CN112337483B - Preparation method of efficient graphene-based cerium nano composite material, product and application thereof - Google Patents
Preparation method of efficient graphene-based cerium nano composite material, product and application thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 56
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 51
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 28
- 229910052684 Cerium Inorganic materials 0.000 title claims abstract description 23
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000003756 stirring Methods 0.000 claims abstract description 37
- 239000000203 mixture Substances 0.000 claims abstract description 34
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 26
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- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 20
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 20
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 20
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims abstract description 20
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 20
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052979 sodium sulfide Inorganic materials 0.000 claims abstract description 20
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000967 suction filtration Methods 0.000 claims abstract description 19
- 238000005406 washing Methods 0.000 claims abstract description 19
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 3
- MYSWGUAQZAJSOK-UHFFFAOYSA-N ciprofloxacin Chemical compound C12=CC(N3CCNCC3)=C(F)C=C2C(=O)C(C(=O)O)=CN1C1CC1 MYSWGUAQZAJSOK-UHFFFAOYSA-N 0.000 claims description 100
- 229960003405 ciprofloxacin Drugs 0.000 claims description 50
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- 238000009210 therapy by ultrasound Methods 0.000 claims description 30
- 238000005303 weighing Methods 0.000 claims description 13
- 230000000593 degrading effect Effects 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 31
- 239000002131 composite material Substances 0.000 abstract description 10
- 150000001875 compounds Chemical class 0.000 abstract description 8
- 230000002195 synergetic effect Effects 0.000 abstract description 3
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 23
- 230000015556 catabolic process Effects 0.000 description 17
- 238000006731 degradation reaction Methods 0.000 description 17
- 239000011259 mixed solution Substances 0.000 description 13
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 12
- 230000001105 regulatory effect Effects 0.000 description 11
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 3
- 229940012189 methyl orange Drugs 0.000 description 3
- 229960000907 methylthioninium chloride Drugs 0.000 description 3
- 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 description 3
- 229940043267 rhodamine b Drugs 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- XMPZTFVPEKAKFH-UHFFFAOYSA-P ceric ammonium nitrate Chemical compound [NH4+].[NH4+].[Ce+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O XMPZTFVPEKAKFH-UHFFFAOYSA-P 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
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- 238000005260 corrosion Methods 0.000 description 1
- ZXJXZNDDNMQXFV-UHFFFAOYSA-M crystal violet Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1[C+](C=1C=CC(=CC=1)N(C)C)C1=CC=C(N(C)C)C=C1 ZXJXZNDDNMQXFV-UHFFFAOYSA-M 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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- B01J27/04—Sulfides
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Abstract
The invention discloses a preparation method of a high-efficiency graphene-based cerium nano composite material, a product and an application thereof, which comprises the steps of placing graphite oxide in deionized water, and uniformly dispersing by ultrasonic to obtain a graphite oxide aqueous solution; adding ammonium ceric nitrate into the graphite oxide aqueous solution, uniformly stirring, adding cadmium nitrate and sodium sulfide, continuously stirring to fully and uniformly mix the system, and adjusting the pH value to obtain a mixed reaction system; and carrying out hydrothermal reaction on the mixed reaction system, carrying out suction filtration, washing and drying, and grinding to obtain the graphene-based cerium nano composite material. Graphene and CeO in the composite material2And the good synergistic effect is achieved between the compound and the CdS, so that the photocatalytic performance of the compound material is improved.
Description
Technical Field
The invention belongs to the technical field of photocatalytic degradation, and particularly relates to a preparation method of a high-efficiency graphene-based cerium nano composite material, and a product and application thereof.
Background
With the progress of science and technology and the development of industry, the human society has more abundant materials and the living standard is continuously improved, but the human society also brings along the development process of industrySerious environmental pollution and energy shortage. Semiconductor photocatalytic technology is considered as one of safe and effective methods for solving global energy shortage and environmental pollution. The semiconductor photocatalytic material can effectively utilize solar energy to thoroughly decompose organic matters into CO2Inorganic micromolecules such as water and the like, and no secondary pollution is caused; meanwhile, water can be directly decomposed by utilizing the photocatalysis technology to prepare clean energy hydrogen, so that the two problems of energy shortage and environmental pollution are fundamentally solved.
