CN115074772A - Electrocatalyst nickel-vanadium-cobalt ternary layered double hydroxide, preparation method and application - Google Patents
Electrocatalyst nickel-vanadium-cobalt ternary layered double hydroxide, preparation method and application Download PDFInfo
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Abstract
The invention discloses an electrocatalyst nickel-vanadium-cobalt ternary layered double hydroxide, a preparation method and application, wherein the electrocatalyst nickel-vanadium-cobalt ternary layered double hydroxide is used for electrocatalytic oxidation of 5-hydroxymethylfurfural, and the preparation method comprises the following steps: step 1, cutting foam nickel NF, and carrying out ultrasonic cleaning to obtain pretreated foam nickel; step 2, adding NiCl 2 ·6H 2 O、CoCl 2 ·6H 2 O and VCl 3 Dissolving the mixture in water, adding urea, and uniformly stirring to obtain a first mixed solution; and putting the foamed nickel into a high-pressure reaction kettle for reaction to obtain the high-efficiency electrocatalyst nickel-vanadium-cobalt ternary layered double hydroxide NiVCo-LDHs. The electric catalystThe oxidant can be used for selectively and electrically catalyzing and oxidizing the HMF to prepare high-value FDCA, the oxidation of the HMF at a low potential has high oxidation current density, and stable yield and Faraday efficiency of the FDCA can be obtained in 10 continuous cyclic electrolysis.
Description
Technical Field
The invention relates to the field of electrocatalysts, in particular to a high-efficiency electrocatalyst nickel-vanadium-cobalt ternary layered double hydroxide, a preparation method and application thereof.
Background
5-Hydroxymethylfurfural (HMF) is a typical C6-based carbohydrate derived biomass platform molecule widely used for the production of pharmaceutical intermediates, polymer monomers and agrochemicals. The oxidation product 2, 5-furancarboxylic acid (FDCA) is an important polymer monomer, has a structure similar to that of petroleum-based terephthalic acid monomer, and can synthesize polyethylene furan ester (PEF) to replace a large amount of ethylene terephthalate (PET) plastic.
At present, the method used for converting 5-Hydroxymethylfurfural (HMF) into 2, 5-furancarboxylic acid (FDCA) is mainly an aerobic oxidation method, which requires harsh conditions of high temperature, high pressure, toxic oxidants or noble metal catalysts, etc., contrary to the concept of green chemistry. Therefore, a more environment-friendly electrocatalysis method is produced, the electrocatalysis method can convert HMF into FDCA at normal temperature and normal pressure through electron transfer with high selectivity, and the method is a green and efficient conversion way. Among the reported electrocatalysts, Ni and Co based catalysts perform optimally, can almost quantitatively convert HMF to FDCA in its entirety, unfortunately usually require high overpotential (1.423V vs. rhe) to drive efficient HMF conversion, and the stability of the catalyst is poor, and in order to achieve an economical and efficient conversion of HMF to FDCA, it is highly desirable to construct an electrocatalyst with high activity, strong stability and inexpensive properties.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a high-efficiency electrocatalyst nickel-vanadium-cobalt ternary layered double hydroxide, a preparation method and application.
The purpose of the invention is realized by adopting the following technical scheme:
in a first aspect, the present invention provides an electrocatalyst nickel-vanadium-cobalt ternary layered double hydroxide, which is a highly efficient electrocatalyst nickel-vanadium-cobalt ternary layered double hydroxide for the electrocatalytic oxidation of 5-hydroxymethylfurfural.
