CN111871413A - Preparation and application of photocatalyst for degrading organic pollutants in water under alkaline condition - Google Patents
Preparation and application of photocatalyst for degrading organic pollutants in water under alkaline condition Download PDFInfo
- Publication number
- CN111871413A CN111871413A CN202010019905.9A CN202010019905A CN111871413A CN 111871413 A CN111871413 A CN 111871413A CN 202010019905 A CN202010019905 A CN 202010019905A CN 111871413 A CN111871413 A CN 111871413A
- Authority
- CN
- China
- Prior art keywords
- soil
- solution
- photocatalyst
- acid
- preparing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 21
- 230000000593 degrading effect Effects 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000002957 persistent organic pollutant Substances 0.000 title abstract description 3
- 239000002689 soil Substances 0.000 claims abstract description 67
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 19
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 17
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 15
- 239000002351 wastewater Substances 0.000 claims abstract description 13
- 238000000975 co-precipitation Methods 0.000 claims abstract description 8
- 238000011065 in-situ storage Methods 0.000 claims abstract description 8
- 238000010304 firing Methods 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 12
- 238000000967 suction filtration Methods 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical class [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 10
- 230000007935 neutral effect Effects 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 8
- 230000015556 catabolic process Effects 0.000 claims description 7
- 238000006731 degradation reaction Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 7
- 239000011790 ferrous sulphate Substances 0.000 claims description 6
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 6
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 6
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 5
- 238000012986 modification Methods 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 239000000498 cooling water Substances 0.000 claims description 4
- 239000006260 foam Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims 1
- 238000004321 preservation Methods 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 15
- 238000011068 loading method Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract 1
- 239000012535 impurity Substances 0.000 abstract 1
- 238000005554 pickling Methods 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000001308 synthesis method Methods 0.000 description 4
- 238000003911 water pollution Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
Images
Classifications
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- 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
- B01J35/33—Electric or magnetic properties
-
- 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
- B01J35/39—Photocatalytic properties
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- 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
- C02F1/722—Oxidation by peroxides
-
- 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
-
- 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
-
- 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
- C02F2305/10—Photocatalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
Abstract
A preparation method and an application of a photocatalyst for degrading organic matters in water under an alkaline condition relate to a preparation method and an application of a photocatalyst and aim to solve the problem that organic matters in wastewater are difficult to degrade under the existing alkaline condition. The method comprises the following steps: firstly, pickling diatomite raw soil, and removing impurities to obtain pickled soil; firing the acid-washed soil to obtain fired soil; modifying by using CTAB to obtain modified soil; and fourthly, loading the nano ferroferric oxide on the modified soil by using an in-situ coprecipitation method to obtain the loaded soil. The catalyst has low preparation cost and good organic pollutant removal effect. The invention is used for removing organic matters in the degraded alkaline wastewater.
Description
Technical Field
The invention relates to a preparation method and application of a photocatalyst capable of degrading organic matters in water under an alkaline condition.
Background
The treatment of water pollution is always important in environmental protection. Water is an indispensable resource for human beings. The problem of water pollution has been a major concern. The water pollution problem is long-standing, the problem is acute, and the water pollution is complex, namely the pollution of inorganic substances and organic substances is included. The pollution of organic matters is difficult to treat, and the fundamental reason is that the organic matters are more in variety and different in properties and are difficult to solve by one method at one time.
The catalytic method is a development hotspot, and has the advantages that the primary conversion does not cause secondary pollution, secondary treatment is not needed, and the photocatalyst is a great class. However, since the photocatalyst is used under severe conditions, it is basically used under neutral and acidic conditions, and is rarely used under alkaline conditions. However, it is difficult to achieve all acidity or all neutrality depending on the place where the waste water is discharged. Therefore, the invention of the photocatalyst capable of efficiently degrading organic matters under the alkaline condition is particularly important.
Disclosure of Invention
The invention mainly solves the problem that the existing photocatalyst can not be applied under the alkaline condition, and provides a preparation method and application of a photocatalyst for degrading organic matters in water under the alkaline condition.