CeO2Have received considerable attention from researchers due to their excellent physicochemical properties. Since CeO2Has high oxygen storage capacity and abundant oxygen vacancies and reversible Ce3+/Ce4+The excellent catalytic performance of the photocatalyst, such as light corrosion resistance, is reported to be a high-efficiency photocatalyst.
However, under visible light irradiation, since pure CeO2The photoproduction electron-hole pair has higher recombination rate, thereby preventing the wide application of the photoproduction electron-hole pair in the aspect of photocatalysis. By the element doping, heterojunction construction, noble metal deposition and other technologies, the visible light absorption performance of the cerium semiconductor material can be effectively improved or the recombination of photogenerated electrons and holes can be inhibited, so that the photocatalytic performance of the cerium semiconductor material is further improved. These methods all play a role in improving the photocatalytic effect to some extent, but the reactivity and stability to visible light still cannot meet the actual needs.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made keeping in mind the above and/or other problems occurring in the prior art.
Therefore, the present invention aims to overcome the defects in the prior art and provide a preparation method of a high efficiency graphene-based cerium nanocomposite.
In order to solve the technical problems, the invention provides the following technical scheme: a preparation method of high-efficiency graphene-based cerium nano composite material comprises the following steps,
placing graphite oxide in deionized water, and uniformly dispersing by ultrasonic to obtain a graphite oxide aqueous solution;
adding ammonium ceric nitrate into the graphite oxide aqueous solution, uniformly stirring, adding cadmium nitrate and sodium sulfide, continuously stirring to fully and uniformly mix the system, and adjusting the pH value to obtain a mixed reaction system;
and carrying out hydrothermal reaction on the mixed reaction system, carrying out suction filtration, washing and drying, and grinding to obtain the graphene-based cerium nano composite material.
As a preferable scheme of the preparation method of the high-efficiency graphene-based cerium nanocomposite material, the preparation method comprises the following steps: and placing the graphite oxide in deionized water for uniform ultrasonic dispersion, wherein the ultrasonic time is 20-50 min, the ultrasonic power is 200-300W, and the ultrasonic frequency is 20-60 kHz.
As a preferable scheme of the preparation method of the high-efficiency graphene-based cerium nanocomposite material, the preparation method comprises the following steps: the cerium ammonium nitrate is added into the graphite oxide aqueous solution and stirred uniformly, wherein the stirring time is 30 min.
As a preferable scheme of the preparation method of the high-efficiency graphene-based cerium nanocomposite material, the preparation method comprises the following steps: and adding cadmium nitrate and sodium sulfide, wherein the molar ratio of the cadmium nitrate to the sodium sulfide is 1: 1-1: 3.
As a preferable scheme of the preparation method of the high-efficiency graphene-based cerium nanocomposite material, the preparation method comprises the following steps: and the pH is adjusted to be 8-10.
As a preferable scheme of the preparation method of the high-efficiency graphene-based cerium nanocomposite material, the preparation method comprises the following steps: the mixed reaction system comprises cerium ammonium nitrate, cadmium nitrate and sodium sulfide in a molar ratio of 3:1: 1-1: 3: 3.
As a preferable scheme of the preparation method of the high-efficiency graphene-based cerium nanocomposite material, the preparation method comprises the following steps: the hydrothermal reaction temperature is 160-200 ℃, and the hydrothermal reaction time is 16-24 h.
As a preferable scheme of the preparation method of the high-efficiency graphene-based cerium nanocomposite material, the preparation method comprises the following steps: and drying at the drying temperature of 60-80 ℃ for 10-14 h.
The invention further aims to overcome the defects in the prior art and provide the nanocomposite prepared by the preparation method of the efficient graphene-based cerium nanocomposite.
The invention also aims to overcome the defects in the prior art and provide the application of the high-efficiency graphene-based cerium nano composite material in degrading ciprofloxacin in water under visible light.
The invention has the beneficial effects that:
CeO prepared by the invention2The size of the-CdS heterojunction composite material is 5-25 nm, and when graphene is introduced, CeO2The CdS/RGO compound has uniform distribution of each component; during photocatalytic degradation, CeO2The CdS/RGO complex favours electrons from CeO2And CdS is transferred to the graphene sheet; graphene and CeO in the composite material2And the good synergistic effect is achieved between the compound and the CdS, so that the photocatalytic performance of the compound material is improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
FIG. 1 shows CeO obtained in example 1 of the present invention2XRD pattern of CdS/RGO composite.
