CN111841631B - Polypyrrole-cerium dioxide-gold composite nano material - Google Patents
Polypyrrole-cerium dioxide-gold composite nano material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 239000010931 gold Substances 0.000 title claims abstract description 28
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 28
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 22
- 229910052684 Cerium Inorganic materials 0.000 title claims abstract description 15
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002105 nanoparticle Substances 0.000 claims abstract description 17
- HEAMKOIGXQVULV-UHFFFAOYSA-N [O-2].[O-2].[Ce+3].[Au+3] Chemical compound [O-2].[O-2].[Ce+3].[Au+3] HEAMKOIGXQVULV-UHFFFAOYSA-N 0.000 claims abstract description 12
- ODKSFYDXXFIFQN-BYPYZUCNSA-N L-arginine Chemical compound OC(=O)[C@@H](N)CCCN=C(N)N ODKSFYDXXFIFQN-BYPYZUCNSA-N 0.000 claims abstract description 11
- 229930064664 L-arginine Natural products 0.000 claims abstract description 11
- 235000014852 L-arginine Nutrition 0.000 claims abstract description 11
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 34
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 12
- 239000012498 ultrapure water Substances 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 239000006228 supernatant Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000003638 chemical reducing agent Substances 0.000 claims description 4
- 238000001308 synthesis method Methods 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- FFEARJCKVFRZRR-UHFFFAOYSA-N L-Methionine Natural products CSCCC(N)C(O)=O FFEARJCKVFRZRR-UHFFFAOYSA-N 0.000 claims description 3
- FFEARJCKVFRZRR-BYPYZUCNSA-N L-methionine Chemical compound CSCC[C@H](N)C(O)=O FFEARJCKVFRZRR-BYPYZUCNSA-N 0.000 claims description 3
- 229930195722 L-methionine Natural products 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- 229960004452 methionine Drugs 0.000 claims description 3
- 239000012279 sodium borohydride Substances 0.000 claims description 3
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims description 3
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 abstract description 12
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 abstract description 12
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- 238000000034 method Methods 0.000 abstract description 3
- 229920000128 polypyrrole Polymers 0.000 abstract description 3
- 230000031700 light absorption Effects 0.000 abstract description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract 1
- 230000005611 electricity Effects 0.000 abstract 1
- 125000002795 guanidino group Chemical group C(N)(=N)N* 0.000 abstract 1
- 238000011065 in-situ storage Methods 0.000 abstract 1
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- ZBKIUFWVEIBQRT-UHFFFAOYSA-N gold(1+) Chemical compound [Au+] ZBKIUFWVEIBQRT-UHFFFAOYSA-N 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
- 229910001112 rose gold Inorganic materials 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution 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
- 230000002779 inactivation Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910001097 yellow gold Inorganic materials 0.000 description 1
- 239000010930 yellow gold Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/04—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing carboxylic acids or their salts
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
-
- 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
- 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
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a polypyrrole-cerium dioxide-gold composite nano material. Firstly, preparing gold nanoparticles, mixing a gold colloid solution with negative electricity with L-arginine and cerium nitrate, wherein guanidino and carboxyl of the L-arginine are respectively connected with gold and Ce3+The cerium dioxide-gold composite nano material is obtained under the heating condition, the catalytic capability of the cerium dioxide and the stability of the gold nano particles can be improved after the cerium dioxide-gold composite nano material and the cerium dioxide are mutually doped, and polypyrrole is modified on the surface of the cerium dioxide by utilizing an in-situ polymerization method, so that the conductivity of the material is increased, and the range of absorbing visible light is widened. The polypyrrole-cerium dioxide-gold composite nanomaterial disclosed by the invention is good in stability, simple in preparation method operation, wide in visible light absorption range, excellent in photocatalytic performance and good in application prospect.
Description
Technical Field
The invention relates to a polypyrrole-cerium dioxide-gold composite nano material, belonging to the field of preparation of composite nano materials.
Background
The photocatalytic oxidation-reduction reaction is used as a green and sustainable catalysis technology, has great potential in the aspects of solving environmental pollution and energy crisis, and the efficiency and stability of the photocatalyst are key factors influencing the photocatalytic performance. Cerium dioxide is an important n-type wide band gap semiconductor, and has been widely studied in the aspects of photocatalytic degradation of pollutants, decomposition of water to produce hydrogen, organic synthesis and the like due to the fact that cerium dioxide is used as a photocatalyst because of the advantages of abundant oxygen vacancies, high oxygen storage capacity, good chemical/photochemical stability and the like. However, the band gap energy of ceria is wide, and only the energy of ultraviolet light region can be utilized, which limits the development of ceria catalyst. At present, gold nanoparticles with plasma characteristics are compounded with wide-band-gap semiconductor cerium dioxide, so that charge transfer between crystal faces of core-shell nano crystals is facilitated, and the absorption of the visible light by the cerium dioxide is realized.
