S-NiV-LDH catalyst as well as preparation method and application thereof
By preparing a sulfur-doped nickel-vanadium layered bimetallic hydroxide catalyst supported on nickel foam, the problem of low efficiency in alcohol electro-oxidation reaction was solved, achieving a highly efficient conversion of 1,5-pentanediol to 1,5-pentanediic acid. This reduced the voltage requirement, produced products with high economic value, and the equipment was simple to operate and environmentally friendly.
Patent Information
- Application Number
- CN202510922320.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-04
- Publication Date
- 2025-11-18
AI Technical Summary
The low efficiency of existing catalysts for alcohol electro-oxidation (AOR) limits the application of renewable biomass-derived alcohols in electrosynthesis technology, especially in the process of electro-oxidation of 1,5-pentanediol to 1,5-pentanediic acid. There is a need to develop efficient, low-initial-potential and stable non-precious metal catalysts.
Using nickel foam as a support, a sulfur-doped nickel-vanadium layered bimetallic hydroxide (S-NiV-LDH) catalyst was prepared by hydrothermal method. The specific steps included washing the nickel foam, mixing nickel chloride hexahydrate, vanadium chloride, urea and thiourea and then carrying out a hydrothermal reaction to form the S-NiV-LDH catalyst, which was then applied to the electro-oxidation of 1,5-pentanediol in an electrochemical reaction cell.
This method achieves efficient conversion of 1,5-pentanediol to 1,5-pentanediic acid through electro-oxidation, reduces voltage requirements, produces products with high economic value, and features simple and easy-to-operate, environmentally friendly equipment.
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Figure CN120967415A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the technical field of electrochemistry, and particularly relates to an S-NiV-LDH catalyst, a preparation method and application thereof. BACKGROUND
[0002] In order to effectively respond to energy and environmental challenges, it is necessary to promote renewable energy-driven electrochemical conversion technology, especially electro-synthesis technology, which has the potential to convert abundant molecules into valuable chemicals and fuels. However, the widespread use of electro-synthesis is often hindered by slow oxygen evolution reaction (OER). In order to overcome this limitation, the prior art uses a more efficient alcohol electro-oxidation reaction (AOR) to produce high-value chemicals using renewable biomass-derived alcohols as an alternative to OER. Therefore, the development of an efficient AOR catalyst, combined with a cathode reduction reaction, is crucial for sustainable and environmentally friendly progress.
[0003] As a key monomer for synthesizing nylon 5,5, 1,5-pentanedioic acid, in combination with bio-based 1,5-pentanediamine, can produce high-performance polyamide materials, which are widely used in engineering plastics, textile fibers and other fields, meet the demand for automobile lightweight and environmentally friendly materials, significantly reduce the dependence on petroleum-based raw materials, and produce 1,5-pentanedioic acid by electro-oxidation of 1,5-pentanediol. This method reduces the voltage required for hydrogen production, and valuable chemicals are produced at the anode. Therefore, it has great value to develop and study a non-noble metal catalyst with low starting potential, high catalytic efficiency and good stability for application in the electro-oxidation reaction of 1,5-pentanediol. SUMMARY
[0004] The purpose of the embodiment of the application is to provide a preparation method of an S-NiV-LDH catalyst, which aims to solve the problems raised in the background.
[0005] The embodiment of the application is implemented in the following manner: a preparation method of an S-NiV-LDH catalyst, comprising the following steps:
[0006] The cut foam nickel is sequentially washed with nitric acid, ethanol and deionized water under ultrasonic and dried;
[0007] Nickel chloride hexahydrate, vanadium chloride, urea and thiourea are dissolved in deionized water and stirred, and then transferred to a polytetrafluoroethylene-lined hydrothermal reactor containing the treated foam nickel, to perform a hydrothermal reaction, and then cooled to room temperature, washed and vacuum dried to obtain the S-NiV-LDH catalyst.
[0008] Preferably, in the step of sequentially washing the cut foam nickel with nitric acid, ethanol and deionized water under ultrasonic and drying, the ultrasonic time is 5-15 minutes, and the concentration of nitric acid is 1-1.2 mol / L.