FIG. 2 shows CeO prepared by the present invention2、CdS、CeO2-CdS、CeO2/RGO and CeO2-graph of photocatalytic degradation of ciprofloxacin under visible light irradiation by CdS/RGO composite.
FIG. 3 is the present inventionInventive CeO2-photo-catalytic degradation pervasive performance diagram of CdS/RGO composite material.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, specific embodiments thereof are described in detail below with reference to examples of the specification.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1:
(1) 1.122g of graphite oxide is put into 60mL of deionized water and subjected to ultrasonic treatment to be uniformly dispersed, wherein the ultrasonic treatment time is 50min, the ultrasonic power is 200W, and the ultrasonic frequency is 40 kHz;
(2) weighing 0.548g of ammonium ceric nitrate, adding into the mixture obtained in the step (1), and continuously stirring for 30 min;
(3) then 0.308g of cadmium nitrate and 0.240g of sodium sulfide are added into the mixture in the step (2) and stirred for 30 min;
(4) regulating the pH value of the mixed solution obtained in the step (3) to 9 by using 3M NaOH, stirring for 30min, and finally carrying out hydrothermal reaction under the reaction conditions of 180 ℃ and 24 h;
(5) and taking out the hydrothermal kettle, and performing suction filtration, washing and drying to obtain the CeO2-CdS/RGO nano composite material.
The prepared CeO2-CdS/RGO nano composite material degrades ciprofloxacin in water under visible light to measure the photocatalytic activity of the ciprofloxacin, and the degradation rate of the ciprofloxacin within 2h is found to be over 90%. The photocatalytic activity measuring method comprises the following steps: the CIP (40mg/L) was degraded at room temperature (25 deg.c) with 20mg of the catalyst, and the change in concentration of CIP was obtained by measuring the absorption peak of the CIP solution at 271nm by an ultraviolet-visible spectrophotometer, thereby calculating the degradation rate of ciprofloxacin.
FIG. 1 is an XRD pattern of the prepared CeO2-CdS/RGO photocatalytic material, and the prepared product is CeO2-CdS/RGO by X-ray powder diffraction characterization.
Example 2:
(1) 0.537g of graphite oxide is put into 60mL of deionized water and subjected to ultrasonic treatment to be uniformly dispersed, wherein the ultrasonic treatment time is 50min, the ultrasonic power is 200W, and the ultrasonic frequency is 40 kHz;
(2) weighing 0.548g of ammonium ceric nitrate, adding into the mixture obtained in the step (1), and continuously stirring for 30 min;
(3) then 0.308g of cadmium nitrate and 0.240g of sodium sulfide are added into the mixture in the step (2) and stirred for 30 min;
(4) regulating the pH value of the mixed solution obtained in the step (3) to 9 by using 3M NaOH, stirring for 30min, and finally carrying out hydrothermal reaction under the reaction conditions of 180 ℃ and 24 h;
(5) and taking out the hydrothermal kettle, and performing suction filtration, washing and drying to obtain the CeO2-CdS/RGO nano composite material.
The prepared CeO2-CdS/RGO nano composite material degrades ciprofloxacin in water under visible light to measure the photocatalytic activity of the ciprofloxacin, and the degradation rate of the ciprofloxacin within 2h is found to be more than 82%.
Example 3:
(1) 0.823g of graphite oxide is placed in 60mL of deionized water and subjected to ultrasonic treatment to be uniformly dispersed, wherein the ultrasonic treatment time is 50min, the ultrasonic power is 200W, and the ultrasonic frequency is 40 kHz;
(2) weighing 0.548g of ammonium ceric nitrate, adding into the mixture obtained in the step (1), and continuously stirring for 30 min;
(3) then 0.308g of cadmium nitrate and 0.240g of sodium sulfide are added into the mixture in the step (2) and stirred for 30 min;
(4) regulating the pH value of the mixed solution obtained in the step (3) to 9 by using 3M NaOH, stirring for 30min, and finally carrying out hydrothermal reaction under the reaction conditions of 180 ℃ and 24 h;
(5) and taking out the hydrothermal kettle, and performing suction filtration, washing and drying to obtain the CeO2-CdS/RGO nano composite material.
The prepared CeO2-CdS/RGO nano composite material degrades ciprofloxacin in water under visible light to measure the photocatalytic activity of the ciprofloxacin, and the degradation rate of the ciprofloxacin within 2h is found to be more than 82%.