In a second aspect, the present invention provides a method for preparing an electrocatalyst nickel-vanadium-cobalt ternary layered double hydroxide, comprising the steps of:
cutting the foam nickel NF, ultrasonically cleaning to remove impurities, and drying at room temperature to obtain pretreated foam nickel;
firstly, NiCl is added 2 ·6H 2 O、CoCl 2 ·6H 2 O and VCl 3 Dissolving the mixture in water to form a transparent solution, adding urea, and uniformly stirring to obtain a first mixed solution;
secondly, placing the pretreated foamed nickel into a high-pressure reaction kettle, transferring the first mixed solution into the high-pressure reaction kettle, screwing the high-pressure reaction kettle, placing the high-pressure reaction kettle into an oven, carrying out high-pressure sealing reaction, washing the foamed nickel by using water and ethanol after the reaction is cooled to room temperature, and drying the foamed nickel overnight to obtain the high-efficiency electrocatalyst nickel-vanadium-cobalt ternary layered double hydroxide NiVCo-LDHs.
Preferably, in the step 1, the nickel foam NF is cut into the size of 1cm × 3 cm.
Preferably, in the step 1, the ultrasonic cleaning is performed by sequentially using acetone, diluted hydrochloric acid, deionized water and ethanol.
Preferably, in the step 2, NiCl 2 ·6H 2 O、CoCl 2 ·6H 2 O and VCl 3 The molar ratio of (A) to (B) is 3:0-1: 0-1.
Preferably, in the step 2, NiCl 2 ·6H 2 O、CoCl 2 ·6H 2 O and VCl 3 In a molar ratio of 3:0.33:0.67, 30mL of water, Ni 2+ 、Co 2+ And V 3+ The total molar amount in the solution was 1.08 mmol.
Preferably, in the step 2, the adding amount of the urea is 240.24mg, and the stirring time is 30-60 min.
Preferably, in the step 2, the reaction temperature of the high-pressure reaction kettle is 120 ℃, and the reaction time is 12 hours; after the reaction, the washed foamed nickel was dried in an oven at 60 ℃.
In a third aspect, the invention provides a high-efficiency electrocatalyst nickel-vanadium-cobalt ternary layered double hydroxide, which is applied to electrocatalytic conversion of 5-Hydroxymethylfurfural (HMF) into 2, 5-furancarboxylic acid (FDCA).
The invention has the beneficial effects that:
1. the invention discloses a NiVCo-LDHs electrocatalyst prepared on a foamed nickel substrate, which has the advantages that the electrocatalyst is used for selectively carrying out electrocatalytic oxidation on HMF in 1mol/LKOH to prepare high-value FDCA, the electrocatalyst is used for oxidizing the HMF at a low potential, has high oxidation current density, and can obtain stable yield and Faraday efficiency of the FDCA in 10 continuous circulating electrolysis.
2. In the invention, NiVCo-LDHs are synthesized by a simple hydrothermal method, and the NiVCo-LDHs with the optimal performance are screened out by simple initial raw material preparation and are used as an advanced electrocatalyst for converting the HMF into the FDCA. The NiVCo-LDHs have a wrinkled nano-sheet structure, and the current density of oxidizing HMF under the voltage of 1.37Vvs RHE can reach 100 mA-cm -2 . In addition, the prepared NiVCo-LDHs have excellent durability, and the yield of the FDCA is 93.2-99.7% and the yield of the FE is 86.5-97.8% in 10 continuous cycles, which is far better than most of the reported LDHs and nickel-based oxide catalysts.
3, the invention shows through characterization that the specific surface area can be increased by constructing a folded nanosheet structure through the addition of V atoms, and active sites are enriched by introducing oxygen vacancies. The invention prepares the ternary LDHs electrocatalyst with cost benefit, has satisfactory durability and conversion efficiency, and promotes the development of converting HMF into FDCA by a green electrochemical method.
Drawings
The invention is further illustrated by means of the attached drawings, but the embodiments in the drawings do not constitute any limitation to the invention, and for a person skilled in the art, other drawings can be obtained on the basis of the following drawings without inventive effort.