[0009] Preferably, in the step of stirring the nickel chloride hexahydrate, vanadium chloride, urea, and thiourea in deionized water, the molar ratio of the nickel chloride hexahydrate, vanadium chloride, urea, and thiourea is 0.6-1.5:0.6-1.5:3-6:0.375-1.5.
[0010] Preferably, the temperature of the hydrothermal reaction is 100-140 degrees Celsius, and the time is 10-14 hours.
[0011] Another object of the embodiments of the present application is to provide an S-NiV-LDH catalyst prepared by the above preparation method.
[0012] Another object of the embodiments of the present application is to provide an application of an S-NiV-LDH catalyst in the electrocatalytic oxidation of 1,5-pentanediol to 1,5-pentanedioic acid, comprising the following steps:
[0013] The S-NiV-LDH catalyst is placed in an electrochemical reaction cell, 1,5-pentanediol is used as a raw material, and 1,5-pentanedioic acid is generated on the surface of the working electrode under the catalysis of the S-NiV-LDH catalyst under the condition of power supply.
[0014] Preferably, the electrochemical reaction cell is an H-type electrolytic cell, a three-electrode system is used, the S-NiV-LDH catalyst is used as an anode electrocatalyst, a platinum sheet is used as a cathode electrocatalyst, mercury / mercury oxide is used as a reference electrode, the anode electrolyte in the H-type electrolytic cell is a mixed solution of potassium hydroxide and 1,5-pentanediol, the cathode electrolyte is potassium hydroxide, and the electro-oxidation reaction of 1,5-pentanediol is driven under the condition of power supply.
[0015] Preferably, the potential applied under the condition of power supply is 1.1-1.7 V relative to a reversible hydrogen electrode.
[0016] The S-NiV-LDH catalyst provided by the embodiments of the present application can be used for the electrocatalytic oxidation of 1,5-pentanediol to 1,5-pentanedioic acid, the equipment of the electrochemical production process is simple and easy to operate, is green, environmentally friendly, energy-saving, and the product generated by the reaction has a high economic value. BRIEF DESCRIPTION OF DRAWINGS
[0017] Figure 1 The XRD characterization graph of the S-NiV-LDH catalyst prepared in Embodiment 1 of the present application; 0.75 The XRD characterization graph of the S-NiV-LDH catalyst prepared in Embodiment 1 of the present application;
[0018] Figure 2 The cyclic voltammogram of the S-NiV-LDH catalyst prepared in Embodiment 1 of the present application in a mixed solution of potassium hydroxide and 1,5-pentanediol; 0.75 The cyclic voltammogram of the S-NiV-LDH catalyst prepared in Embodiment 1 of the present application in a mixed solution of potassium hydroxide and 1,5-pentanediol;
[0019] Figure 3Cyclic voltammogram of the sample prepared for the present application comparative example 1 in a mixed solution of potassium hydroxide and 1,5-pentanediol;
[0020] Figure 4 Double-layer capacitance value of the sample prepared for the present application example 1 and comparative example 1 in a mixed solution of potassium hydroxide and 1,5-pentanediol;
[0021] Figure 5 Comparison chart of LSV of the sample prepared for the present application example 1 and comparative example 1 in a mixed solution of potassium hydroxide and 1,5-pentanediol;
[0022] Figure 6 Comparison chart of LSV of the sample prepared for the present application examples 1-4 in a mixed solution of potassium hydroxide and 1,5-pentanediol. DETAILED DESCRIPTION
[0023] In order to make the objects, technical solutions and advantages of the present application clearer, the present application is further described in detail below in combination with the drawings and examples. It should be understood that the specific examples described herein are only used to explain the present application and do not limit the present application.
