CN107673441B - Method for degrading rhodamine B under irradiation of ultraviolet lamp light source - Google Patents
Method for degrading rhodamine B under irradiation of ultraviolet lamp light source Download PDFInfo
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- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229940043267 rhodamine b Drugs 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 14
- 230000000593 degrading effect Effects 0.000 title claims abstract description 7
- 239000011941 photocatalyst Substances 0.000 claims abstract description 35
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 31
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 22
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 21
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004472 Lysine Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- 230000001699 photocatalysis Effects 0.000 claims abstract description 9
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 8
- 238000001179 sorption measurement Methods 0.000 claims abstract description 4
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 44
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 36
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 15
- 235000019441 ethanol Nutrition 0.000 claims description 13
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 11
- 229910017604 nitric acid Inorganic materials 0.000 claims description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 11
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- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 238000002835 absorbance Methods 0.000 description 4
- 239000002957 persistent organic pollutant Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
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- HTRJDXQPCKIFIU-UHFFFAOYSA-N silver;ethanol;nitrate Chemical compound [Ag+].CCO.[O-][N+]([O-])=O HTRJDXQPCKIFIU-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
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- 239000010842 industrial wastewater Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000013048 microbiological method Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
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Abstract
The invention belongs to a method for degrading rhodamine B under the irradiation of an ultraviolet lamp light source, which comprises the steps of adding 100mL of rhodamine B solution with the concentration of 10mg/L into a reaction tube of a photocatalytic instrument, adding 0.02g of graphene-loaded Ag photocatalyst with a concave cubic morphology prepared through hydrothermal reaction, carrying out ultrasonic dispersion for 4min, statically adsorbing in a dark room for 30min to achieve reaction adsorption balance, starting an ultraviolet light source and a magnetic stirring device, irradiating for 2 hours under ultraviolet light with the wavelength of 254nm, and loading the Ag catalyst on graphene, so that the defects that the common Ag photocatalyst is large in size, poor in dispersibility and easy to agglomerate are overcome; by adding CTAB and lysine and combining hydrothermal reaction conditions, the graphene-supported Ag photocatalyst with the concave cubic morphology and high selectivity is prepared, and the photocatalyst shows good catalytic activity on the degradation rate of rhodamine B under an ultraviolet light source.
Description
Technical Field
The invention belongs to the technical field of organic pollutant degradation, and particularly relates to a method for degrading rhodamine B by using a graphene-loaded Ag photocatalyst with a concave cubic morphology.
Background
Organic matters in industrial wastewater and waste gas are treated by a photocatalytic degradation method, attention is paid to people in recent years, the photocatalytic performance of a catalyst can be improved by controlling the structure and the shape, doping and the like, and in the research of photocatalytic degradation of organic pollutants, the metal dispersion degree and the dispersion condition of the catalyst in a dye solution are key factors influencing the catalytic activity of a photocatalytic degradation dye molecule. Compared with the general photocatalytic material, the nano photocatalytic material is mainly reflected in two aspects on the activity action of promoting the photocatalytic reaction: in view of the above photocatalytic mechanism, the strength of the oxidation and reduction depends on the concentration of the photo-generated electrons and holes. It is apparent that the smaller the photocatalyst particle size, the larger the total surface area, the higher the light absorption efficiency, and the greater the probability of electrons and holes moving to the surface. The powder graphene gradually becomes the focus of research due to large specific surface area, so that the application of the photocatalytic technology in the field of water treatment becomes possible. Since the 70 s of the 20 th century, people increasingly pay attention to the work of oxidizing pollutants in water by using metal photocatalysts, and the metal photocatalysts have the advantages that: firstly, the method utilizes the metal photocatalyst to oxidize and degrade pollutants in water, is different from water treatment of a simple physical method, a chemical method and a biological method, has simple treatment flow, does not have secondary pollution, and has higher treatment speed than a microbiological method; secondly, the metal photocatalyst can treat various inorganic and organic pollutants to mineralize the inorganic and organic pollutants, is an oxidation treatment method, and most importantly, the photocatalytic oxidation process can utilize sunlight resources, so that the energy is saved, and no pollution is caused.
