CN110681386B - Preparation method of FeOOH coated praseodymium cuprate nano catalytic powder - Google Patents
Preparation method of FeOOH coated praseodymium cuprate nano catalytic powder Download PDFInfo
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- CN110681386B CN110681386B CN201911010285.6A CN201911010285A CN110681386B CN 110681386 B CN110681386 B CN 110681386B CN 201911010285 A CN201911010285 A CN 201911010285A CN 110681386 B CN110681386 B CN 110681386B
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- 239000000843 powder Substances 0.000 title claims abstract description 58
- 229910052777 Praseodymium Inorganic materials 0.000 title claims abstract description 42
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910002588 FeOOH Inorganic materials 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 230000003197 catalytic effect Effects 0.000 title claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000001301 oxygen Substances 0.000 claims abstract description 16
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000001257 hydrogen Substances 0.000 claims abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 13
- FDZZZRQASAIRJF-UHFFFAOYSA-M malachite green Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](C)C)C=C1 FDZZZRQASAIRJF-UHFFFAOYSA-M 0.000 claims abstract description 12
- 229940107698 malachite green Drugs 0.000 claims abstract description 12
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 6
- 230000007062 hydrolysis Effects 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 71
- 238000003756 stirring Methods 0.000 claims description 35
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 33
- 239000008367 deionised water Substances 0.000 claims description 22
- 229910021641 deionized water Inorganic materials 0.000 claims description 22
- 150000003839 salts Chemical class 0.000 claims description 22
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical group CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- WJJMNDUMQPNECX-UHFFFAOYSA-N dipicolinic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=N1 WJJMNDUMQPNECX-UHFFFAOYSA-N 0.000 claims description 18
- 239000010949 copper Substances 0.000 claims description 17
- 239000003513 alkali Substances 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 11
- 239000011858 nanopowder Substances 0.000 claims description 11
- YWECOPREQNXXBZ-UHFFFAOYSA-N praseodymium(3+);trinitrate Chemical compound [Pr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YWECOPREQNXXBZ-UHFFFAOYSA-N 0.000 claims description 11
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 239000013078 crystal Substances 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- 229910052802 copper Inorganic materials 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000005469 granulation Methods 0.000 claims description 7
- 230000003179 granulation Effects 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000010298 pulverizing process Methods 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 239000007921 spray Substances 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 238000012546 transfer Methods 0.000 claims description 6
- WYOIGGSUICKDNZ-UHFFFAOYSA-N 2,3,5,6,7,8-hexahydropyrrolizin-1-one Chemical compound C1CCC2C(=O)CCN21 WYOIGGSUICKDNZ-UHFFFAOYSA-N 0.000 claims description 5
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 5
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 5
- LHBNLZDGIPPZLL-UHFFFAOYSA-K praseodymium(iii) chloride Chemical group Cl[Pr](Cl)Cl LHBNLZDGIPPZLL-UHFFFAOYSA-K 0.000 claims description 5
- 150000001879 copper Chemical class 0.000 claims description 4
- 230000000593 degrading effect Effects 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 238000010907 mechanical stirring Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 13
- 238000006555 catalytic reaction Methods 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 3
- 229910021645 metal ion Inorganic materials 0.000 abstract description 2
- 239000010419 fine particle Substances 0.000 abstract 1
- 239000012535 impurity Substances 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000007769 metal material Substances 0.000 abstract 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- LVPMIMZXDYBCDF-UHFFFAOYSA-N isocinchomeronic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)N=C1 LVPMIMZXDYBCDF-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- GJAWHXHKYYXBSV-UHFFFAOYSA-N pyridinedicarboxylic acid Natural products OC(=O)C1=CC=CN=C1C(O)=O GJAWHXHKYYXBSV-UHFFFAOYSA-N 0.000 description 2
- 241000446313 Lamella Species 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- MUYSADWCWFFZKR-UHFFFAOYSA-N cinchomeronic acid Chemical compound OC(=O)C1=CC=NC=C1C(O)=O MUYSADWCWFFZKR-UHFFFAOYSA-N 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 208000013409 limited attention Diseases 0.000 description 1
- 239000010814 metallic waste Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000007709 nanocrystallization Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- -1 praseodymium ions Chemical class 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
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Abstract
The invention belongs to the technical field of electrocatalysis materials, and discloses a preparation method for FeOOH coated praseodymium cuprate nano catalysis powder by a coordination method. The preparation method adopts a coordination method to prepare the nanometer electro-catalysis powder, and the FeOOH coated praseodymium cuprate nanometer electro-catalysis powder prepared by the method has high purity, small and uniform granularity and large specific surface area, can be used for photocatalytic degradation of malachite green in a water body, and has potential application space in aspects of electro-catalysis hydrolysis hydrogen production and oxygen production. The preparation method provided by the invention is simple and easy to operate, has low cost and fine particles, does not introduce impurities or cause metal material loss, can ensure the stoichiometric ratio of metal ions in precipitates by a coordination method, and can be popularized and applied to industrial production.