[0024] A foamed nickel loaded sulfur-doped nickel vanadium layered double hydroxide (S-NiV-LDH) electrocatalytic material, a preparation method thereof comprises the following steps:
[0025] S1, cut the foamed nickel into a size of 2*3 cm, and then sequentially ultrasonic in 1 mol / L nitric acid for 10 minutes, in ethanol for 10 minutes, and in deionized water for 10 minutes, so as to activate the foamed nickel;
[0026] S2, place the activated foamed nickel in a reaction kettle lined with polytetrafluoroethylene, and then dissolve 0.6-1.5 mmol of nickel chloride hexahydrate, 0.6-1.5 mmol of vanadium chloride, 3-6 mmol of urea, and 0.375-1.5 mmol of thiourea in 30 mL of deionized water, and then transfer the mixture to the polytetrafluoroethylene-lined hydrothermal reaction kettle after ultrasonic for 20 minutes, and then react at 120 degrees Celsius for 12 hours, and then cool the reaction kettle to room temperature after the reaction is completed, and then wash the foamed nickel in the reaction kettle with deionized water, and then vacuum dry at 60 degrees Celsius for 6 hours to obtain the S-NiV-LDH catalyst.
[0027] The prepared foam nickel supported sulfur doped nickel vanadium layered double hydroxide (S-NiV-LDH) catalyst is applied to the electrochemical oxidation of 1,5-pentanediol, specifically including the following steps: setting an H-type electrolytic cell as an electrochemical reaction cell, adopting a three-electrode system, taking the prepared S-NiV-LDH catalyst as a working electrode, a reference electrode being mercury / mercury oxide, and a counter electrode being a platinum sheet, an anode electrolyte being a mixed solution of 1 mol / L potassium hydroxide solution and 0.3 mol / L 1,5-pentanediol, and a cathode electrolyte being 1 mol / L potassium hydroxide, and the potential applied when power is supplied being 1.1-1.7 V relative to a reversible hydrogen electrode.
[0028] The specific implementation of the present application is described in detail below in combination with specific examples.
[0029] Example 1, a foam nickel supported sulfur doped nickel vanadium layered double hydroxide (S 0.75 -NiV-LDH) catalyst, and a preparation method thereof, specifically as follows:
[0030] The cut foam nickel is sequentially washed with 1 mol / L nitric acid, ethanol and deionized water under ultrasonic for 10 minutes, and then vacuum dried at 60 degrees Celsius; the raw materials are selected as 1.5 mmol of analytical grade nickel chloride hexahydrate, 0.6 mmol of vanadium chloride, 6 mmol of urea and 0.75 mmol of thiourea, dissolved in 30 mL of deionized water, and then transferred into a polytetrafluoroethylene lined hydrothermal reactor after ultrasonic for 20 minutes, and the treated foam nickel is placed in the reactor, and reacted at 120 degrees Celsius for 12 hours; after the reaction is completed, the reactor is cooled to room temperature, the foam nickel in the reactor is washed with deionized water, and then vacuum dried at 60 degrees Celsius for 6 hours to obtain the S 0.75 -NiV-LDH catalyst.
[0031] Example 2, a foam nickel supported sulfur doped nickel vanadium layered double hydroxide (S 0.375 -NiV-LDH) catalyst, and a preparation method thereof, specifically as follows:
[0032] The cut foam nickel is sequentially washed with 1 mol / L nitric acid, ethanol and deionized water under ultrasonic for 10 minutes, and then vacuum dried at 60 degrees Celsius; the raw materials are selected as 1.5 mmol of analytical grade nickel chloride hexahydrate, 0.6 mmol of vanadium chloride, 6 mmol of urea and 0.75 mmol of thiourea, dissolved in 30 mL of deionized water, and then transferred into a polytetrafluoroethylene lined hydrothermal reactor after ultrasonic for 20 minutes, and the treated foam nickel is placed in the reactor, and reacted at 120 degrees Celsius for 12 hours; after the reaction is completed, the reactor is cooled to room temperature, the foam nickel in the reactor is washed with deionized water, and then vacuum dried at 60 degrees Celsius for 6 hours to obtain the S 0.375 -NiV-LDH catalyst.