The invention discloses a preparation method of a photocatalyst for degrading organic matters in water under alkaline conditions, which is characterized by comprising the following steps:
firstly, acid washing of diatomite: preparing 30% sulfuric acid solution, placing diatomite in a beaker, adding 30% sulfuric acid solution, and immersing the diatomite. Heating to react for 1h at 90 ℃, and stirring intermittently. After the reaction is finished, cooling to room temperature, carrying out suction filtration, and washing while carrying out suction filtration until the diatomite is neutral. Drying at 100 deg.C, grinding, sealing and storing. Obtaining the acid-washed soil.
Firing acid-washing soil: and (4) taking a proper amount of acid-washed soil, and firing the acid-washed soil in a muffle furnace to obtain the burned soil.
Thirdly, CTAB modification: taking a proper amount of burnt soil, dissolving the burnt soil in deionized water, and ultrasonically dispersing for 0.5 h. According to the mass ratio of the burnt soil to the solid CTAB of 7: 3 ratio configuration 20
t% CTAB solution. Added to the calcined soil solution and adjusted pH =11 using saturated sodium hydroxide solution. Stirring at 80 deg.C for 120 min. After the reaction is finished, cooling to room temperature and standing for 24 hours. Suction filtration and alternate washing with ethanol and deionized water until no foam is generated. Drying at 110 ℃ to obtain the modified soil.
Tetra, nano-tetraoxidePreparing iron-loaded soil: and preparing the nano ferroferric oxide loaded soil by using an in-situ coprecipitation method. Dissolving a certain amount of modified soil in deionized water, and performing ultrasonic dispersion for 5 min. Modifying soil according to the mass ratio: nano ferroferric oxide = 7: 3, calculating and weighing ferrous sulfate and ferric trichloride according to the proportion, respectively preparing the ferrous sulfate and the ferric trichloride into 0.1mol/L solution, and keeping Fe in the solution2+With Fe3+Always in a molar ratio of 3: 4. and introducing nitrogen for 5min to drive oxygen, and keeping introducing nitrogen all the time. The circulating cooling water was switched on, the stirring was switched on, and the temperature was maintained at 80 ℃. The reaction was stirred for 1h with pH =9-10 adjusted using saturated sodium hydroxide solution. The product was transferred to a beaker after cooling to room temperature and washed alternately with deionized water and absolute ethanol until the solution was neutral. And (5) drying in vacuum. Grinding and sieving with a 200-mesh sieve to obtain the nano ferroferric oxide loaded soil.
And step three, the ultrasonic power in step four is 40-60W.
Further, the burning temperature in the step two is 500-600 ℃.
Further, the burning time in the step two is 0-30min
The photocatalyst prepared by the method can be applied to degrading organic matters in wastewater under the alkaline condition.
The invention can degrade the organic matters in the alkaline wastewater, and the degradation efficiency can reach more than 99%.
The principle of the invention is as follows:
alkaline wastewater is used as one type of wastewater, because of the special pH value condition, the traditional photocatalyst can not be used for degradation treatment, if the alkaline wastewater is directly discharged without treatment, immeasurable loss can be caused to the ecological environment, and therefore, the photocatalyst capable of degrading organic matters in water under the alkaline condition is invented.
The main working principle of the catalyst in the process of degrading organic wastewater is that the diatomite has a large specific surface area, the specific surface area of a sample modified by CTAB is increased, the adsorption capacity is increased, the diatomite provides an active site through adsorption, the nano ferroferric oxide decomposes hydrogen peroxide under the action of sunlight irradiation to generate a hydrogen peroxide radical and a peroxy radical, and the two radicals have high redox potential and can effectively degrade organic matters in water, so that the degradation of the organic matters is realized.
The invention has the beneficial effects that:
the method takes diatomite as a raw material and adopts an in-situ coprecipitation synthesis method to prepare the photocatalyst. Therefore, the photocatalyst can be used for degrading organic matters in the alkaline wastewater.
The diatomite has good chemical stability and hydrophobicity and can be stably dispersed in water, so that the diatomite can show good stability and stably exist in the water, and is beneficial to adsorption and catalysis.
The invention is synthesized by an in-situ coprecipitation synthesis method, and has the advantages of simple preparation method, wide raw material source and simple operation. The product prepared by the in-situ coprecipitation synthesis method has magnetism and is beneficial to separation and reuse. The huge specific surface area of the diatomite is beneficial to adsorption and catalytic degradation of pollutants, so that the degradation efficiency of organic matters can reach more than 99%. The photocatalyst has good practicability and wide application prospect. .