Description
Technical Field
The invention belongs to the technical field of electrocatalytic materials, particularly relates to the technical field of electrocatalytic full-hydrolysis, and discloses a preparation method of FeOOH coated praseodymium cuprate nano catalytic powder.
As energy consumption and environmental problems are increased due to the use of a large amount of fossil fuels, it is urgent to find some effective methods for utilizing and converting clean energy such as solar energy and electric power. Among them, the decomposition of water into hydrogen and oxygen by electricity is one of the most important methods to solve the future shortage of chemical fuels and to reduce environmental pollution associated with fossil fuel consumption. Water splitting consists of two half-reactions, namely the Hydrogen Evolution Reaction (HER) and the Oxygen Evolution Reaction (OER). The anode OER has a slow reaction speed due to its complicated four-electron transfer, which seriously hinders the overall conversion efficiency of water decomposition. Therefore, high overpotential of OER is one of the biggest problems to be solved in this field as far as now.
The rare earth element has a special electronic structure, so that the substance added with the rare earth element has special chemical and physical properties, such as catalysis assisting property, and the catalysis assisting property of the rare earth element is widely applied, has a great application prospect, has important application in chemical industries such as petrochemical industry and the like, and can make great contribution to the development of environment and the aspect of clean energy. Among transition metals, iron, which is one of the most abundant metals on earth, has received limited attention as a catalyst for OER. Due to its adjustable d-orbital and various chemical structures, it is a viable alternative to OER catalysts.
The FeOOH coated praseodymium cuprate nano catalytic powder is prepared by a coordination method. The metal cation is reacted with organic solvent to combine the metal ion and the ligand in the form of coordinate bond, so as to form the coordination ion with certain composition or space configuration.
At present, the existing preparation method of praseodymium cuprate is not satisfactory, and the problems of complex preparation process, difficult popularization, poor performance of the obtained product and the like exist. The preparation method provided by the invention can solve the problems, and FeOOH nano powder is coated on Pr prepared by a coordination method simultaneously2CuO4On the nano powder, the prepared powder has high purity, uniform granularity, good controllability and excellent performance. In addition, the nano powder prepared by the method can be used for degrading the pollutant malachite green in the water body, and also has potential application space in the aspects of hydrogen production and oxygen production through electrocatalysis hydrolysis.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method and application of FeOOH coated praseodymium cuprate nano catalytic powder. The powder prepared by the method has the advantages of high powder purity, uniform granularity, good controllability and excellent performance, and the prepared praseodymium cuprate nano powder can be used for degrading malachite green and can also be used as a catalyst for producing oxygen by electrolyzing water to produce hydrogen.