Disclosure of Invention
The invention aims to provide a preparation method of a graphene-loaded Ag photocatalyst with a concave cubic morphology, which has high degradation rate on rhodamine B and short degradation time.
In order to achieve the purpose, the invention adopts the technical scheme that the preparation method of the Ag photocatalyst with the concave cubic morphology and loaded by graphene comprises the following steps: adding graphene into mixed acid of concentrated sulfuric acid and concentrated nitric acid at 85-100 ℃, wherein the weight ratio of the graphene to the mixed acid is 0.5-2: 1, filtering after 2-8 hours, washing, and drying to obtain modified graphene; dissolving silver nitrate in absolute ethyl alcohol to obtain an ethanol solution of the silver nitrate with the concentration of 0.3-1 mol/L, adding the modified graphene prepared in the step one into the ethanol solution of the silver nitrate with the concentration of 0.3-1 mol/L according to the solid-to-liquid ratio of 1 g: 20 ml-1 g: 30ml, and performing ultrasonic dispersion for 0.5-1 h to obtain a solution A; dissolving NaOH in 70-75% ethanol (volume fraction) to obtain solution B, wherein the concentration of NaOH in the solution B is 1.5-2 mol/L; dripping the solution B into the solution A under the stirring condition to obtain solution C, wherein the molar ratio of NaOH in the solution B to silver nitrate in the solution A is 1-1.05: 1; and fifthly, adding CTAB (cetyl trimethyl ammonium bromide) and lysine into the C solution, uniformly stirring, transferring to a reaction kettle, carrying out hydrothermal reaction at 180-200 ℃ for 2-4 h, filtering, washing and drying to obtain the graphene-loaded Ag photocatalyst with the concave cubic morphology.
Preferably, in the fifth step, the mass ratio of CTAB to lysine is 1-1.5: 1, and the solid-to-liquid ratio of CTAB to C liquid is 8-10 g: 1L.
In the step (i), the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is 2-4: 1, the concentration of the concentrated sulfuric acid is 98wt%, and the concentration of the concentrated nitric acid is 69 wt%.
The invention has the following beneficial effects: according to the invention, the Ag catalyst is loaded on the graphene, so that the defects of large size, poor dispersibility and easy agglomeration of a common Ag photocatalyst are avoided; by adding CTAB and lysine and combining hydrothermal reaction conditions, the graphene-supported Ag photocatalyst with the concave cubic morphology and high selectivity is prepared, and the photocatalyst shows good catalytic activity on the degradation rate of rhodamine B under an ultraviolet light source, and has a wide application prospect.
Drawings
Fig. 1 is a transmission electron micrograph of the graphene-supported Ag photocatalyst having a concave cubic morphology prepared in example 1;
fig. 2 is an XRD pattern of the graphene-supported Ag photocatalyst having a concave cubic morphology prepared in example 1;
fig. 3 is a graph of the degradation effect of the graphene-supported Ag photocatalyst with a concave cubic morphology on rhodamine B prepared in example 1;
fig. 4 is a transmission electron micrograph of the graphene-supported Ag photocatalyst prepared in control experiment 1.
Detailed Description
The invention will be further illustrated with reference to specific examples, without however restricting the scope of the invention thereto.
Example 1
A preparation method of a graphene-supported Ag photocatalyst with a concave cubic morphology comprises the following steps: adding graphene into mixed acid of concentrated sulfuric acid and concentrated nitric acid (the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is 3: 1) at 90 ℃, filtering, washing and drying after 6 hours to obtain modified graphene; dissolving silver nitrate in absolute ethyl alcohol to obtain an ethanol solution of the silver nitrate with the concentration of 0.6mol/L, adding the modified graphene prepared in the step I into the ethanol solution of the silver nitrate with the concentration of 0.6mol/L according to the solid-to-liquid ratio of 1 g: 25ml, and performing ultrasonic dispersion for 0.5h to obtain a solution A; dissolving NaOH in 75% ethanol to obtain solution B, wherein the concentration of NaOH in the solution B is 1.5 mol/L; dripping the solution B into the solution A under the stirring condition to obtain solution C, wherein the molar ratio of NaOH in the solution B to silver nitrate in the solution A is 1: 1; and fifthly, adding CTAB (cetyl trimethyl ammonium bromide) and lysine into the C solution, uniformly stirring, transferring the mixture into a reaction kettle, carrying out hydrothermal reaction for 2 hours at 180 ℃, filtering, washing and drying to obtain the graphene-loaded Ag photocatalyst with the shape of a concave cube. In the fifth step, the mass ratio of CTAB to lysine is 1: 1, and the solid-to-liquid ratio of CTAB to C liquid is 10 g: 1L.