Example 4:
(1) 0.970g of graphite oxide is put into 60mL of deionized water and subjected to ultrasonic treatment to be uniformly dispersed, wherein the ultrasonic treatment time is 50min, the ultrasonic power is 200W, and the ultrasonic frequency is 40 kHz;
(2) weighing 0.548g of ammonium ceric nitrate, adding into the mixture obtained in the step (1), and continuously stirring for 30 min;
(3) then 0.308g of cadmium nitrate and 0.240g of sodium sulfide are added into the mixture in the step (2) and stirred for 30 min;
(4) regulating the pH value of the mixed solution obtained in the step (3) to 9 by using 3M NaOH, stirring for 30min, and finally carrying out hydrothermal reaction under the reaction conditions of 180 ℃ and 24 h;
(5) and taking out the hydrothermal kettle, and performing suction filtration, washing and drying to obtain the CeO2-CdS/RGO nano composite material.
The prepared CeO2-CdS/RGO nano composite material degrades ciprofloxacin in water under visible light to measure the photocatalytic activity of the ciprofloxacin, and the degradation rate of the ciprofloxacin within 2h is found to be over 84%.
Example 5:
(1) 1.433g of graphite oxide is put in 60mL of deionized water and subjected to ultrasonic treatment to be uniformly dispersed, wherein the ultrasonic treatment time is 50min, the ultrasonic power is 200W, and the ultrasonic frequency is 40 kHz;
(2) weighing 0.548g of ammonium ceric nitrate, adding into the mixture obtained in the step (1), and continuously stirring for 30 min;
(3) then 0.308g of cadmium nitrate and 0.240g of sodium sulfide are added into the mixture in the step (2) and stirred for 30 min;
(4) regulating the pH value of the mixed solution obtained in the step (3) to 9 by using 3M NaOH, stirring for 30min, and finally carrying out hydrothermal reaction under the reaction conditions of 180 ℃ and 24 h;
(5) and taking out the hydrothermal kettle, and performing suction filtration, washing and drying to obtain the CeO2-CdS/RGO nano composite material.
The prepared CeO2-CdS/RGO nano composite material degrades ciprofloxacin in water under visible light to measure the photocatalytic activity of the ciprofloxacin, and the degradation rate of the ciprofloxacin within 2h is found to be over 84%.
Example 6:
(1) 3.224g of graphite oxide is put into 60mL of deionized water and subjected to ultrasonic treatment to be uniformly dispersed, wherein the ultrasonic treatment time is 50min, the ultrasonic power is 200W, and the ultrasonic frequency is 40 kHz;
(2) weighing 0.548g of ammonium ceric nitrate, adding into the mixture obtained in the step (1), and continuously stirring for 30 min;
(3) then 0.308g of cadmium nitrate and 0.240g of sodium sulfide are added into the mixture in the step (2) and stirred for 30 min;
(4) regulating the pH value of the mixed solution obtained in the step (3) to 9 by using 3M NaOH, stirring for 30min, and finally carrying out hydrothermal reaction under the reaction conditions of 180 ℃ and 24 h;
(5) and taking out the hydrothermal kettle, and performing suction filtration, washing and drying to obtain the CeO2-CdS/RGO nano composite material.
The prepared CeO2-CdS/RGO nano composite material degrades ciprofloxacin in water under visible light to measure the photocatalytic activity of the ciprofloxacin, and the degradation rate of the ciprofloxacin within 2h is found to be more than 81%.
Example 7:
(1) 0.823g of graphite oxide is placed in 60mL of deionized water and subjected to ultrasonic treatment to be uniformly dispersed, wherein the ultrasonic treatment time is 50min, the ultrasonic power is 200W, and the ultrasonic frequency is 40 kHz;
(2) weighing 0.548g of ammonium ceric nitrate, adding into the mixture obtained in the step (1), and continuously stirring for 30 min;
(3) then 0.308g of cadmium nitrate and 0.240g of sodium sulfide are added into the mixture in the step (2) and stirred for 30 min;
(4) regulating the pH value of the mixed solution obtained in the step (3) to 9 by using 3M NaOH, stirring for 30min, and finally carrying out hydrothermal reaction under the reaction conditions of 180 ℃ and 24 h;
(5) and taking out the hydrothermal kettle, and performing suction filtration, washing and drying to obtain the CeO2-CdS/RGO nano composite material.