A preparation method of FeOOH coated praseodymium cuprate nano catalytic powder comprises the following steps:
(1) dissolving a certain amount of soluble salt of iron in deionized water, stirring uniformly, adding a certain amount of hydrochloric acid, adjusting the pH value of the solution to 4-6, putting the solution into a stainless steel hydrothermal kettle, and heating for 2-3h at 120 ℃ to obtain a solution A;
(2) according to Pr2CuO4Weighing soluble salt of Cu and soluble salt of Pr according to the stoichiometric ratio of Cu to Pr, dissolving the soluble salts of Cu and Pr in deionized water, and uniformly mixing to obtain a solution B;
(3) adding a certain amount of acetonitrile and a certain amount of 3-4 dipicolinic acid into the solution B, heating the solution at 60-90 ℃, stirring for 2-3h, adding 5-10mL of 1mol/L alkali liquor by using a liquid transfer gun, and stirring until the alkali liquor is dissolved to prepare a solution C;
(4) putting the solution C into an oven, reacting for 3-6 hours at a constant temperature of 120-150 ℃, and cooling to room temperature in the air; after the solution system is stable, filtering the obtained mixed solution, washing the obtained solid with water for 2-4 times to obtain flaky crystals, putting the obtained crystals into liquid nitrogen for pulverization, and taking out the obtained powder D;
(5) and adding the powder D into the solution A, uniformly stirring for 20-30min, performing spray granulation by using a sprayer, and drying for 1-2h in an oven at the temperature of 60-90 ℃ to prepare the nano powder required by the application.
The soluble salt of iron in the step (1) can be ferric chloride, ferric nitrate or ferric acetate.
In the step (1), the dosage of the soluble salt of iron is 1-2 times of the total molar amount of the soluble salt of copper and the soluble salt of praseodymium, and the volume dosage of the deionized water is 4-6 times of the total molar amount of the soluble salt of copper and the soluble salt of praseodymium.
The stirring conditions in the steps (1), (3) and (5) are mechanical stirring or magnetic stirring, and the rotation number of a rotor is 500-1000 r/min.
The soluble salt of copper in the step (2) can be copper chloride, copper nitrate, copper acetate and the like, and the soluble salt of praseodymium can be praseodymium chloride, praseodymium nitrate or praseodymium acetate.
In the step (3), the using amount of the acetonitrile is 3-4 times of the molar amount of the copper salt, and the using amount of the 3-4 dipicolinic acid is 1-2 times of the molar amount of the copper salt.
In the step (3), the solute of the alkali liquor is triethylamine, and the solvent is ethanol.
The FeOOH coated praseodymium cuprate nano catalytic powder can be used for degrading malachite green in a water body, and can also be used for producing hydrogen and oxygen through electrocatalytic hydrolysis.
Compared with the prior art, the method has the advantages that:
the invention adopts a coordination synthesis method, has simple preparation process and good metal atom matching property, does not cause metal waste, pollutes the environment and saves the cost;
(2) in the original simple solution preparation process, acetonitrile and 3.4 pyridine dicarboxylic acid are added, so that copper ions and praseodymium ions are effectively dispersed; the preparation method has the advantages that the pulverization is carried out in liquid nitrogen, so that the prepared powder is finer and is beneficial to nanocrystallization, and particularly, the 3.4 dipicolinic acid and copper ions are effectively coordinated, so that copper and praseodymium can be fully dissolved in an acetonitrile solution, and the experimental effect required by the application can be hardly achieved by using other dispersing agents.
(3) The powder prepared by the method has high purity, uniform granularity, good controllability and excellent performance, and related reports of the powder on the catalysis of the electrolyzed water are not found at present. Opens up potential application space in the aspects of hydrogen production and oxygen production by electrocatalysis hydrolysis, and develops new performance.
Drawings
FIG. 1 is a scanning electron microscope image of FeOOH coated praseodymium cuprate nano catalytic powder prepared in example 1 of the present invention;
FIG. 2 is a graph showing degradation of FeOOH-coated praseodymium cuprate nano catalytic powder prepared in example 2 of the present invention on malachite green;
FIG. 3 is a hydrogen evolution curve of FeOOH coated praseodymium cuprate nano catalytic powder prepared in example 3 of the present invention.
FIG. 4 is an oxygen evolution curve of FeOOH coated praseodymium cuprate nano catalytic powder prepared in example 3 of the present invention.