FIG. 1 is an SEM image, TEM image (c) and energy dispersive X-ray elemental map (d-g) of NiVCo-LDHs of the present invention at low resolution (a) and high resolution (b);
FIG. 2 is a comparison of XRD spectra of NiVCo-LDHs, NiCo-LDHs, NiV-LDHs and NiOOH of examples of the present invention (a) and XPS spectra of Ni2p, (c) V2 p and (d) Co 2p (b);
FIG. 3 (a) shows LSV curves for NiVCo-LDHs scanned at 10mV s-1 in 1M KOH with and without 10mM HMF; (b) shows LSV curves for NiVCo-LDHs, NiV-LDHs and NiCo-LDHs in 1M KOH with 10mM HMF; (c) comparing the oxidized HMF current densities at different potentials;
FIG. 4 is a Tafel comparison plot (a) of NiVCo-LDHs, NiV-LDHs and NiCo-LDHs and a plot of capacitance current density versus scan rate at a potential of 0.95Vvs RHE for examples of the present invention (b);
FIG. 5 (a) shows the HPLC spectra when different charges pass; (b) shows the concentration of HMF and its oxidation products as a function of the charge passed in 10mL of 1.0MKOH containing 10mM HMF at a potential of 1.376V vs RHE; (c) a graph showing the comparison of the conversion of HMF, the yield of FDCA and the FE of FDCA on electrodes NiVCo-LDHs, NiV-LDHs and NiCo-LDHs at a RHE voltage of 1.376 Vvs; (d) two routes representing the potential for oxidation of HMF to FDCA; (e) shows that the yield and FE of FDCA are obtained under continuous 10-cycle electrolysis of the NiVCo-LDHs electrode;
FIG. 6 is an XPS analysis of (a) Ni2p (b) V2 p and (c) Co 2p and (d) O1s of NiVCo-LDHs freshly prepared and after 10 cycles in examples of the present invention.
Detailed Description
For the purpose of more clearly illustrating the present invention and more clearly understanding the technical features, objects and advantages of the present invention, the technical solutions of the present invention will now be described in detail below, but the present invention should not be construed as being limited to the implementable scope of the present invention.
The starting materials, reagents or apparatuses used in the following examples are conventionally commercially available or can be obtained by conventionally known methods, unless otherwise specified.
The invention is further described with reference to the following examples.
Examples
The embodiment of the invention provides an electrocatalyst nickel-vanadium-cobalt ternary layered double hydroxide, and particularly relates to an efficient electrocatalyst nickel-vanadium-cobalt ternary layered double hydroxide for electrocatalytic oxidation of 5-hydroxymethylfurfural.
The preparation method of the electrocatalyst nickel-vanadium-cobalt ternary layered double hydroxide for efficiently carrying out electrocatalytic oxidation on 5-hydroxymethylfurfural comprises the following steps:
cutting foamed Nickel (NF) into 1cm × 3cm, respectively performing ultrasonic cleaning treatment with acetone, dilute hydrochloric acid, deionized water and ethanol to remove pollutants, blow-drying the surface with nitrogen, and naturally drying at room temperature.
under moderate agitation, NiCl is added 2 ·6H 2 O、CoCl 2 ·6H 2 O and VCl 3 Dissolving in 30mL of water at a ratio of 3:0.33:0.67, wherein Ni 2+ 、Co 2+ And V 3+ The total amount of (2) was 1.08 mmol. Due to VCl 3 Moisture absorption is easy, and the product needs to be weighed quickly for use; after a clear solution was formed, 240.24mg of urea was further added to the solution and stirred for 30 minutes at medium intensity; putting fresh and clean foam nickel into a 50mL high-pressure reaction kettle in an inclined manner according to the wall, and adding the Ni 2+ 、Co 2+ And V 3+ Transferring the mixed solution into a reaction kettle; screwing down the high-pressure reaction kettle, placing the high-pressure reaction kettle in a drying oven, and carrying out high-pressure sealing reaction for 12 hours at 120 ℃; after the reaction is cooled to room temperature, a large amount of water and ethanol are used for washing the foamed nickel, and the foamed nickel is dried at 60 ℃ overnight to obtain the catalyst NiVCo-LDHs.
Comparative example 1
An electrocatalyst NiV-LDHs is prepared by the same method as the example, except that in step 2, no CoCl is added 2 ·6H 2 O，NiCl 2 ·6H 2 O and VCl 3 Is 3: 1.