The prepared CeO2-CdS/RGO nano composite material degrades methyl violet (BV), Methylene Blue (MB), rhodamine B (RhB), Methyl Orange (MO) and active blue (RB) in water under visible light to measure the universal performance of the photocatalytic activity, and as shown in FIG. 3, the degradation rates of BV, MB, RhB, MO and RB within 2h are 100%, 92%, 89%, 75% and 72%.
Example 8:
(1) 2.144g of graphite oxide is put into 60mL of deionized water and subjected to ultrasonic treatment to be uniformly dispersed, wherein the ultrasonic treatment time is 50min, the ultrasonic power is 200W, and the ultrasonic frequency is 40 kHz;
(2) weighing 0.548g of ammonium ceric nitrate, adding into the mixture obtained in the step (1), and continuously stirring for 30 min;
(3) then 0.924g of cadmium nitrate and 0.720g of sodium sulfide are added into the mixture obtained in the step (2), and the mixture is stirred for 30 min;
(4) regulating the pH value of the mixed solution obtained in the step (3) to 9 by using 3M NaOH, stirring for 30min, and finally carrying out hydrothermal reaction under the reaction conditions of 180 ℃ and 24 h;
(5) and taking out the hydrothermal kettle, and performing suction filtration, washing and drying to obtain the CeO2-CdS/RGO nano composite material.
The prepared CeO2-CdS/RGO nano composite material degrades ciprofloxacin in water under visible light to measure the photocatalytic activity of the ciprofloxacin, and the degradation rate of the ciprofloxacin within 2h is found to be over 84%.
Example 9:
(1) 2.144g of graphite oxide is put into 60mL of deionized water and subjected to ultrasonic treatment to be uniformly dispersed, wherein the ultrasonic treatment time is 50min, the ultrasonic power is 200W, and the ultrasonic frequency is 40 kHz;
(2) 1.644g of ammonium ceric nitrate is weighed and added into the mixture in the step (1), and the mixture is continuously stirred for 30 min;
(3) then 0.308g of cadmium nitrate and 0.240g of sodium sulfide are added into the mixture in the step (2) and stirred for 30 min;
(4) regulating the pH value of the mixed solution obtained in the step (3) to 9 by using 3M NaOH, stirring for 30min, and finally carrying out hydrothermal reaction under the reaction conditions of 180 ℃ and 24 h;
(5) and taking out the hydrothermal kettle, and performing suction filtration, washing and drying to obtain the CeO2-CdS/RGO nano composite material.
The prepared CeO2-CdS/RGO nano composite material degrades ciprofloxacin in water under visible light to measure the photocatalytic activity of the ciprofloxacin, and the degradation rate of the ciprofloxacin within 2h is found to be more than 82%.
Example 10:
(1) 0.823g of graphite oxide is placed in 60mL of deionized water and subjected to ultrasonic treatment to be uniformly dispersed, wherein the ultrasonic treatment time is 50min, the ultrasonic power is 200W, and the ultrasonic frequency is 40 kHz;
(2) weighing 0.548g of ammonium ceric nitrate, adding into the mixture obtained in the step (1), and continuously stirring for 30 min;
(3) then 0.308g of cadmium nitrate and 0.240g of sodium sulfide are added into the mixture in the step (2) and stirred for 30 min;
(4) regulating the pH value of the mixed solution obtained in the step (3) to 9 by using 3M NaOH, stirring for 30min, and finally carrying out hydrothermal reaction under the reaction conditions of 180 ℃ and 16 h;
(5) and taking out the hydrothermal kettle, and performing suction filtration, washing and drying to obtain the CeO2-CdS/RGO nano composite material.
The prepared CeO2-CdS/RGO nano composite material degrades ciprofloxacin in water under visible light to measure the photocatalytic activity of the ciprofloxacin, and the degradation rate of the ciprofloxacin within 2h is found to be more than 81%.
Example 11:
1) 0.823g of graphite oxide is placed in 60mL of deionized water and subjected to ultrasonic treatment to be uniformly dispersed, wherein the ultrasonic treatment time is 50min, the ultrasonic power is 200W, and the ultrasonic frequency is 40 kHz;
(2) weighing 0.548g of ammonium ceric nitrate, adding into the mixture obtained in the step (1), and continuously stirring for 30 min;
(3) then 0.308g of cadmium nitrate and 0.240g of sodium sulfide are added into the mixture in the step (2) and stirred for 30 min;
(4) adjusting the pH value of the mixed solution obtained in the step (3) to 9 by using 3M NaOH, stirring for 30min, and finally carrying out hydrothermal reaction under the reaction conditions of 180 ℃ and 20 h;
(5) and taking out the hydrothermal kettle, and performing suction filtration, washing and drying to obtain the CeO2-CdS/RGO nano composite material.