The product prepared by the method has uniform size, simple synthesis method, cheap and easily-obtained raw materials and low cost, and the prepared product is non-toxic, has better photocatalytic performance and has wide application prospect in the fields of environment monitoring, treatment and the like and material chemistry.
Drawings
FIG. 1 is a scanning electron microscope image of the catalyst prepared in example 1 (the catalyst has a particle size of about 100. mu.m)
m)；
FIG. 2 is an XRD spectrum of the catalyst prepared in example 1;
FIG. 3 is an IR spectrum of the catalyst prepared in example 1
FIG. 4 is a kinetic curve of the catalytic reaction of the catalyst prepared in example 1 under basic conditions:
FIG. 5 is a plot of the number of uses of the catalyst prepared in example 1 under basic conditions;
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
The first embodiment is as follows: the method for preparing the photocatalyst of the present embodiment is characterized by comprising the steps of:
firstly, acid washing of diatomite: preparing 30% sulfuric acid solution, placing diatomite in a beaker, adding 30% sulfuric acid solution, and immersing the diatomite. Heating to react for 1h at 90 ℃, and stirring intermittently. After the reaction is finished, cooling to room temperature, carrying out suction filtration, and washing with deionized water while carrying out suction filtration until the filtrate is neutral. The prepared sample is dried at 100 ℃, ground, sealed and stored. Obtaining the acid-washed soil.
Firing acid-washing soil: and (3) taking a proper amount of acid-washed soil, and burning the acid-washed soil in a muffle furnace at 500 ℃ to obtain burned soil.
Thirdly, CTAB modification: taking a proper amount of burnt soil, dissolving the burnt soil in deionized water, and ultrasonically dispersing for 0.5 h. According to the mass ratio of the burnt soil to the solid CTAB of 7: 3 ratio configuration 20
t% CTAB solution. Added to the calcined soil solution and adjusted pH =11 using saturated sodium hydroxide solution. Stirring at 80 deg.C for 120 min. After the reaction is finished, cooling to room temperature and standing for 24 hours. Suction filtration and alternate washing with ethanol and deionized water until no foam is generated. Drying at 110 ℃ to obtain the modified soil.
Preparing the nano ferroferric oxide loaded soil: and preparing the nano ferroferric oxide loaded soil by using an in-situ coprecipitation method. Dissolving a certain amount of modified soil in deionized water, and performing ultrasonic dispersion for 5 min. The modified soil comprises the following components in percentage by mass: nano ferroferric oxide = 7: 3, calculating and weighing ferrous sulfate and ferric trichloride according to the proportion, respectively preparing the ferrous sulfate and the ferric trichloride into 0.1mol/L solution, and keeping Fe in the solution2+With Fe3+Always in a molar ratio of 3: 4. introducing nitrogen for 5min to drive oxygen, andthe nitrogen was kept constantly introduced. The circulating cooling water was turned on, stirring was started, and the temperature was maintained at 80 ℃. The reaction was stirred for 1h with pH =9-10 adjusted using saturated sodium hydroxide solution. The product was transferred to a beaker after cooling to room temperature and washed alternately with deionized water and absolute ethanol until the solution was neutral. Vacuum drying, grinding and sieving with a 200-mesh sieve to obtain the nano ferroferric oxide loaded soil.
The following examples are given to illustrate the present invention, and the following examples are carried out on the premise of the technical solution of the present invention, and give detailed embodiments and specific procedures, but the scope of the present invention is not limited to the following examples.
Example 1:
firstly, acid washing of diatomite: preparing 30% sulfuric acid solution, placing diatomite in a beaker, adding 30% sulfuric acid solution, and immersing the diatomite. Heating to react for 1h at 90 ℃ and stirring intermittently. After the reaction is finished, cooling to room temperature, carrying out suction filtration, and washing while carrying out suction filtration until the filtrate is neutral. Drying at 100 deg.C, grinding, sealing and storing. Obtaining the acid-washed soil.
Firing acid-washing soil: and (3) taking a proper amount of acid-washed soil, and burning the acid-washed soil in a muffle furnace at 500 ℃ to obtain burned soil.