[0033] Example 3, a foam nickel supported sulfur doped nickel vanadium layered double hydroxide (S-NiV-LDH) catalyst, the preparation method is as follows: 1.125 -NiV-LDH) catalyst, the preparation method is as follows:
[0034] The cut foam nickel is sequentially washed with 1 mol / L nitric acid, ethanol, and deionized water under ultrasonic for 10 minutes, and then vacuum dried at 60 degrees Celsius. The raw materials are 1.5 mmol of analytical pure nickel chloride hexahydrate, 0.6 mmol of vanadium chloride, 6 mmol of urea, and 1.125 mmol of thiourea, which are dissolved in 30 mL of deionized water, and then transferred to a polytetrafluoroethylene lined autoclave after ultrasonic for 20 minutes. The treated foam nickel is placed in the autoclave and reacted at 120 degrees Celsius for 12 hours. After the reaction is completed, the autoclave is cooled to room temperature, and the foam nickel in the autoclave is washed with deionized water. Then, vacuum drying is performed at 60 degrees Celsius for 6 hours to obtain a S 1.125 -NiV-LDH catalyst.
[0035] Example 4, a foam nickel supported sulfur doped nickel vanadium layered double hydroxide (S 1.5 -NiV-LDH) catalyst, the preparation method is as follows:
[0036] The cut foam nickel is sequentially washed with 1 mol / L nitric acid, ethanol, and deionized water under ultrasonic for 10 minutes, and then vacuum dried at 60 degrees Celsius. The raw materials are 1.5 mmol of analytical pure nickel chloride hexahydrate, 0.6 mmol of vanadium chloride, 6 mmol of urea, and 1.5 mmol of thiourea, which are dissolved in 30 mL of deionized water, and then transferred to a polytetrafluoroethylene lined autoclave after ultrasonic for 20 minutes. The treated foam nickel is placed in the autoclave and reacted at 120 degrees Celsius for 12 hours. After the reaction is completed, the autoclave is cooled to room temperature, and the foam nickel in the autoclave is washed with deionized water. Then, vacuum drying is performed at 60 degrees Celsius for 6 hours to obtain a S 1.5 -NiV-LDH catalyst.
[0037] Example 5, a foam nickel supported sulfur doped nickel vanadium layered double hydroxide (S-NiV-LDH-100℃) catalyst, the preparation method is as follows:
[0038] The cut foam nickel is sequentially washed with 1 mol / L nitric acid, ethanol, and deionized water under ultrasonic for 10 minutes, and then vacuum dried at 60 degrees Celsius; the raw materials are 1.5 mmol of analytical pure nickel chloride hexahydrate, 0.6 mmol of vanadium chloride, 6 mmol of urea, and 0.75 mmol of thiourea, which are dissolved in 30 mL of deionized water, and then transferred into a polytetrafluoroethylene-lined hydrothermal reactor after ultrasonic for 20 minutes, and then the treated foam nickel is put into the reactor, and reacted at 100 degrees Celsius for 12 hours; after the reaction is completed, the reactor is cooled to room temperature, the foam nickel in the reactor is washed with deionized water, and then vacuum dried at 60 degrees Celsius for 6 hours to obtain the S-NiV-LDH-100℃ catalyst.
[0039] Example 6, a foam nickel loaded sulfur doped nickel vanadium layered double hydroxide (S-NiV-LDH-110℃) catalyst, and the preparation method is as follows:
[0040] The cut foam nickel is sequentially washed with 1 mol / L nitric acid, ethanol, and deionized water under ultrasonic for 10 minutes, and then vacuum dried at 60 degrees Celsius; the raw materials are 1.5 mmol of analytical pure nickel chloride hexahydrate, 0.6 mmol of vanadium chloride, 6 mmol of urea, and 0.75 mmol of thiourea, which are dissolved in 30 mL of deionized water, and then transferred into a polytetrafluoroethylene-lined hydrothermal reactor after ultrasonic for 20 minutes, and then the treated foam nickel is put into the reactor, and reacted at 110 degrees Celsius for 12 hours; after the reaction is completed, the reactor is cooled to room temperature, the foam nickel in the reactor is washed with deionized water, and then vacuum dried at 60 degrees Celsius for 6 hours to obtain the S-NiV-LDH-110℃ catalyst.