A Transmission Electron Microscope (TEM) photograph of the graphene-supported Ag photocatalyst with a concave cubic morphology prepared in example 1 is shown in fig. 1, and it can be seen from fig. 1 that the prepared graphene-supported Ag photocatalyst is a regular concave cubic, and has good morphology selectivity.
Comparative example 1
The difference between the comparative example 1 and the example 1 is that CTAB and lysine are not added in the step (v), the solution C is directly transferred into a reaction kettle, hydrothermal reaction is carried out for 2h at 180 ℃, and then filtration, washing and drying are carried out.
The graphene-supported Ag photocatalyst prepared in comparative example 1 is shown in fig. 4, and it can be seen from fig. 4 that the morphology of the prepared photocatalyst is irregular.
Example 2
A preparation method of a graphene-supported Ag photocatalyst with a concave cubic morphology comprises the following steps: adding graphene into mixed acid of concentrated sulfuric acid and concentrated nitric acid (the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is 4: 1) at 100 ℃, filtering, washing and drying after 2 hours to obtain modified graphene; dissolving silver nitrate in absolute ethyl alcohol to obtain an ethanol solution of the silver nitrate with the concentration of 0.3mol/L, adding the modified graphene prepared in the step I into the ethanol solution of the silver nitrate with the concentration of 0.3mol/L according to the solid-to-liquid ratio of 1 g: 20ml, and performing ultrasonic dispersion for 1h to obtain a solution A; dissolving NaOH in 70% ethanol to obtain solution B, wherein the concentration of NaOH in the solution B is 2 mol/L; dripping the solution B into the solution A under the stirring condition to obtain solution C, wherein the molar ratio of NaOH in the solution B to silver nitrate in the solution A is 1.05: 1; and fifthly, adding CTAB (cetyl trimethyl ammonium bromide) and lysine into the C solution, uniformly stirring, transferring the mixture into a reaction kettle, carrying out hydrothermal reaction for 2 hours at 200 ℃, filtering, washing and drying to obtain the graphene-loaded Ag photocatalyst with the shape of a concave cube. In the fifth step, the mass ratio of CTAB to lysine is 1.5: 1, and the solid-to-liquid ratio of CTAB to C liquid is 8 g: 1L.
Example 3
A preparation method of a graphene-supported Ag photocatalyst with a concave cubic morphology comprises the following steps: adding graphene into mixed acid of concentrated sulfuric acid and concentrated nitric acid (the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is 2: 1) at 85 ℃, filtering, washing and drying after 8 hours to obtain modified graphene; dissolving silver nitrate in absolute ethyl alcohol to obtain a silver nitrate ethanol solution with the concentration of 1mol/L, adding the modified graphene prepared in the step I into the silver nitrate ethanol solution with the concentration of 1mol/L according to the solid-to-liquid ratio of 1 g: 30ml, and performing ultrasonic dispersion for 0.5h to obtain a solution A; dissolving NaOH in 75% ethanol to obtain solution B, wherein the concentration of NaOH in the solution B is 1.5 mol/L; dripping the solution B into the solution A under the stirring condition to obtain solution C, wherein the molar ratio of NaOH in the solution B to silver nitrate in the solution A is 1.03: 1; and fifthly, adding CTAB (cetyl trimethyl ammonium bromide) and lysine into the C solution, uniformly stirring, transferring the mixture into a reaction kettle, carrying out hydrothermal reaction for 4 hours at 180 ℃, filtering, washing and drying to obtain the graphene-loaded Ag photocatalyst with the shape of a concave cube. In the fifth step, the mass ratio of CTAB to lysine is 1-1.2: 1, and the solid-to-liquid ratio of CTAB to C liquid is 9 g: 1L.