Comparative example 2
The preparation method of the electrocatalyst NiCo-LDHs is the same as that of the electrocatalyst NiCo-LDHsExample with the difference that in step 2, no VCl is added 3 ，NiCl 2 ·6H 2 O and CoCl 2 ·6H 2 The molar ratio of O is 3: 1.
Comparative example 3
An electrocatalyst, NiOOH, was prepared as in the example, except that in step 2, no CoCl was added 2 ·6H 2 O and VCl 3 。
Examples of the experiments
(1) Electrochemical performance testing of oxidized HMF:
cutting foamed nickel loaded with NiVCo-LDHs into a size of 1cm multiplied by 0.5cm, clamping and exposing 0.5cm multiplied by 0.5cm by using an electrode as a working electrode, using a saturated Ag/AgCl electrode as a reference electrode, and using a carbon rod as a counter electrode; using CHI 920E electrochemical workstation in 1mol/L KOH solution at a potential interval of 0.2V-0.65V with 10mV s -1 Performing a linear sweep voltammetry technique (LSV) to test the performance of the oxidized water; adding fresh 10mmol/L HMF into 1mol/LKOH solution, and testing the performance of selectively oxidizing the HMF by using the same linear sweep voltammetry; in the above LSV test, the solution resistance was tested by CHI 920e and 85% of iR compensation was applied to all LSV tests.
(2) Cycle stability testing of electrochemically oxidized HMF:
an H-type electrolytic cell separated by an N117 proton exchange membrane (Sigma-Aldrich) is filled with 10mL of 1M KOH solution in a cathode chamber and 10mL of 1M KOH solution containing 10mM HMF in an anode chamber; cutting 1.5cm multiplied by 1cm foam nickel loaded with NiVCo-LDHs, clamping the foam nickel exposed by 1cm multiplied by 1cm by a Pt electrode clamp, placing the foam nickel in an anode chamber as a working electrode, and placing a carbon rod in a cathode chamber as a counter electrode; adding a stirrer in the anode chamber, and carrying out electrocatalytic oxidation on the HMF by using a constant potential electrolysis technology of a DC-EC 1200 electrochemical analyzer (Changchun Dingcheng science and technology Co., Ltd.) under mild stirring until the HMF passes through a charge of 57.89C and then is electrolyzed for one time; after one round of electrolysis is finished, the electrolyte in the electrode chamber is reconfigured, and the same working electrode is washed by a large amount of deionized water and dried and then continuously used as the working electrode for the next round of electrolysis reaction, so that the electrolysis experiment is repeatedly carried out for 10 times.
(3) Qualitative and quantitative analysis of oxidation products:
the separation of the reaction product was carried out by a Tech comp LC2000A high performance liquid chromatograph and a BioRad Aminex HPX-87H column (300X 7.8 mm), and the detection wavelength of an ultraviolet-visible detector was set to 265 nm. Periodically extracting a reaction sample from the reactor, filtering the reaction solution by using a filter head with the diameter of 0.22 mu m, diluting 10 mu L of filtrate by 50 times by using deionized water, and injecting the diluted filtrate into a chromatographic column for analysis; 5mM sulfuric acid was used as mobile phase at 60 ℃ at 0.5mLmin -1 Is subjected to equal separation at a constant flow rate; and carrying out qualitative and quantitative analysis on the separated sample according to the retention time of the standard sample and a standard curve drawn by different concentrations.
The experimental results and their analysis are as follows:
scanning Electron Microscope (SEM) as shown in fig. 1(a) and (b) shows that NiVCo-LDHs nanosheets vertically grow on the surface of the NF substrate, and the size of the nanosheets is micron-sized lateral length and nano-sized ultra-thin thickness.
Transmission electron microscopy image (TEM) in fig. 1 (c) further shows that NiVCo-LDHs nanosheets have abundant wrinkles.