[0041] Example 7, a foam nickel loaded sulfur doped nickel vanadium layered double hydroxide (S-NiV-LDH-130℃) catalyst, and the preparation method is as follows:
[0042] The cut foam nickel is sequentially washed with 1 mol / L nitric acid, ethanol, and deionized water under ultrasonic for 10 minutes, and then vacuum dried at 60 degrees Celsius; the raw materials are 1.5 mmol of analytical pure nickel chloride hexahydrate, 0.6 mmol of vanadium chloride, 6 mmol of urea, and 0.75 mmol of thiourea, which are dissolved in 30 mL of deionized water, and then transferred into a polytetrafluoroethylene-lined hydrothermal reactor after ultrasonic for 20 minutes, and then the treated foam nickel is put into the reactor, and reacted at 130 degrees Celsius for 12 hours; after the reaction is completed, the reactor is cooled to room temperature, the foam nickel in the reactor is washed with deionized water, and then vacuum dried at 60 degrees Celsius for 6 hours to obtain the S-NiV-LDH-130℃ catalyst.
[0043] Example 8, a kind of foam nickel supported sulfur doped nickel vanadium layered double hydroxide (S-NiV-LDH-140℃) catalyst, its preparation method is as follows:
[0044] The cut foam nickel is washed with 1 mol / L nitric acid, ethanol and deionized water under ultrasonic for 10 minutes, respectively, and then vacuum dried at 60 degrees Celsius; The raw materials are selected as 1.5 mmol of analytical grade nickel chloride hexahydrate, 0.6 mmol of vanadium chloride, 6 mmol of urea and 0.75 mmol of thiourea, dissolved in 30 mL of deionized water, and then transferred to a polytetrafluoroethylene-lined hydrothermal reactor after ultrasonic for 20 minutes, and then the treated foam nickel is placed in the reactor, and reacted at 140 degrees Celsius for 12 hours. After the reaction is completed, the reactor is cooled to room temperature, the foam nickel in the reactor is washed with deionized water, and then vacuum dried at 60 degrees Celsius for 6 hours to obtain the S-NiV-LDH-140℃ catalyst.
[0045] Example 9, a kind of foam nickel supported sulfur doped nickel vanadium layered double hydroxide (S-NiV-LDH-10h) catalyst, its preparation method is as follows:
[0046] The cut foam nickel is washed with 1 mol / L nitric acid, ethanol and deionized water under ultrasonic for 10 minutes, respectively, and then vacuum dried at 60 degrees Celsius; The raw materials are selected as 1.5 mmol of analytical grade nickel chloride hexahydrate, 0.6 mmol of vanadium chloride, 6 mmol of urea and 0.75 mmol of thiourea, dissolved in 30 mL of deionized water, and then transferred to a polytetrafluoroethylene-lined hydrothermal reactor after ultrasonic for 20 minutes, and then the treated foam nickel is placed in the reactor, and reacted at 120 degrees Celsius for 10 hours. After the reaction is completed, the reactor is cooled to room temperature, the foam nickel in the reactor is washed with deionized water, and then vacuum dried at 60 degrees Celsius for 6 hours to obtain the S-NiV-LDH-10h catalyst.
[0047] Example 10, a kind of foam nickel supported sulfur doped nickel vanadium layered double hydroxide (S-NiV-LDH-14h) catalyst, its preparation method is as follows:
[0048] The cut foam nickel is sequentially washed with 1 mol / L nitric acid, ethanol, and deionized water under ultrasonic for 10 minutes, and then vacuum dried at 60 degrees Celsius; the raw materials are 1.5 mmol of analytical grade nickel chloride hexahydrate, 0.6 mmol of vanadium chloride, 6 mmol of urea, and 0.75 mmol of thiourea, which are dissolved in 30 mL of deionized water, and then transferred into a polytetrafluoroethylene-lined hydrothermal reactor after ultrasonic for 20 minutes, and then the treated foam nickel is put into the reactor, and reacted at 120 degrees Celsius for 14 hours; after the reaction is completed, the reactor is cooled to room temperature, the foam nickel in the reactor is washed with deionized water, and then vacuum dried at 60 degrees Celsius for 6 hours to obtain the S-NiV-LDH-14h catalyst.