FIG. 5 is a scanning electron microscope image of FeOOH coated praseodymium cuprate nano catalytic powder prepared in comparative example 1 of the present invention;
FIG. 6 is an oxygen evolution curve of FeOOH coated praseodymium cuprate nano catalytic powder prepared in comparative example 1 and comparative example 2 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings, but the scope of the present invention is not limited by the embodiments.
Example 1
(1) Dissolving 3mmol of ferric chloride in 18mmol of deionized water, magnetically stirring for 10min at 500r/min, adding a certain amount of hydrochloric acid, adjusting the pH value of the solution to 4, and heating the solution in a stainless steel hydrothermal kettle at 120 ℃ for 2h to obtain a solution A;
(2) weighing 1mmol of copper chloride and 2mmol of praseodymium chloride according to the stoichiometric ratio of Cu to Pr in Pr2CuO4, dissolving the copper chloride and the praseodymium chloride in deionized water, wherein the volume usage of the deionized water is 6 times of the total molar mass of the copper chloride and the praseodymium chloride, and uniformly mixing to obtain a solution B;
(3) adding 3mmol acetonitrile into the solution B, adding 2mmol 3-4 dipicolinic acid, heating at 60 ℃, magnetically stirring for 2h at 500r/min, adding 5ml of 1mol/L alkali liquor (the solute is triethylamine and the solvent is ethanol) by using a liquid-transferring gun, and stirring for 20min until the alkali liquor is dissolved to prepare a solution C.
(4) Putting the solution C into an oven, reacting for 3 hours at a constant temperature of 120 ℃, and cooling to room temperature in the air; and after the solution system is stable, filtering the obtained mixed solution, washing the obtained solid for 2 times by using water, putting the obtained crystal into liquid nitrogen for pulverization, and taking out the powder D.
(5) And adding the powder D into the solution A, uniformly stirring, magnetically stirring for 20min at 500r/min, performing spray granulation by using a sprayer, and drying for 2h in an oven at the temperature of 60 ℃ to prepare the nano powder required by the application.
Fig. 1 is a scanning electron microscope image of FeOOH coated praseodymium cuprate nano catalytic powder prepared in embodiment 1 of the present invention, and it can be seen from fig. 1 that the prepared powder has uniform small layers with a dimension of 50nm, uniform lamella, good dispersibility, large specific surface area, and is beneficial for catalytic reaction.
Example 2
(1) Dissolving 6mmol of ferric nitrate in 18mmol of deionized water, magnetically stirring for 20min at 700r/min, adding a certain amount of hydrochloric acid, adjusting the pH value of the solution to 6, and heating the solution in a stainless steel hydrothermal kettle at 120 ℃ for 2h to obtain a solution A;
(2) weighing 1mmol of copper nitrate and 2mmol of praseodymium nitrate according to the stoichiometric ratio of Cu to Pr in Pr2CuO4, dissolving the copper nitrate and the praseodymium nitrate in deionized water, wherein the volume usage of the deionized water is 6 times of the total molar mass of the copper nitrate and the praseodymium nitrate, and uniformly mixing to obtain a solution B;
(3) adding 3mmol acetonitrile and 1mmol 3-4 dipicolinic acid into the solution B, heating at 60 ℃, magnetically stirring for 2h at 700r/min, adding 5ml of 1mol/L alkali liquor (the solute is triethylamine and the solvent is ethanol) by using a liquid transfer gun, and stirring until the alkali liquor is dissolved to prepare a solution C.
(4) Putting the solution C into an oven, reacting for 3 hours at a constant temperature of 120 ℃, and cooling to room temperature in the air; and after the solution system is stable, filtering the obtained mixed solution, washing the obtained solid for 2 times by using water, putting the obtained crystal into liquid nitrogen for pulverization, and taking out the powder D.
(5) And adding the powder D into the solution A, uniformly stirring, magnetically stirring for 20min at 700r/min, performing spray granulation by using a sprayer, and drying for 2h in an oven at the temperature of 60 ℃ to prepare the nano powder required by the application.