The element mapping image of scanning transmission electron microscope energy dispersive X-ray spectroscopy (STEM-EDX) in fig. 1 (d) shows that the Ni, V, Co and O elements are uniformly distributed and overlapped on the NiVCo-LDHs nanosheets. Scanning Electron Microscope (SEM) and Transmission Electron Microscope (TEM) characterization in fig. 1 shows that the addition of V atoms can increase the specific surface area of NiVCo-LDHs by building a wrinkled nanosheet structure.
② FIG. 2 (a) X-ray diffraction (XRD) shows that NiOOH is hexagonal alpha-Ni (OH) 2 NiCo-LDHs and NiV-LDHs are nickel cobalt hydroxide (JCPDS:33-0429) and nickel vanadium hydroxide (JCPDS:052-1627), respectively, indicating that a typically pure LDH phase is formed during doping. The XRD spectrum of NiVCo-LDHs is consistent with that of NiV-LDHs, which shows that the NiVCo-LDHs and the NiV-LDH have the same structure.
In FIG. 2(b), the high resolution XPS spectrum of Ni2p is at Ni2p 3/2 (854.4eV) and Ni2p 1/2 Two characteristic peaks of (872.3eV), and satellite peaks at 878.4eV and 860.1eV are Ni 2+ Characteristic peak of (2).
In FIG. 2(c)High resolution XPS spectra of V2 p show V2 p 3/2 Three peaks, V, can be fit at 516.2eV, 517.1eV, and 518.0eV 3+ 、V 4+ And V 5+ Indicates V 3+ Oxidized to higher valence state under hydrothermal treatment.
In FIG. 2(d), the high resolution XPS of Co 2p has two main peaks at 780.6eV and 796.2eV, corresponding to Co 2p 3/2 And Co 2p 1/2 The binding energy of (1).
The XPS spectrum of FIG. 2 shows that the binding energy of Ni2p, Co 2p and V2 p of NiVCo-LDHs is slightly shifted negatively compared to that of NiV-LDHs and NiCo-LDHs, indicating that there is a synergistic electronic interaction between Ni, Co and V.
③ As shown in FIG. 3, NiVCo-LDHs oxidize water when the potential is higher than 1.55V vs RHE, LSV increases rapidly after HMF is added, and the current density of oxidizing HMF reaches 100mA cm at 1.37V vs RHE -2 . The lower initial oxidation potential and increased HMF oxidation current density indicate that NiVCo-LDHs favor the oxidation of HMF. The oxidation current density comparison of HMF under different potentials is obtained from LSV curves of oxidizing the HMF by NiV-LDHs, NiCo-LDHs and NiVCo-LDHs, and the NiVCo-LDHs is found to have higher current density and lower initial potential than the NiV-LDHs and the NiCo-LDHs, thereby further emphasizing the good performance of the HMF in oxidation.
Fourthly, as shown in FIG. 4, the Tafel slope value (18.05mV dec) of NiVCo-LDHs -1 ) Less than NiV-LDH (19.14mV dec) -1 ) And NiCo-LDH (21.59mV dec) -1 ) It is shown that Co-doping of V and Co plays a key role in promoting HMF oxidation kinetics and improving intrinsic activity. Cyclic Voltammetry (CV) measurements collected in the non-faradaic zone at 0.90-1.00V vs RHE showed electrochemically active specific surface area (ECSR) of the catalyst, NiVCo-LDHs (1.56mF cm) -2 ) And NiV-LDHs (1.49 mF. cm) -2 ) The ECSR of the strain is almost equivalent to but higher than that of NiCo-LDHs (1.13mF cm) -2 ) It is shown that the addition of V is crucial to increase the specific surface area of NiVCo-LDHs to construct a multi-folded nanosheet structure.