The prepared CeO2-CdS/RGO nano composite material degrades ciprofloxacin in water under visible light to measure the photocatalytic activity of the ciprofloxacin, and the degradation rate of the ciprofloxacin within 2h is found to be more than 85%.
Example 12:
(1) 0.823g of graphite oxide is placed in 60mL of deionized water and subjected to ultrasonic treatment to be uniformly dispersed, wherein the ultrasonic treatment time is 50min, the ultrasonic power is 200W, and the ultrasonic frequency is 40 kHz;
(2) weighing 0.548g of ammonium ceric nitrate, adding into the mixture obtained in the step (1), and continuously stirring for 30 min;
(3) then 0.308g of cadmium nitrate and 0.240g of sodium sulfide are added into the mixture in the step (2) and stirred for 30 min;
(4) adjusting the pH value of the mixed solution obtained in the step (3) to 7 by using 3M NaOH, stirring for 30min, and finally carrying out hydrothermal reaction under the reaction conditions of 180 ℃ and 24 h;
(5) and taking out the hydrothermal kettle, and performing suction filtration, washing and drying to obtain the CeO2-CdS/RGO nano composite material.
The prepared CeO2-CdS/RGO nano composite material degrades ciprofloxacin in water under visible light to measure the photocatalytic activity of the ciprofloxacin, and the degradation rate of the ciprofloxacin within 2h is found to be more than 80%.
Example 13:
(1) 0.823g of graphite oxide is placed in 60mL of deionized water and subjected to ultrasonic treatment to be uniformly dispersed, wherein the ultrasonic treatment time is 50min, the ultrasonic power is 200W, and the ultrasonic frequency is 40 kHz;
(2) weighing 0.548g of ammonium ceric nitrate, adding into the mixture obtained in the step (1), and continuously stirring for 30 min;
(3) then 0.308g of cadmium nitrate and 0.240g of sodium sulfide are added into the mixture in the step (2) and stirred for 30 min;
(4) regulating the pH value of the mixed solution obtained in the step (3) to 11 by using 3M NaOH, stirring for 30min, and finally carrying out hydrothermal reaction under the reaction conditions of 180 ℃ and 24 h;
(5) and taking out the hydrothermal kettle, and performing suction filtration, washing and drying to obtain the CeO2-CdS/RGO nano composite material.
The prepared CeO2-CdS/RGO nano composite material degrades ciprofloxacin in water under visible light to measure the photocatalytic activity of the ciprofloxacin, and the degradation rate of the ciprofloxacin within 2h is found to be more than 76%.
Comparative example 1:
(1) 0.548g of ammonium ceric nitrate is put into 60mL of deionized water and continuously stirred for 30 min;
(2) adjusting the pH value to 9 by using 3M NaOH, stirring for 30min, and finally carrying out hydrothermal reaction under the reaction conditions of 180 ℃ and 24 h;
(3) and taking out the hydrothermal kettle, and carrying out suction filtration, washing and drying to obtain the CeO2 nano material.
The prepared CeO2 photocatalytic material is used for degrading ciprofloxacin in water under visible light to measure the photocatalytic activity of ciprofloxacin, and the degradation rate of ciprofloxacin within 2h is found to exceed 53%.
Comparative example 2:
(1) 0.548g of ammonium ceric nitrate is put into 60mL of deionized water and continuously stirred for 30 min;
(2) adding 0.308g of cadmium nitrate and 0.240g of sodium sulfide into the mixture obtained in the step (1), continuously stirring for 30min, and finally carrying out hydrothermal reaction under the reaction conditions of 180 ℃ and 24 h;
(3) and taking out the hydrothermal kettle, and carrying out suction filtration, washing and drying to obtain the CeO2-CdS nanocomposite.
The prepared CeO2-CdS photocatalytic material is used for degrading ciprofloxacin in water under visible light to measure the photocatalytic activity of the ciprofloxacin, and the degradation rate of the ciprofloxacin within 2h is found to be more than 77%.