Weighing 0.1g of malachite green, preparing a 1g/L malachite green solution, adding water, putting 0.2g of the powder prepared in the example 2 into a reaction bottle for a photocatalysis experiment, measuring the photocatalysis effect of the malachite green after reacting for different time,
fig. 2 is a graph showing the degradation efficiency of the FeOOH-coated praseodymium cuprate nano catalytic powder prepared in example 2 on the malachite green, and it can be seen from fig. 2 that the degradation efficiency on the malachite green after 180min is 90%, and it can be seen that the FeOOH-coated praseodymium cuprate nano catalytic powder prepared in the present application has a good photocatalytic effect on the malachite green.
Example 3
(1) Dissolving 3mmol of ferric nitrate in 12mmol of deionized water, magnetically stirring for 10min at 800r/min, adding a certain amount of hydrochloric acid, adjusting the pH value of the solution to 5, and heating the solution in a stainless steel hydrothermal kettle at 120 ℃ for 2h to obtain a solution A;
(2) weighing 1mmol of copper nitrate and 2mmol of praseodymium nitrate according to the stoichiometric ratio of Cu to Pr in Pr2CuO4, dissolving the copper nitrate and the praseodymium nitrate in deionized water, wherein the volume usage of the deionized water is 6 times of the total molar mass of the copper nitrate and the praseodymium nitrate, and uniformly mixing to obtain a solution B;
(3) adding 3mmol acetonitrile and 1mmol 3-4 dipicolinic acid into the solution B, heating at 60 ℃, magnetically stirring for 2h at 700r/min, adding 5ml of 1mol/L alkali liquor (the solute is triethylamine and the solvent is ethanol) by using a liquid transfer gun, and stirring until the alkali liquor is dissolved to prepare a solution C.
(4) Putting the solution C into an oven, reacting for 3 hours at a constant temperature of 120 ℃, and cooling to room temperature in the air; and after the solution system is stable, filtering the obtained mixed solution, washing the obtained solid for 2 times by using water, putting the obtained crystal into liquid nitrogen for pulverization, and taking out the powder D.
(5) And adding the powder D into the solution A, uniformly stirring, magnetically stirring for 20min at 700r/min, performing spray granulation by using a sprayer, and drying for 2h in an oven at the temperature of 60 ℃ to prepare the nano powder required by the application.
The electro-catalysis hydrogen evolution and oxygen evolution performance of FeOOH coated praseodymium cuprate nano catalytic powder is tested by adopting a three-electrode system, a Pt sheet is taken as a counter electrode, a Saturated Calomel Electrode (SCE) is taken as a reference electrode, and a working electrode is an ITO electrode of which the surface is dropwise coated with a cuprate rare earth electro-catalysis material; the testing instrument is a PARSTAT 2273 electrochemical workstation; the test solution was 1mol/L KOH.
The working electrode is prepared by adopting a dripping coating method, and the specific process is as follows: weighing 0.04g of FeOOH coated praseodymium cuprate nano catalytic powder, placing the powder into a small glass bottle, adding 500ml of ethanol, 500ml of deionized water and 30 mul of DuPont solution with the mass fraction of 5%, and carrying out ultrasonic treatment on the mixture for more than 20min to form a catalyst solution. When the ITO is used as an electrode, the ITO is required to be washed by sequentially using acetone, ethanol and deionized water, then 20 mu l of the catalyst solution is coated on the ITO conductive surface, and the ITO conductive surface is dried in a drying oven for 1h at 60 ℃ to be tested.
Testing parameters: the scan rate for the LSV test was 5 mV/s.