[0049] Example 11, a foam nickel loaded sulfur-doped nickel vanadium layered double hydroxide (S-Ni 0.6 V 1.5 -LDH) catalyst, and a preparation method thereof is as follows:
[0050] The cut foam nickel is sequentially washed with 1 mol / L nitric acid, ethanol, and deionized water under ultrasonic for 10 minutes, and then vacuum dried at 60 degrees Celsius; the raw materials are 1.5 mmol of analytical grade nickel chloride hexahydrate, 0.6 mmol of vanadium chloride, 6 mmol of urea, and 0.75 mmol of thiourea, which are dissolved in 30 mL of deionized water, and then transferred into a polytetrafluoroethylene-lined hydrothermal reactor after ultrasonic for 20 minutes, and then the treated foam nickel is put into the reactor, and reacted at 120 degrees Celsius for 14 hours; after the reaction is completed, the reactor is cooled to room temperature, the foam nickel in the reactor is washed with deionized water, and then vacuum dried at 60 degrees Celsius for 6 hours to obtain the S-NiV-LDH-14h catalyst. 0.6 V 1.5 -LDH catalyst.
[0051] Example 12, a foam nickel loaded sulfur-doped nickel vanadium layered double hydroxide (S-Ni1V 1.1 -LDH) catalyst, and a preparation method thereof is as follows:
[0052] The cut foam nickel is sequentially washed with 1 mol / L nitric acid, ethanol, and deionized water under ultrasonic for 10 minutes, and then vacuum dried at 60 degrees Celsius; the raw materials are 1.5 mmol of analytical grade nickel chloride hexahydrate, 0.6 mmol of vanadium chloride, 6 mmol of urea, and 0.75 mmol of thiourea, which are dissolved in 30 mL of deionized water, and then transferred into a polytetrafluoroethylene-lined hydrothermal reactor after ultrasonic for 20 minutes, and then the treated foam nickel is put into the reactor, and reacted at 120 degrees Celsius for 14 hours; after the reaction is completed, the reactor is cooled to room temperature, the foam nickel in the reactor is washed with deionized water, and then vacuum dried at 60 degrees Celsius for 6 hours to obtain the S-NiV-LDH-14h catalyst. 1.1 -LDH catalyst.
[0053] Comparative Example 1, a foam nickel supported nickel vanadium layered double hydroxide (NiV-LDH) catalyst, was prepared according to the following method:
[0054] The cut foam nickel was sequentially washed with 1 mol / L nitric acid, ethanol, and deionized water under ultrasonic for 10 minutes, and then vacuum dried at 60 degrees Celsius. Analytically pure 1.5 mmol nickel chloride hexahydrate, 0.6 mmol vanadium chloride, and 6 mmol urea were dissolved in 30 mL deionized water, and after ultrasonic for 20 minutes, the solution was transferred into a polytetrafluoroethylene lined hydrothermal reactor, and the treated foam nickel was placed in the reactor. The reactor was reacted at 120 degrees Celsius for 12 hours. After the reaction was completed, the reactor was cooled to room temperature, and the foam nickel in the reactor was washed with deionized water. The foam nickel was then vacuum dried at 60 degrees Celsius for 6 hours to obtain the NiV-LDH catalyst.