Comparative example 3
(1) 1.122g of graphite oxide is put into 60mL of deionized water and subjected to ultrasonic treatment to be uniformly dispersed, wherein the ultrasonic treatment time is 50min, the ultrasonic power is 200W, and the ultrasonic frequency is 40 kHz;
(2) adding 0.548g of ammonium ceric nitrate into the mixture obtained in the step (1), continuously stirring for 30min, and finally carrying out hydrothermal reaction under the reaction conditions of 180 ℃ and 24 h;
(3) and taking out the hydrothermal kettle, and carrying out suction filtration, washing and drying to obtain the CeO2/RGO nano composite material.
The prepared CeO2/RGO photocatalytic material is used for degrading ciprofloxacin in water under visible light to measure the photocatalytic activity of the ciprofloxacin, and the degradation rate of the ciprofloxacin within 2h is over 64%.
FIG. 2 shows the obtained CeO2、CdS、CeO2-CdS、CeO2/RGO and CeO2The photocatalytic degradation of ciprofloxacin from the-CdS/RGO composite material under the irradiation of visible light is shown, and CeO2The CdS/RGO composite material has better catalytic effect.
According to the CeO2/RGO photocatalytic material prepared by the invention, under the irradiation of light, electron-hole pairs are photogenerated on the surface of CeO2/CdS/RGO, wherein e-is excited into a Conduction Band (CB) of CeO2 and CdS, and h is kept in a Valence Band (VB); h when photo-generated electrons are transferred from CB of CdS to electron transfer of CeO2+From VB of CeO2 to VB of CdS, thereby promoting separation of electron-hole pairs and suppressing heavy electronsGroup (d); RGO acts as an acceptor and donor for e-providing another nanochannel for e-transfer and extending the lifetime of electron-hole pairs.
CeO prepared by the invention2The size of the-CdS heterojunction composite material is 5-25 nm, and when graphene is introduced, CeO2The CdS/RGO compound has uniform distribution of each component; during photocatalytic degradation, CeO2The CdS/RGO complex favours electrons from CeO2And CdS is transferred to the graphene sheet; graphene and CeO in the composite material2And the good synergistic effect is achieved between the compound and the CdS, so that the photocatalytic performance of the compound material is improved.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (3)
1. A preparation method of a high-efficiency graphene-based cerium nano composite material is characterized by comprising the following steps: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
putting 1.122g of graphite oxide in 60mL of deionized water, and performing ultrasonic treatment to uniformly disperse the graphite oxide to prepare a graphite oxide aqueous solution, wherein the ultrasonic treatment time is 50min, the ultrasonic power is 200W, and the ultrasonic frequency is 40 kHz;
weighing 0.548g of ammonium ceric nitrate, adding the ammonium ceric nitrate into the graphite oxide aqueous solution, continuously stirring for 30min, uniformly stirring, adding 0.308g of cadmium nitrate and 0.240g of sodium sulfide, stirring for 30min to fully and uniformly mix the system, adjusting the pH value to 9 by using 3M NaOH, and stirring for 30min to obtain a mixed reaction system;
carrying out hydrothermal reaction on the mixed reaction system, carrying out suction filtration, washing and drying, and grinding to obtain the graphene-based cerium nano composite material CeO2-CdS/RGO, wherein the hydrothermal reaction temperature is 180 ℃ and the hydrothermal reaction time is 24 h.
2. The nanocomposite prepared by the preparation method of the high-efficiency graphene-based cerium nanocomposite according to claim 1.
3. The use of the high efficiency graphene-based cerium nanocomposite as claimed in claim 2 for degrading ciprofloxacin in water under visible light.
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| CN104689835A (en) * | 2015-03-18 | 2015-06-10 | 湖南大学 | CeO2 (Cerium Oxide) nano-particle/CdS (Cadmium Sulfide) nano-rod composite photo-catalyst as well as preparation method and application thereof |
| CN110152609A (en) * | 2019-06-12 | 2019-08-23 | 常州大学 | A kind of high-efficient graphite alkenyl bismuth system nanocomposite and preparation method thereof |
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| CN108176407B (en) * | 2017-12-13 | 2020-01-24 | 江苏大学 | Ce-In composite material photocatalyst and preparation method and application thereof |
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| CN110152609A (en) * | 2019-06-12 | 2019-08-23 | 常州大学 | A kind of high-efficient graphite alkenyl bismuth system nanocomposite and preparation method thereof |
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