pattern of the aerogel materials prepared in examples 1 and 5, fig. 2 is a raman spectroscopy pattern of the aerogel materials prepared in examples 1 and 5, and fig. 3 is a fourier transform infrared spectroscopy pattern of the aerogel materials prepared in examples 1 and 5. Wherein, the aerogel material prepared in example 1 is recorded as blank graphene gel, and the aerogel material prepared in example 5 is recorded as graphene gel reduced by 40% hydrazine hydrate, and as can be seen from fig. 1 to 3, the pore structure, defect sites and functional groups (especially carbonyl) of the aerogel material prepared by reduction by 40% hydrazine hydrate are changed, thereby being beneficial to improving the catalytic activity of the aerogel material.
Example 10
And (3) carrying out performance detection on the aerogel materials prepared in the embodiments 1 to 6, specifically, adsorbing 15mg/L sulfamonomethoxine wastewater by the aerogel materials for 40min at room temperature, adding potassium hydrogen persulfate with the same weight as the aerogel materials, and detecting the degradation rate of the sulfamonomethoxine wastewater after 120 min. Specific detection results are shown in table 1.
TABLE 1 test results Table
| Group of | Degradation rate |
| Example 1 | 20.35％ |
| Example 2 | 38.84％ |
| Example 3 | 41.5％ |
| Example 4 | 75.58％ |
| Example 5 | 94.19％ |
| Example 6 | 86.37％ |
As can be seen from Table 1, the degradation rate of the aerogel material on the sulfa-metodiazine wastewater can be effectively improved by the same matching of the graphene oxide aqueous dispersion and the hydrazine hydrate aqueous solution, wherein the degradation rate of the aerogel material on the sulfa-metodiazine wastewater of 15mg/L is 94.19% by treating the aerogel material with 40% by mass of the hydrazine hydrate aqueous solution. In addition, the aerogel materials prepared in the embodiments 1 to 6 have no change in form after being impacted by water flow in the catalytic degradation process, have good mechanical stability, can remove interstitial water in an extrusion mode, and are convenient to recycle.
The preparation method has the beneficial effects that the aerogel material prepared by the preparation method has good catalytic performance, persulfate can have enhanced oxidation capacity and high degradation efficiency, and the change of atomic arrangement, pore structure, defect sites and functional groups (particularly carbonyl) in the aerogel material is beneficial to improving the catalytic activity of the aerogel material; moreover, the aerogel material easy to recycle is prepared by a simple and convenient hydrothermal method, can promote persulfate to oxidize and adsorb water on the surface of the aerogel material to directly generate OH free radicals to participate in degrading organic pollutants together, and can efficiently catalyze persulfate to degrade sulfa-methoxypyrimidine wastewater with the concentration of not less than 15mg/L under natural aeration.
While the preferred embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art. This need not be, nor should it be exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the scope of the invention.
Claims (5)
1. A method for degrading sulfonamide wastewater is characterized by comprising the following steps: mixing the sulfonamide wastewater to be degraded with a catalyst prepared from an aerogel material, and then adding peroxymonosulfate for aeration;
the aerogel material comprises the following raw materials in parts by weight: 29-31 parts of graphene oxide aqueous dispersion and 0.10-0.15 part of hydrazine hydrate aqueous solution, wherein the mass fraction of the hydrazine hydrate aqueous solution is 0-50%, and the concentration of the graphene oxide aqueous dispersion is 3-5 mg/mL; the graphene oxide in the graphene oxide aqueous dispersion comprises the following raw materials in parts by weight: 3-5 parts of graphite powder, 45-55 parts of sulfuric acid aqueous solution, 8-10 parts of potassium permanganate, 38-42 parts of hydrogen peroxide and 450 parts of deionized water, wherein the mass fraction of the sulfuric acid aqueous solution is not less than 70%; the preparation method of the graphene oxide in the graphene oxide aqueous dispersion liquid comprises the following steps: weighing graphite powder according to a proportion, adding the graphite powder into a sulfuric acid aqueous solution for mixing, then adding potassium permanganate, stirring at the temperature of 58-62 ℃, then heating to 95-97 ℃, adding deionized water for mixing, cooling to room temperature, then adding hydrogen peroxide for oxidation reaction, and then sequentially centrifuging, cleaning and drying.
2. A method for degrading sulfonamide wastewater according to claim 1, comprising the steps of:
weighing graphene oxide aqueous dispersion according to the weight parts, mixing the graphene oxide aqueous dispersion with a hydrazine hydrate aqueous solution, keeping the mixture at the temperature of 190-210 ℃ for 2-4h, and cooling the mixture to room temperature to obtain hydrogel;
dialyzing the hydrogel to obtain the dialyzed hydrogel;
and (3) freeze-drying the dialyzed hydrogel to obtain the hydrogel.
3. A method for degrading sulfonamide wastewater according to claim 2, wherein the dialysis comprises the steps of sealing the hydrogel in a dialysis bag, standing the hydrogel in deionized water for 7-9 hours, and taking out the hydrogel.
4. The method for degrading sulfonamide wastewater according to claim 3, wherein the freeze-drying is performed by freezing the dialyzed hydrogel at-10 ℃ to-50 ℃ and then drying the dialyzed hydrogel at 1.3Pa to 13 Pa.
5. Use of the method of degrading sulfonamide waste water of claim 1 in the treatment of organic pollutants.
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