CN-121976220-A - Preparation method of phosphorus-defect bimetallic oxygen evolution catalyst

CN121976220ACN 121976220 ACN121976220 ACN 121976220ACN-121976220-A

Abstract

The invention relates to a preparation method of a phosphorus defect bimetallic oxygen evolution catalyst, which comprises the following steps of S1, dissolving 2.4mmol of nickel chloride hexahydrate, 0.8mmol of vanadium chloride and 300mg of urea in 80 ml deionized water, uniformly stirring for 10min, putting a product in S2:S1 and foam nickel together into a 100ml reaction kettle to react for 12h at 120 ℃, putting the reaction product into a drying box to dry, S3, putting the product S2 and 0.8g of sodium dihydrogen phosphate into a tubular furnace, heating to 350 ℃ at a heating rate of 3 ℃ per min under argon atmosphere, reacting for 3h to obtain nickel vanadium phosphide supported foam nickel, and S4, putting the product S3 into sodium borohydride solution to soak for 30min, taking out and drying to obtain a final product, namely the nickel vanadium phosphide supported foam nickel with vacancy defects.

Inventors

TIAN LEI
ZHANG JITANG
ZHANG LE
SHEN SHIJIE
WANG JIACHENG
ZHANG LILI
SHI XINXING

Assignees

台州学院

Dates

Publication Date: 20260505
Application Date: 20260114

Claims (8)

1. The preparation method of the phosphorus-defect bimetallic oxygen evolution catalyst is characterized by comprising the following steps of: S1, dissolving 2.4mmol of nickel chloride hexahydrate, 0.8mmol of vanadium chloride and 300mg of urea in 80 ml deionized water, and uniformly stirring for 10 min; s2, placing the product in S1 and foam nickel together into a 100ml reaction kettle to react for 12 hours at 120 ℃, and drying in a drying oven after the reaction; S3, putting the S2 product and 0.8g of sodium dihydrogen phosphate into a tube furnace, heating to 350 ℃ at a heating rate of 3 ℃ per minute under argon atmosphere, and reacting for 3 hours to obtain nickel vanadium phosphide loaded foam nickel; S4, soaking the S3 product in sodium borohydride solution for 30min, taking out and drying to obtain a final product, namely nickel vanadium phosphide supported foam nickel with vacancy defects; The tubular furnace comprises a furnace seat, a furnace cover, a first furnace tube, a second furnace tube, a third furnace tube, a drawing mechanism and a locking mechanism, wherein the furnace cover is rotatably arranged on the furnace seat, the first furnace tube is detachably arranged on the furnace seat, the second furnace tube is slidably arranged on the first furnace tube, the drawing mechanism is arranged on the first furnace tube, the second furnace tube and the third furnace tube, the locking mechanism is arranged on the furnace seat, the furnace cover, the second furnace tube and the third furnace tube, the drawing mechanism comprises a first drawing assembly and a second drawing assembly, and the locking mechanism comprises a first locking assembly and a second locking assembly.
2. The method for preparing the phosphorus defect bimetallic oxygen evolution catalyst according to claim 1, wherein the first drawing component comprises a first sliding groove, a first stop block, a first through groove, a second through groove, a first placement seat, a first baffle, a first sealing ring and a second sealing ring, wherein the first sliding groove is fixedly arranged on a second furnace tube, the first stop block is fixedly arranged on the furnace seat and is jointed with the first sliding groove, the first through groove is fixedly arranged on the second furnace tube, the second through groove is fixedly arranged on the second furnace tube, the first placement seat is fixedly arranged on the second furnace tube, the first baffle is fixedly arranged on the second furnace tube, the first sealing ring is fixedly arranged on the first furnace tube, and the second sealing ring is fixedly arranged on the second furnace tube and is jointed with the first sealing ring.
3. The preparation method of the phosphorus defect bimetallic oxygen evolution catalyst according to claim 1, wherein the first locking assembly comprises a plurality of second sliding grooves, a plurality of third sliding grooves, a plurality of fourth sliding grooves, a first locking cover, a plurality of first locking heads, first through holes and a first sealing device, wherein the second sliding grooves are fixedly arranged on a furnace seat and a furnace cover at equal intervals, the third sliding grooves are fixedly arranged on the furnace seat and the furnace cover at equal intervals and are communicated with the second sliding grooves, the fourth sliding grooves are fixedly arranged on the furnace seat and the furnace cover at equal intervals and are communicated with the third sliding grooves, the first locking cover is detachably arranged on a second furnace tube, the first locking heads are fixedly arranged on the first locking cover at equal intervals, the first locking heads can slide along the second sliding grooves, the third sliding grooves and the fourth sliding grooves, the first through holes are fixedly arranged on the first locking cover and are sleeved on the second furnace seat and the furnace cover, and the first sealing device is arranged on the first locking cover, the furnace seat and the furnace cover.
4. The preparation method of the phosphorus defect bimetallic oxygen evolution catalyst according to claim 3 is characterized in that the first sealing device comprises a third sealing ring, a fourth sealing ring, a fifth sealing ring, a sixth sealing ring and a seventh sealing ring, wherein the third sealing ring is fixedly arranged on the first locking cover, the fourth sealing ring is fixedly arranged on the second furnace tube and is attached to the third sealing ring, the fifth sealing ring is fixedly arranged on the furnace cover, the sixth sealing ring is fixedly arranged on the furnace seat, and the seventh sealing ring is fixedly arranged on the first locking cover and is attached to the fifth sealing ring and the sixth sealing ring.
5. The method for preparing a phosphorus-deficient bimetallic oxygen evolution catalyst as set forth in claim 2, wherein the second drawing assembly and the first drawing assembly are identical in structure and symmetrically disposed at two ends of the first furnace tube.
6. The method for preparing a phosphorus-deficient bimetallic oxygen evolution catalyst as set forth in claim 4, wherein the second locking assembly is configured identically and symmetrically to the first locking assembly.
7. The method for preparing a phosphorus-deficient bimetallic oxygen evolution catalyst as set forth in claim 3, wherein the first locking cap is provided with a polygonal handle.
8. The method for preparing a phosphorus-deficient bimetallic oxygen evolution catalyst according to claim 1, wherein the concentration of the sodium borohydride solution is any one of 0mol/L,0.05mol/L,0.1mol/L,0.2mol/L,0.5mol/L and 1mol/L.