Fig. 3 is a hydrogen evolution curve of the FeOOH coated praseodymium cuprate nano catalytic powder prepared in embodiment 3 of the present invention, and fig. 4 is an oxygen evolution curve of the FeOOH coated praseodymium cuprate nano catalytic powder prepared in embodiment 3 of the present invention, as shown in the figure: fig. 3 is a HER curve, the starting point of the curve curving downward represents the starting potential for hydrogen production by reduction, the smaller the better. The slope of the bend represents the reduction rate versus overpotential, with larger being better. Fig. 4 is an OER curve, and the starting point of the curve curving upward represents the starting potential for hydrogen production by oxidation, the smaller the better. The slope of the bend represents the reduction rate versus overpotential, with larger being better.
COMPARATIVE EXAMPLE 1 (not pulverized in liquid nitrogen)
(1) Dissolving 3mmol of ferric acetate in 12mmol of deionized water, magnetically stirring for 20min at 700r/min, adding a certain amount of hydrochloric acid, adjusting the pH value of the solution to 6, and heating the solution in a stainless steel hydrothermal kettle at 120 ℃ for 1h to obtain a solution A;
(2) weighing 1mmol of copper acetate and 2mmol of praseodymium acetate according to the stoichiometric ratio of Cu to Pr in Pr2CuO4, dissolving the copper acetate and the praseodymium acetate in deionized water, wherein the volume usage of the deionized water is 4 times of the total molar mass of the copper acetate and the praseodymium acetate, and uniformly mixing to obtain a solution B;
(3) adding 3mmol acetonitrile and 1mmol 3-4 dipicolinic acid into the solution B, heating at 60 ℃, magnetically stirring for 2h at 700r/min, adding 5ml of 1mol/L alkali liquor (the solute is triethylamine and the solvent is ethanol) by using a liquid transfer gun, and stirring until the alkali liquor is dissolved to prepare a solution C.
(4) Putting the solution C into an oven, reacting for 3 hours at a constant temperature of 120 ℃, and cooling to room temperature in the air; and after the solution system is stable, filtering the obtained mixed solution, and washing the obtained solid with water for 2 times to obtain a flaky crystal D.
(5) And adding the powder D into the solution A, uniformly stirring, magnetically stirring for 20min at 700r/min, performing spray granulation by using a sprayer, and drying for 2h in an oven at the temperature of 60 ℃ to prepare the nano powder required by the application.
Fig. 5 is a scanning electron microscope image of the FeOOH coated praseodymium cuprate nano catalytic powder prepared in comparative example 1 of the present invention, as shown in fig. 5, the powder is not pulverized in liquid nitrogen, the prepared powder has large particles, many powders are adhered together, the size is 5-10um, although the morphology is uniform, the specific surface area is small, and the photocatalytic reaction and the electrocatalytic reaction are not favorably performed.
Comparative example 2 (not pulverized in liquid nitrogen, without 3-4 pyridinedicarboxylic acid)
(1) Dissolving 3mmol of ferric nitrate in 12mmol of deionized water, magnetically stirring at 800r/min for 20min, adding a certain amount of hydrochloric acid, adjusting the pH value of the solution to 5, and heating the solution in a stainless steel hydrothermal kettle at 120 ℃ for 2h to obtain a solution A;
(2) weighing 1mmo of copper nitrate and 2mmol of praseodymium nitrate according to the stoichiometric ratio of Cu to Pr in Pr2CuO4, dissolving the copper nitrate and the praseodymium nitrate in deionized water, wherein the volume usage of the deionized water is 4 times of the total molar mass of the copper nitrate and the praseodymium nitrate, and uniformly mixing to obtain a solution B;
(3) adding 3mmol acetonitrile into the solution B, heating and stirring at 60 ℃ for 2h, adding 5ml of 1mol/L alkali liquor (the solute is triethylamine and the solvent is ethanol) by using a liquid-transferring gun, and magnetically stirring for 20min at 700r/min until dissolution to prepare a solution C.
(4) Putting the solution C into an oven, reacting for 3 hours at a constant temperature of 130 ℃, and cooling to room temperature in the air; and after the solution system is stable, filtering the obtained mixed solution, and washing the obtained solid with water for 3 times to obtain a flaky crystal D.