In addition, the gold nanoparticles are widely used as catalysts, easy agglomeration and inactivation are one of important factors restricting the development of the gold nanoparticles, and cerium dioxide can be used as a carrier of the gold nanoparticles to realize an ultra-small gold heterostructure on a semiconductor material. The cerium dioxide-gold composite nano structure can improve the stability and the dispersity of the gold nano material, is beneficial to the separation of electron-hole pairs, and has synergistic effect between the two to improve the catalytic performance.
At present, polypyrrole has attracted wide attention in the field of photocatalysis, has the advantages of small band gap, good chemical stability, good conductivity, low price, environmental friendliness and the like, is beneficial to charge transfer and electron-hole pair separation, and has visible light photocatalytic activity based on an n-electron conjugated system. Therefore, the polypyrrole-cerium dioxide-gold composite nanomaterial is prepared by combining the comprehensive advantages of cerium dioxide, gold nanoparticles and polypyrrole, the photocatalytic efficiency of the composite material can be greatly improved, and the technical requirements of green and efficient production can be better met.
Disclosure of Invention
Aiming at the existing problems, the invention provides a polypyrrole-cerium dioxide-gold composite nano material, which specifically comprises the following steps:
(1) mixing the reducing agent solution with the chloroauric acid solution to obtain a gold colloid solution;
(2) adding 0.085 g of L-arginine into 10 mL of ultrapure water, and ultrasonically mixing uniformly to obtain an L-arginine solution;
(3) dissolving 0.0035 g of cerium nitrate in 20-40 mL of ethanol water solution with volume fraction of 50%, adding 1-5 mL of prepared gold colloid solution, and dropwise adding 10 mL of prepared L-arginine solution at room temperature; heating the mixed solution at 80 ℃ under the action of magnetic stirring for 2-4 hours for reaction, centrifuging for 15 minutes at the rotating speed of 12000 r/min, removing supernatant, and washing with acetone for several times to obtain cerium dioxide-gold composite nanoparticles;
(4) weighing 500 mg of prepared cerium dioxide-gold composite nano particles, dispersing the cerium dioxide-gold composite nano particles in 10 mL of ultrapure water, quickly adding 50 mu L of pyrrole, magnetically stirring for 30 minutes, dropwise adding 10 mL of 10 mg/mL ferric chloride solution into the mixed solution, continuously stirring for 12 hours, continuously standing at room temperature for 8 hours, centrifuging for 15 minutes at the rotation speed of 10000 r/min, removing supernatant, washing with ethanol and the ultrapure water for several times, and drying in an oven at 60 ℃ for 24 hours to obtain the polypyrrole-cerium dioxide-gold composite nano material.
The reducing agent used for preparing the gold colloid solution is sodium citrate, sodium borohydride or L-methionine.
The invention has the beneficial effects that:
1. the particle size of the polypyrrole-cerium dioxide-gold composite nano material is about 50 nm, the specific surface area is large, more catalytic active sites can be exposed, and the photocatalytic activity is improved.
2. The polypyrrole-cerium dioxide-gold composite nanomaterial combines the excellent catalytic performance of three materials, has large specific surface area, good conductivity and wide visible light absorption range, effectively enhances the photocatalytic performance of the polypyrrole-cerium dioxide-gold composite nanomaterial, and greatly improves the stability of gold nanoparticles and cerium dioxide.
3. The polypyrrole-cerium dioxide-gold composite nanomaterial disclosed by the invention has the advantages of simple synthesis method, environmental friendliness, good repeatability, good stability, high catalytic efficiency, large-scale production value and excellent application potential in the field of photocatalysis.