And fifthly, as shown in fig. 5, the NiVCo-LDHs carries out the electrochemical conversion of the HMF under the external potential of 1.376Vvs RHE, the yield of the finally obtained FDCA is 99.7%, and the Faraday Efficiency (FE) of the FDCA is 97.0%, which indicates that the HMF is successfully converted into the FDCA. While the FE of the FDCA of NiV-LDHs (92.1%) and NiCo-LDHs (90.3%) is inferior. In addition, the prepared NiVCo-LDHs have excellent stability, and the yield of the FDCA is 93.2-99.7% and the yield of the FE is 86.5-97.8% in 10 continuous cycles, which is far better than most of the reported LDHs and nickel-based oxide catalysts (as shown in the following table 1).
TABLE 1 Performance of the different catalysts
Sixthly, in fig. 6, X Photoelectron Spectroscopy (XPS) of the catalyst before and after the reaction further shows that a slight blue shift is observed in the Ni2p region of the NiVCo-LDH after the cycle test (fig. 6a), indicating that high-valence Ni is formed during the reaction and has participated in the oxidation process of HMF. No V2 p signal was detected in NiVCo-LDHs after cycling tests, which could be attributed to dissolution of the higher valence V element (fig. 6 c). In fig. 6d, the X Photoelectron Spectroscopy (XPS) of the catalyst before and after the reaction further shows that active oxygen vacancies are generated during the reaction, providing abundant active sites. In the O1s spectrum, three peaks at 530.8eV (O1), 531.4eV (O2) and 532.2eV (O3) are consistent with the fresh catalyst and can be assigned to the binding energies of the metal-oxygen bond, hydroxyl group and adsorbed water, respectively. Furthermore, O4 at 533.5eV is attributed to surface oxygen defect species, and it is speculated that the dissolution of V species during the reaction initiates oxygen vacancies, the formation of which provides rich active sites, facilitating the electrocatalytic oxidation process of HMF.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (7)
1. An electrocatalyst nickel-vanadium-cobalt ternary layered double hydroxide is characterized in that the electrocatalyst nickel-vanadium-cobalt ternary layered double hydroxide is an electrocatalyst nickel-vanadium-cobalt ternary layered double hydroxide for electrocatalytic oxidation of 5-hydroxymethylfurfural.
2. A preparation method of an electrocatalyst nickel-vanadium-cobalt ternary layered double hydroxide is characterized by comprising the following steps:
step 1, pretreatment of a carrier:
cutting the foam nickel NF, ultrasonically cleaning to remove impurities, and drying at room temperature to obtain pretreated foam nickel;
step 2, preparing a NiVCo-LDHs catalyst:
21: mixing NiCl 2 ·6H 2 O、CoCl 2 ·6H 2 O and VCl 3 Dissolving the mixture in water to form a transparent solution, adding urea, and uniformly stirring to obtain a first mixed solution;
22 placing the pretreated foamed nickel into a high-pressure reaction kettle, transferring the first mixed solution into the high-pressure reaction kettle, screwing down the high-pressure reaction kettle, placing the high-pressure reaction kettle into an oven, carrying out high-pressure sealing reaction, cooling the reaction to room temperature, washing the foamed nickel by using water and ethanol, and drying to obtain the high-efficiency electrocatalyst nickel-vanadium-cobalt ternary layered double hydroxide NiVCo-LDHs.
3. The method of claim 2, wherein in the step 1, the nickel foam NF is cut to a size of 1cm x 3 cm.
4. The preparation method according to claim 2, wherein in the step 1, the ultrasonic cleaning is performed by using acetone, 3mol/L diluted hydrochloric acid, deionized water and ethanol in sequence.
5. The method of claim 2, wherein in step 2, NiCl is added 2 ·6H 2 O、CoCl 2 ·6H 2 O and VCl 3 In a molar ratio of 3:0.33:0.67, 30mL of water, Ni 2+ 、Co 2+ And V 3+ The total molar amount in the solution was 1.08 mmol.
6. The method according to claim 2, wherein the urea is added in an amount of 240.24mg and the stirring time is 30min in step 2.
7. The preparation method according to claim 2, wherein in the step 2, the reaction temperature of the high-pressure reaction kettle is 120 ℃, and the reaction time is 12 hours; after the reaction, the washed nickel foam was dried at 60 ℃.
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