Thirdly, CTAB modification: taking a proper amount of burnt soil, dissolving the burnt soil in deionized water, and ultrasonically dispersing for 0.5 h. According to the mass ratio of the burnt soil to the solid CTAB of 7: 3 ratio configuration 20
t% CTAB solution. Added to the calcined soil solution and adjusted pH =11 using saturated sodium hydroxide solution. Stirring at 80 deg.C for 120 min. After the reaction is finished, cooling to room temperature and standing for 24 hours. Suction filtration and alternate washing with ethanol and deionized water until no foam is generated. Drying at 110 ℃. Obtaining the modified soil.
Preparing the nano ferroferric oxide loaded soil: and preparing the nano ferroferric oxide loaded soil by using an in-situ coprecipitation method. Dissolving a certain amount of modified soil in deionized water, and performing ultrasonic dispersion for 5 min. Modifying soil according to the mass ratio: nano ferroferric oxide = 7: 3 and weighing sulfuric acidIron and ferric trichloride are respectively prepared into 0.1mol/L solution, and Fe in the solution is maintained2+With Fe3+Always in a molar ratio of 3: 4. and introducing nitrogen for 5min to drive oxygen, and keeping introducing nitrogen all the time. The circulating cooling water was turned on, stirring was started, and the temperature was maintained at 80 ℃. The reaction was stirred for 1h with the pH =9-10 adjusted using bag and sodium hydroxide solution. The product was transferred to a beaker after cooling to room temperature and washed alternately with deionized water and absolute ethanol until the solution was neutral. Vacuum drying, grinding and sieving with a 200-mesh sieve to obtain the nano ferroferric oxide loaded soil.
The scanning electron micrograph of the catalyst prepared in this example is shown in FIG. 1, and the catalyst has uniform size and good dispersibility, and the size is about 100
m。
Fig. 2 is an XRD spectrum of the catalyst prepared in this example, and it can be seen that the loading was successful.
FIG. 3 is an IR spectrum of the catalyst prepared in this example, and the success of the preparation can be seen
FIG. 4 is a graph showing the reaction rate of the catalyst prepared in this example, and it can be seen that the reaction is a first-order reaction and the reaction rate is relatively high.
Fig. 5 is a reaction use frequency curve of the catalyst prepared in this example, and the degradation efficiency can still reach more than 95% after repeated use, which shows that the catalyst has good catalytic efficiency.
Claims (6)
1. Firstly, acid washing of diatomite: preparing a 30% sulfuric acid solution, putting diatomite into a beaker, adding the 30% sulfuric acid solution, immersing the diatomite, heating to react for 1h at 90 ℃, and intermittently stirring; after the reaction is finished, cooling to room temperature, carrying out suction filtration, washing with deionized water while carrying out suction filtration until the filtrate is neutral, drying at 100 ℃, grinding, and carrying out sealed preservation to obtain acid-washed soil; firing acid-washing soil: taking a proper amount of acid-washed soil, and firing the acid-washed soil in a muffle furnace to obtain burned soil; thirdly, CTAB modification: taking a proper amount of burning soil, dissolving the burning soil with deionized water, and ultrasonically dispersing for 0.5h, wherein the mass ratio of the burning soil to solid CTAB is 7: 3 ratio configuration 20
Adding a t% CTAB solution into the burned soil solution, adjusting the pH to be =11 by using a saturated sodium hydroxide solution, and stirring at the constant temperature of 80 ℃ for 120 min; cooling to room temperature after the reaction is finished, standing for 24h, performing suction filtration, alternately washing with ethanol and deionized water until no foam is generated, and drying at 110 ℃ to obtain modified soil; preparing the nano ferroferric oxide loaded soil: preparing nano ferroferric oxide loaded soil by using an in-situ coprecipitation method; dissolving a certain amount of modified soil in deionized water, and performing ultrasonic dispersion for 5 min; modifying soil according to the mass ratio: nano ferroferric oxide = 7: 3, calculating and weighing ferrous sulfate and ferric trichloride according to the proportion, respectively preparing the ferrous sulfate and the ferric trichloride into 0.1mol/L solution, and keeping Fe in the solution2+With Fe3+Always in a molar ratio of 3: 4; introducing nitrogen for 5min to drive oxygen, and keeping introducing nitrogen all the time; connecting circulating cooling water, starting stirring, and maintaining the temperature at 80 ℃; adjusting the pH to be 9-10 by using saturated sodium hydroxide solution, and stirring for reaction for 1 h; cooling to room temperature, transferring the product into a beaker, and alternately washing the product with deionized water and absolute ethyl alcohol in sequence until the solution is neutral; vacuum drying; grinding and sieving with a 200-mesh sieve to obtain the nano ferroferric oxide loaded soil.