(5) And adding the powder D into the solution A, uniformly stirring, magnetically stirring for 20min at 700r/min, performing spray granulation by using a sprayer, and drying for 1.5h in an oven at the temperature of 80 ℃ to prepare the nano powder required by the application.
Fig. 6 is an oxygen evolution curve of FeOOH coated praseodymium cuprate nano catalytic powder prepared in comparative example 1 and comparative example 2 of the present invention, as shown in the figure: the slope of the bend represents the reduction rate versus overpotential, with larger being better. As can be seen from FIG. 6, the powders prepared in comparative examples 1 and 2 have poor oxygen evolution effect, especially the oxygen evolution curve of comparative example 2 has large particles, poor dispersion and poor oxygen evolution performance due to no pulverization in liquid nitrogen and no addition of 3-4 pyridinedicarboxylic acid.
Claims (7)
1. A preparation method of FeOOH coated praseodymium cuprate nano catalytic powder is characterized by comprising the following steps:
(1) dissolving a certain amount of soluble salt of iron in deionized water, stirring uniformly, adding a certain amount of hydrochloric acid, adjusting the pH value of the solution to 4-6, putting the solution into a stainless steel hydrothermal kettle, and heating for 2-3h at 120 ℃ to obtain a solution A; the dosage of the soluble salt of iron is 1-2 times of the total molar amount of the soluble salt of copper and the soluble salt of praseodymium;
(2) according to Pr2CuO4Weighing soluble salt of Cu and soluble salt of Pr according to the stoichiometric ratio of Cu to Pr, dissolving the soluble salts of Cu and Pr in deionized water, and uniformly mixing to obtain a solution B;
(3) adding a certain amount of acetonitrile and a certain amount of 3-4 dipicolinic acid into the solution B, heating the solution at 60-90 ℃, stirring for 2-3h, adding 5-10mL of 1mol/L alkali liquor by using a liquid transfer gun, and stirring until the alkali liquor is dissolved to prepare a solution C;
(4) putting the solution C into an oven, reacting for 3-6 hours at a constant temperature of 120-150 ℃, and cooling to room temperature in the air; after the solution system is stable, filtering the obtained mixed solution, washing the obtained solid with water for 2-4 times to obtain flaky crystals, putting the obtained crystals into liquid nitrogen for pulverization, and taking out the obtained powder D;
(5) adding the powder D into the solution A, uniformly stirring for 20-30min, performing spray granulation by using a sprayer, and drying for 1-2h in an oven at the temperature of 60-90 ℃ to prepare the required nano powder.
2. The preparation method of FeOOH coated praseodymium cuprate nano catalytic powder according to claim 1, characterized in that: the soluble salt of iron in the step (1) is ferric chloride, ferric nitrate or ferric acetate.
3. The preparation method of FeOOH coated praseodymium cuprate nano catalytic powder according to claim 1, characterized in that: the stirring conditions in the steps (1), (3) and (5) are mechanical stirring or magnetic stirring, and the rotating speed of a rotor is 500-1000 r/min.
4. The preparation method of FeOOH coated praseodymium cuprate nano catalytic powder according to claim 1, characterized in that: the soluble salt of copper in the step (2) is copper chloride, copper nitrate and copper acetate, and the soluble salt of praseodymium is praseodymium chloride, praseodymium nitrate or praseodymium acetate.
5. The preparation method of FeOOH coated praseodymium cuprate nano catalytic powder according to claim 1, characterized in that: in the step (3), the using amount of the acetonitrile is 3-4 times of the molar amount of the copper salt, and the using amount of the 3-4 dipicolinic acid is 1-2 times of the molar amount of the copper salt.
6. The preparation method of FeOOH coated praseodymium cuprate nano catalytic powder according to claim 1, characterized in that: in the step (3), the solute of the alkali liquor is triethylamine, and the solvent is ethanol.
7. The application of FeOOH coated praseodymium cuprate nano catalytic powder prepared by the preparation method according to claim 1 is characterized in that: the powder is not only used for degrading malachite green in a water body, but also used for producing hydrogen and oxygen by electrocatalysis hydrolysis.
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