Drawings
FIG. 1 is a scanning electron microscope image of the prepared polypyrrole-ceria-gold composite nanomaterial.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
Example 1
(1) Heating 80 mL of ultrapure water to 90 ℃, adding 0.8 mL of chloroauric acid solution with the mass fraction of 1%, continuing to heat to 96 ℃ for 1 minute, finally adding 2.8 mL of sodium citrate with the mass fraction of 1%, and heating for 15 minutes to obtain a wine red gold colloidal solution;
(2) adding 0.085 g of L-arginine into 10 mL of ultrapure water, and ultrasonically mixing uniformly to obtain an L-arginine solution;
(3) dissolving 0.0035 g of cerium nitrate in 20-40 mL of ethanol water with volume fraction of 50%, adding 1-5 mL of prepared gold colloid solution, and dropwise adding 10 mL of L-arginine solution at room temperature; heating the mixed solution at 80 ℃ under the action of magnetic stirring for 2-4 hours for reaction, centrifuging for 15 minutes at the rotating speed of 12000 r/min, removing supernatant, and washing with acetone for several times to obtain cerium dioxide-gold composite nanoparticles;
(4) weighing 500 mg of prepared cerium dioxide-gold composite nano particles, dispersing the cerium dioxide-gold composite nano particles in 10 mL of ultrapure water, quickly adding 50 mu L of pyrrole, magnetically stirring for 30 minutes, dropwise adding 10 mL of 10 mg/mL ferric chloride solution into the mixed solution, continuously stirring for 12 hours, continuously standing at room temperature for 8 hours, centrifuging for 15 minutes at the rotation speed of 10000 r/min, removing supernatant, washing with ethanol and the ultrapure water for several times, and drying in an oven at 60 ℃ for 24 hours to obtain the polypyrrole-cerium dioxide-gold composite nano material.
Example 2
The preparation procedure is the same as in example 1, except that: the synthesis method of the gold colloid solution in the step (1) comprises the following steps: adding 0.5 mL of chloroauric acid solution with the mass fraction of 1% into 25-45 mL of ultrapure water, reacting for 5 minutes under the action of magnetic stirring, slowly adding 0.8 mL of sodium borohydride solution with the mass fraction of 1%, and continuously stirring the mixed solution for 1 hour in the dark at room temperature to obtain a wine-red gold colloidal solution.
Example 3
The preparation procedure is the same as in example 1, except that: the synthesis method of the gold colloid solution in the step (1) comprises the following steps: adding 0.0060 g of L-methionine, 0.8 mL of chloroauric acid solution with the mass fraction of 1% and 0.6 mL of 0.5M sodium hydroxide solution into 3.6 mL of ultrapure water, carrying out magnetic stirring reaction for 6 hours at 37 ℃, then adding 0.5 mL of 1M sulfuric acid solution, centrifuging at the rotating speed of 6000 rpm for 2 minutes to remove supernatant, washing with 0.1M sulfuric acid solution for several times, adding 5 mL of ammonia water with the mass fraction of 1.4% into the precipitate, carrying out magnetic stirring reaction for 30 minutes at 70 ℃ to obtain yellow gold colloid solution, and storing for later use at 4 ℃ in the dark.
Claims (2)
1. A polypyrrole-cerium dioxide-gold composite nano material is characterized by comprising the following preparation steps:
(1) mixing the reducing agent solution with the chloroauric acid solution to obtain a gold colloid solution;
(2) adding 0.085 g of L-arginine into 10 mL of ultrapure water, and ultrasonically mixing uniformly to obtain an L-arginine solution;
(3) dissolving 0.0035 g of cerium nitrate in 20-40 mL of ethanol water solution with volume fraction of 50%, adding 1-5 mL of prepared gold colloid solution, and dropwise adding 10 mL of prepared L-arginine solution at room temperature; heating the mixed solution at 80 ℃ under the action of magnetic stirring for 2-4 hours for reaction, centrifuging for 15 minutes at the rotating speed of 12000 r/min, removing supernatant, and washing with acetone for several times to obtain cerium dioxide-gold composite nanoparticles;
(4) weighing 500 mg of prepared cerium dioxide-gold composite nano particles, dispersing the cerium dioxide-gold composite nano particles in 10 mL of ultrapure water, quickly adding 50 mu L of pyrrole, magnetically stirring for 30 minutes, dropwise adding 10 mL of 10 mg/mL ferric chloride solution into the mixed solution, continuously stirring for 12 hours, continuously standing at room temperature for 8 hours, centrifuging for 15 minutes at the rotation speed of 10000 r/min, removing supernatant, washing with ethanol and the ultrapure water for several times, and drying in an oven at 60 ℃ for 24 hours to obtain the polypyrrole-cerium dioxide-gold composite nano material.
2. The polypyrrole-ceria-gold composite nanomaterial according to claim 1, wherein the reducing agent used in the synthesis method of the gold colloid solution in the step (1) is sodium citrate, sodium borohydride or L-methionine.
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