Description

Preparation method of phosphorus-defect bimetallic oxygen evolution catalyst Technical Field The invention relates to the technical field of oxygen evolution catalysts, in particular to a preparation method of a phosphorus defect bimetallic oxygen evolution catalyst. Background The oxygen evolution catalyst is a material capable of obviously reducing the overpotential of the oxygen evolution reaction, improving the reaction rate and enhancing the reaction stability, and is widely applied to the fields of water electrolysis hydrogen production, renewable fuel cells, photoelectrochemical water decomposition tanks and the like. The existing oxygen evolution catalyst mainly comprises a noble metal-based catalyst, such as a catalyst with iridium oxide and ruthenium oxide as base materials, but the catalyst is expensive, has less metal reserves and is unfavorable for large-scale industrial application, and the transition metal-based catalyst has the advantages of low cost and huge reserves as an alternative scheme, and is a common bimetallic phosphide catalyst, but the performance of the transition metal-based catalyst is still greatly different from that of the noble metal-based catalyst, so that a phosphorus defect bimetallic oxygen evolution catalyst is needed to solve the problems. Disclosure of Invention The summary of the application is provided to introduce a selection of concepts in a simplified form that are further described below in the detailed description. The summary of the application is not intended to identify key features or essential features of the claimed subject matter, nor is it intended to be used to limit the scope of the claimed subject matter. In order to solve the technical problems mentioned in the background section above, some embodiments of the present application provide a method for preparing a phosphorus-deficient bimetallic oxygen evolution catalyst, comprising the steps of: S1, dissolving 2.4mmol of nickel chloride hexahydrate, 0.8mmol of vanadium chloride and 300mg of urea in 80 ml deionized water, and uniformly stirring for 10 min; s2, placing the product in S1 and foam nickel together into a 100ml reaction kettle to react for 12 hours at 120 ℃, and drying in a drying oven after the reaction; S3, putting the S2 product and 0.8g of sodium dihydrogen phosphate into a tube furnace, heating to 350 ℃ at a heating rate of 3 ℃ per minute under argon atmosphere, and reacting for 3 hours to obtain nickel vanadium phosphide loaded foam nickel; S4, soaking the S3 product in sodium borohydride solution for 30min, taking out and drying to obtain a final product, namely nickel vanadium phosphide supported foam nickel with vacancy defects; The tubular furnace comprises a furnace seat, a furnace cover, a first furnace tube, a second furnace tube, a third furnace tube, a drawing mechanism and a locking mechanism, wherein the furnace cover is rotatably arranged on the furnace seat, the first furnace tube is detachably arranged on the furnace seat, the second furnace tube is slidably arranged on the first furnace tube, the drawing mechanism is arranged on the first furnace tube, the second furnace tube and the third furnace tube, the locking mechanism is arranged on the furnace seat, the furnace cover, the second furnace tube and the third furnace tube, the drawing mechanism comprises a first drawing assembly and a second drawing assembly, and the locking mechanism comprises a first locking assembly and a second locking assembly. The first drawing component comprises a first sliding groove, a first stop block, a first through groove, a second through groove, a first placing seat, a first baffle, a first sealing ring and a second sealing ring, wherein the first sliding groove is fixedly arranged on the second furnace tube, the first stop block is fixedly arranged on the furnace seat and is attached to the first sliding groove, the first through groove is fixedly arranged on the second furnace tube, the second through groove is fixedly arranged on the second furnace tube, the first placing seat is fixedly arranged on the second furnace tube, the first baffle is fixedly arranged on the second furnace tube, the first sealing ring is fixedly arranged on the first furnace tube, and the second sealing ring is fixedly arranged on the second furnace tube and is attached to the first sealing ring. The first locking assembly comprises a plurality of second sliding grooves, a plurality of third sliding grooves, a plurality of fourth sliding grooves, a first locking cover, a plurality of first locking heads, first through holes and a first sealing device, wherein the second sliding grooves are fixedly arranged on the furnace seat and the furnace cover at equal intervals in a circumferential manner, the third sliding grooves are fixedly arranged on the furnace seat and the furnace cover at equal intervals in a circumferential manner and are communicated with the second sliding grooves, the fourth sliding gr