Degradation test
The degradation experiment steps of the graphene-supported Ag photocatalyst with the concave cubic morphology on rhodamine B under the irradiation of an ultraviolet light source are as follows: adding 100mL of 10mg/L rhodamine B solution into a reaction tube of a photocatalytic instrument, then adding 0.02g of Ag photocatalyst prepared by hydrothermal reaction, performing ultrasonic dispersion for 4min, statically adsorbing in a dark room for 30min to reach reaction adsorption balance, starting an ultraviolet light source and a magnetic stirring device, sampling at intervals of 20min in the illumination process, performing centrifugal separation, taking supernatant at the position where the maximum absorption wavelength L =554nm of rhodamine B, measuring the absorbance of the sample by using a 722N visible spectrophotometer, and determining the absorbance by using a formula: DC = [ (a0-Ai)/a0 ]' 100% complete the calculation of the degradation rate, where a0 is the absorbance of 10mg/L of the rhodamine B solution, and Ai is the absorbance of the rhodamine B solution measured at the time of the timed sampling. When the rhodamine B is irradiated for 2 hours under ultraviolet light with the wavelength of 254nm, the degradation rate of the rhodamine B is 97.1 percent.
Claims (3)
1. A method for degrading rhodamine B under the irradiation of an ultraviolet lamp light source is characterized in that 100mL of rhodamine B solution with the concentration of 10mg/L is added into a reaction tube of a photocatalytic instrument, then 0.02g of graphene-loaded Ag photocatalyst with a concave cubic morphology prepared through hydrothermal reaction is added, ultrasonic dispersion is carried out for 4min, reaction adsorption balance is achieved after static adsorption is carried out in a dark room for 30min, an ultraviolet light source and a magnetic stirring device are started, and irradiation is carried out for 2 hours under ultraviolet light with the wavelength of 254nm, and the method is characterized in that: the preparation method of the graphene-loaded Ag photocatalyst with the concave cubic morphology comprises the following steps: adding graphene into mixed acid of concentrated sulfuric acid and concentrated nitric acid at 85-100 ℃, wherein the weight ratio of the graphene to the mixed acid is 0.5-2: 1, filtering after 2-8 hours, washing, and drying to obtain modified graphene; dissolving silver nitrate in absolute ethyl alcohol to obtain an ethanol solution of the silver nitrate with the concentration of 0.3-1 mol/L, adding the modified graphene prepared in the step one into the ethanol solution of the silver nitrate with the concentration of 0.3-1 mol/L according to the solid-to-liquid ratio of 1 g: 20 ml-1 g: 30ml, and performing ultrasonic dispersion for 0.5-1 h to obtain a solution A; dissolving NaOH in ethanol with the volume fraction of 70-75% to obtain solution B, wherein the concentration of NaOH in the solution B is 1.5-2 mol/L; dripping the solution B into the solution A under the stirring condition to obtain solution C, wherein the molar ratio of NaOH in the solution B to silver nitrate in the solution A is 1-1.05: 1; and fifthly, adding CTAB and lysine into the C solution, uniformly stirring, transferring to a reaction kettle, carrying out hydrothermal reaction at 180-200 ℃ for 2-4 h, filtering, washing and drying to obtain the graphene-loaded Ag photocatalyst with the concave cubic morphology.
2. The method for degrading rhodamine B under the irradiation of an ultraviolet lamp light source according to claim 1, wherein in the fifth step, the mass ratio of CTAB to lysine is 1-1.5: 1, and the solid-to-liquid ratio of CTAB to C liquid is 8-10 g: 1L.
3. The method for degrading rhodamine B under the irradiation of an ultraviolet lamp light source of claim 1, wherein the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid in the step (i) is 2-4: 1.
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| CN201711187905.4A CN107673441B (en) | 2016-04-11 | 2016-04-11 | Method for degrading rhodamine B under irradiation of ultraviolet lamp light source |
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| CN102631939B (en) * | 2012-03-28 | 2014-05-28 | 江苏大学 | Graphene/silver phosphate composite visible light photocatalyst and preparation method thereof |
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