[0055] Performance test:
[0056] The S 0.75 -NiV-LDH catalyst prepared in Example 1 was analyzed, and the obtained XRD spectrum is shown in Figure 1 ;
[0057] The samples prepared in Example 1 and Comparative Example 1 were respectively tested by cyclic voltammetry, and the double-layer capacitance values were calculated. The cyclic voltammetry curve of the sample prepared in Example 1 in a potassium hydroxide and 1,5-pentanediol mixed electrolyte is shown in Figure 2 , and the cyclic voltammetry curve of Comparative Example 1 is shown in Figure 3 . The double-layer capacitance value results are shown in Figure 4 ;
[0058] The samples prepared in Example 1 and Comparative Example 1 were used as electrocatalytic materials to test their performance in the electrochemical oxidation of 1,5-pentanediol to 1,5-pentanedioic acid. The two samples were respectively used as working electrodes, and platinum sheets were used as counter electrodes. The mercury / mercury oxide electrode was used as a reference electrode. The potential applied during power supply was 1.1-1.7 V relative to the reversible hydrogen electrode. The LSV curve obtained is shown in Figure 5 . According to Figure 5 , it can be seen that the foam nickel supported sulfur doped nickel vanadium layered double hydroxide (S 0.75 -NiV-LDH) catalyst prepared in Example 1 can obtain a current density of 10 mA / cm 2 to drive the electrochemical oxidation of 1,5-pentanediol in a solution of 1 mol / L potassium hydroxide + 0.3 mol / L 1,5-pentanediol, only requiring 1.32 V (relative to the reversible hydrogen electrode), and can reach a current density of 100 mA / cm 2The current density required is only 1.35V (relative to the standard hydrogen electrode);
[0059] The samples prepared in Examples 1, 2, 3, and 4 were used as electrocatalytic materials to test their performance in the electrochemical oxidation of 1,5-pentanediol to 1,5-pentanediic acid. Four samples were used as working electrodes, with a platinum sheet as the counter electrode and a mercury / mercuric oxide electrode as the reference electrode. Electrochemical workstation measurements showed that the applied potential during energization was 1.1–1.7 V compared to the reversible hydrogen electrode, yielding the following results: Figure 6 The LSV curve shown is shown.
[0060] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included within the protection scope of the present invention.
Claims
1. A method for preparing an S-NiV-LDH catalyst, characterized in that, Includes the following steps: The cut nickel foam was washed and dried sequentially with nitric acid, ethanol, and deionized water under ultrasonic conditions. Nickel chloride hexahydrate, vanadium chloride, urea, and thiourea were dissolved in deionized water and stirred. The solution was then transferred to a hydrothermal reactor lined with polytetrafluoroethylene containing treated nickel foam for hydrothermal reaction. After cooling to room temperature, washing, and vacuum drying, the S-NiV-LDH catalyst was obtained.
2. The method for preparing the S-NiV-LDH catalyst according to claim 1, characterized in that, In the step of washing and drying the cut nickel foam sequentially with nitric acid, ethanol, and deionized water under ultrasonic conditions, the concentration of the nitric acid is 1~1.2 mol / L.
3. The method for preparing the S-NiV-LDH catalyst according to claim 1, characterized in that, In the step of dissolving nickel chloride hexahydrate, vanadium chloride, urea, and thiourea in deionized water and stirring, the molar ratio of nickel chloride hexahydrate, vanadium chloride, urea, and thiourea is 0.6~1.5:0.6~1.5:3~6:0.375~1.
5.
4. The method for preparing the S-NiV-LDH catalyst according to claim 1, characterized in that, The hydrothermal reaction is carried out at a temperature of 100-140 degrees Celsius for 10-14 hours.
5. An S-NiV-LDH catalyst, characterized in that, It is prepared using the preparation method described in any one of claims 1-4.
6. The application of the S-NiV-LDH catalyst as described in claim 5 in the electrocatalytic oxidation of 1,5-pentanediol to 1,5-pentanediic acid, characterized in that, Includes the following steps: The S-NiV-LDH catalyst was placed in an electrochemical reaction cell, and 1,5-pentanediol was used as a raw material. Under the influence of electricity, 1,5-pentanediol was generated on the surface of the working electrode through the catalytic action of the S-NiV-LDH catalyst.
7. The application according to claim 6, characterized in that, The electrochemical reaction cell is an H-type electrolytic cell, employing a three-electrode system. The S-NiV-LDH catalyst is used as the anode electrocatalyst, a platinum sheet as the cathode electrocatalyst, and mercury / mercuric oxide as the reference electrode. The anode electrolyte in the H-type electrolytic cell is a mixed solution of potassium hydroxide and 1,5-pentanediol, and the cathode electrolyte is potassium hydroxide. The electro-oxidation reaction of 1,5-pentanediol is driven by an electric current.
8. The application according to claim 6, characterized in that, The potential applied under the energized condition is 1.1~1.7V compared to the reversible hydrogen electrode.