2. The method for preparing the photocatalyst for degrading alkaline wastewater according to claim 1, wherein the ultrasonic power in the third step and the ultrasonic power in the fourth step are 40-60W.
3. The method as claimed in claim 2, wherein the burning temperature in step two is 500-600 ℃.
4. The method according to claim 3, wherein the burning time in step two is 0-30 min.
5. The method for preparing the photocatalyst for degrading alkaline wastewater according to claim 4, wherein CTAB is used for modification in the third step.
6. The photocatalyst prepared by the method of claim 1 is used for degradation treatment of wastewater under alkaline conditions.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010019905.9A CN111871413A (en) | 2020-01-09 | 2020-01-09 | Preparation and application of photocatalyst for degrading organic pollutants in water under alkaline condition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010019905.9A CN111871413A (en) | 2020-01-09 | 2020-01-09 | Preparation and application of photocatalyst for degrading organic pollutants in water under alkaline condition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111871413A true CN111871413A (en) | 2020-11-03 |
Family
ID=73154338
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010019905.9A Pending CN111871413A (en) | 2020-01-09 | 2020-01-09 | Preparation and application of photocatalyst for degrading organic pollutants in water under alkaline condition |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111871413A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113275014A (en) * | 2021-05-24 | 2021-08-20 | 南京工业大学 | High-molecular surface modified gamma-Fe2O3Diatomite catalyst, preparation method and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318132A (en) * | 2007-06-08 | 2008-12-10 | 中山大学 | Method for preparing supported nano-iron oxide/tripolite compound catalyst |
| CN104722273A (en) * | 2013-12-18 | 2015-06-24 | 江南大学 | Method for preparing organic modified clay for removing organic pollutants from wastewater |
| CN108393089A (en) * | 2018-04-18 | 2018-08-14 | 西北师范大学 | A kind of loess loading nanometer Fe nton photochemical catalysts and preparation method thereof |
| CN108393064A (en) * | 2018-01-23 | 2018-08-14 | 吉林化工学院 | A kind of modification infusorial earth material and preparation method thereof of absorption dyestuff direct scarlet 4BS |
| CN109794222A (en) * | 2019-01-07 | 2019-05-24 | 广西大学 | A kind of organic decoration Magnetic Bentonite and its preparation method and application |
| CN110013827A (en) * | 2019-04-12 | 2019-07-16 | 成都理工大学 | Crystalline state diatomite loading nanometer Fe3O4The difunctional magnetic adsorbent of Large ratio surface and preparation method thereof |
-
2020
- 2020-01-09 CN CN202010019905.9A patent/CN111871413A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318132A (en) * | 2007-06-08 | 2008-12-10 | 中山大学 | Method for preparing supported nano-iron oxide/tripolite compound catalyst |
| CN104722273A (en) * | 2013-12-18 | 2015-06-24 | 江南大学 | Method for preparing organic modified clay for removing organic pollutants from wastewater |
| CN108393064A (en) * | 2018-01-23 | 2018-08-14 | 吉林化工学院 | A kind of modification infusorial earth material and preparation method thereof of absorption dyestuff direct scarlet 4BS |
| CN108393089A (en) * | 2018-04-18 | 2018-08-14 | 西北师范大学 | A kind of loess loading nanometer Fe nton photochemical catalysts and preparation method thereof |
| CN109794222A (en) * | 2019-01-07 | 2019-05-24 | 广西大学 | A kind of organic decoration Magnetic Bentonite and its preparation method and application |
| CN110013827A (en) * | 2019-04-12 | 2019-07-16 | 成都理工大学 | Crystalline state diatomite loading nanometer Fe3O4The difunctional magnetic adsorbent of Large ratio surface and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| XINGPING WU ET AL: "Degradation of rhodamine B by a novel Fe3O4/SiO2 double-mesoporousshelled hollow spheres through photo-Fenton process", 《MATERIALS CHEMISTRY AND PHYSICS》 * |
| 王妙婷等: "磁性硅藻土非均相Fenton催化剂制备及其催化性能", 《工业水处理》 * |
| 谭凌智等: "改性硅藻土对水中DDTs的吸附机理", 《地球科学-中国地质大学学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113275014A (en) * | 2021-05-24 | 2021-08-20 | 南京工业大学 | High-molecular surface modified gamma-Fe2O3Diatomite catalyst, preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP6801844B2 (en) | Catalytic material for catalytically activating persulfate and targeting and decomposing typical pollutants in paper wastewater, its synthesis method and application | |
| CN111495367B (en) | Magnetic polyaniline-porous carbon-Fe 3 O 4 Preparation method and application of photo-Fenton catalyst | |
| CN108993550B (en) | Surface oxygen vacancy modified bismuth oxybromide photocatalyst and preparation method thereof | |
| CN107837816B (en) | Fe2O3/g-C3N4Composite system, preparation method and application | |
| CN106268908A (en) | A kind of graphite-phase C removing removal organic polluter3n4doping TiO2float type ecological restoration material of load expanded perlite and preparation method thereof | |
| CN111659453B (en) | Catalyst for visible light-ozone synergistic catalysis and preparation method thereof | |
| CN111185210A (en) | Titanium carbide/titanium dioxide/black phosphorus nanosheet composite photocatalyst and preparation method and application thereof | |
| CN113877599A (en) | Cobalt-manganese spinel material and preparation method and application thereof | |
| CN110170328B (en) | Preparation method and application of cobalt manganate/N-doped graphene composite catalyst | |
| CN109482209B (en) | Method for removing antibiotics by using silver phosphate/bismuth sulfide/bismuth oxide double-Z-type photocatalyst | |
| CN108940349B (en) | Method for removing dye pollutants by using silver chromate/sulfur-doped nitrogen carbon Z-type photocatalyst | |
| Wang et al. | Facile preparation of graphitic carbon nitride nanosheet/agar composite hydrogels for removal of tetracycline via the synergy of adsorption and photocatalysis | |
| CN111871413A (en) | Preparation and application of photocatalyst for degrading organic pollutants in water under alkaline condition | |
| CN113117721B (en) | Cyano-functionalized g-C 3 N 4 Colloidal catalyst, preparation method and application thereof | |
| CN113318740A (en) | Cu2O/MgFe2O4Catalyst, preparation method and application thereof | |
| CN116943692A (en) | Bismuth ferrite/bismuth oxysulfate/ferric oxide strip composite material and preparation method and application thereof | |
| CN108793312B (en) | Method for removing antibiotics by using carbon nitride/nitrogen doped hollow mesoporous carbon/bismuth trioxide ternary Z-shaped photocatalyst | |
| CN115430451B (en) | Iron-titanium co-doped porous graphite phase carbon nitride photo-Fenton catalyst and preparation method and application thereof | |
| CN113600216B (en) | Preparation method of carbon cloth-supported bismuth phosphate/bismuth oxyhalide flower-like photocatalyst | |
| CN113304742B (en) | Activated carbon supported Ti 3+ Self-doping TiO 2 Preparation method of photocatalytic material | |
| CN109078644A (en) | Graphene-supported Bi-BiOCl-TiO2Photochemical catalyst and preparation method | |
| CN113145099B (en) | Bismuth-loaded bismuth titanate/calcium titanate composite photocatalyst, and preparation method and application thereof | |
| CN113244929A (en) | Iron bismuth oxide Bi2Fe4O9Preparation method and application in organic wastewater treatment | |
| CN112062257A (en) | Method for treating antibiotic wastewater by using iron ion doped metal organic framework material | |
| CN113019403B (en) | Double Z-type Bi loaded with cocatalyst2MoO6/Bi2WO6\ AgI/Ag photocatalyst and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20201103 |
|
| WD01 | Invention patent application deemed withdrawn after publication |