CN109234754B - Synthesis of NH4V4O10Preparation method of/CF water cracking catalyst - Google Patents

Synthesis of NH4V4O10Preparation method of/CF water cracking catalyst Download PDF

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CN109234754B
CN109234754B CN201811148545.1A CN201811148545A CN109234754B CN 109234754 B CN109234754 B CN 109234754B CN 201811148545 A CN201811148545 A CN 201811148545A CN 109234754 B CN109234754 B CN 109234754B
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黄剑锋
巩颖波
冯亮亮
曹丽云
杨丹
王琳琳
王潇
杜盈盈
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Shaanxi University of Science and Technology
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    • C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
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Abstract

The invention discloses a method for synthesizing NH4V4O10/CPreparing 10mL of solution A containing complexing agent triethylamine, cleaning foamy copper, and placing the foamy copper into an aqueous solution with nitrogen for temporary storage; weighing NH4VO3、C3H6O3And CO (NH)2)2Adding the mixture into deionized water, performing ultrasonic oscillation to obtain a clear solution B, mixing the solution A and the solution B, and reacting in a phase reactor at 100-150 ℃ for 12-24 h; collecting the product; the final product is directly synthesized by adopting one-step hydrothermal reaction, the process is simple and efficient, the synthesis temperature is low, regular nanosheets are formed on the foamy copper, the free inlet and outlet of ions are facilitated, and NH can be improved4V4O10The electrochemical performance of (2).

Description

Synthesis of NH4V4O10Preparation method of/CF water cracking catalyst
Technical Field
The invention relates to a preparation process of a photoelectric catalytic material, in particular to a method for synthesizing NH4V4O10A preparation method of a/CF water cracking catalyst.
Background
Energy problems are one of the main problems which plague the faster development of the current society. Due to the extensive use of fossil fuels, and the series of problems that arise, it is important for human development to solve these problems. The electrolytic water technology is one of the effective ways to generate clean energy. In the water splitting process, two parts of hydrogen production and oxygen production are involved. Hydrogen is a zero-pollution high-efficiency clean energy, and the cleanest method for preparing hydrogen is to prepare hydrogen by electrocatalysis water splitting. The best electrocatalysts for hydrogen production reaction by electrolysis of water are Pt-based materials, and these noble metal catalysts are very efficient in hydrogen production, but their extensive use on a large scale is limited due to their high price. In order to reduce the cost and improve the hydrogen production, the development of an electrocatalyst which is cheap, rich in earth content, good in stability and capable of overcoming the hydrogen production potential is urgently needed.
As shown in the study, NH4V4O10Has electrochemical performance and photocatalytic performance, and both the two sides have application. However, the water-based catalytic decomposition performance of such materials is still unknown. Pure NH4V4O10The banded nano-structure is compact, and the nanobelts are thick and almost have no electrochemical hydrogen evolution performance. The conductivity of the composite foam copper is improved, the structure of the composite foam copper is changed, and some hydrogen evolution performances are shown. NH synthesized by hydrothermal method4V4O10the/CF has the performance of catalyzing hydrogen production.
Currently, NH is synthesized4V4O10The method comprises a hydrothermal method and a thermal decomposition method, and the synthesized flower has a strip shape and a strip-shaped assembled flower shape. The method of Large scale hydrothermal synthesis and electrochemistry of ammonium vanadia bronzes Zhang K F, Zhang G Q, Liu X and the like successfully prepares NH by using oxalic acid and ammonium metavanadate through hydrothermal reheat decomposition4V4O10A nanoribbon. Ningning uses NH4VO3 and H2C2O 4.2H2O as raw materials to prepare flower-shaped NH by a hydrothermal method4V4O10The electrode material with the micro-nano structure is expected to be a novel lithium ion battery anode material.
Disclosure of Invention
The invention aims to provide a method for synthesizing NH4V4O10Preparation method of/CF water cracking catalyst, which is easy to operate, mild in condition, short in time consumption and capable of preparing NH4V4O10The product has high crystallinity, uniform appearance and electrocatalytic hydrogen evolution performance.
In order to achieve the purpose, the invention adopts the following technical scheme:
synthesis of NH4V4O10The preparation method of the/CF water cracking catalyst comprises the following steps:
(1) preparing 10mL of solution A containing complexing agent triethylamine, wherein the concentration is 0.001-0.005 mol/L;
(2) immersing the foamy copper into a pure acetone solution for ultrasonic oscillation cleaning, immersing the foamy copper into hydrochloric acid for ultrasonic oscillation cleaning, finally alternately flushing the foamy copper for a plurality of times by using ethanol and deionized water respectively, and temporarily storing the foamy copper in an aqueous solution with introduced nitrogen;
(3) weighing NH according to the molar ratio of (3-6) to (2-4) to (3-5)4VO3、C3H6O3And CO (NH)2)2Simultaneously adding the mixture into 50mL of deionized water to ensure NH in the solution4VO3The concentration is 0.06-0.12 mol/L, the concentration of lactic acid is 0.04-0.8 mol/L, the concentration of urea is 0.06-0.1 mol/L, and the clear solution B is obtained by ultrasonic oscillation and uniform mixing at room temperature;
(4) mixing the solution A obtained in the step (1) and the solution B obtained in the step (3), wherein NH in the mixed solution4VO3The concentration of the sodium lactate is 0.05-0.1 mol/L, the concentration of the lactic acid is 0.03-0.7 mol/L, the concentration of the urea is 0.05-0.08 mol/L, the concentration of the triethylamine is 0.00017-0.00083 mol/L, the copper foam sheets processed in the step (2) are added, the copper foam sheets are transferred into the reaction lining together and then sealed, then the lining is arranged in an outer kettle and fixed, then the inner kettle is placed in a homogeneous phase reactor, and then the reaction is carried out for 12-24 hours at the temperature of 100-150 ℃;
(5) after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, taking out the cooled foamy copper product after the reaction, then alternately cleaning the foamy copper product with water and alcohol, collecting the product, and drying the collected product to obtain NH4V4O10a/CF composite water cracking catalyst.
Further, in the step (2), soaking the foamy copper into a pure acetone solution for ultrasonic vibration cleaning for 5-15 min, then soaking the foamy copper into 2-4 mol/L hydrochloric acid for ultrasonic vibration cleaning for 5-15 min, and finally alternately washing with ethanol and deionized water for several times.
Further, in the step (2), ethanol and deionized water are alternately washed for 3-5 times.
Further, weighing NH in the step (3)4VO3、C3H6O3And CO (NH)2)2Simultaneously adding into 50mL of deionized water, and placing in a chamberAnd carrying out ultrasonic oscillation for 10-30 min at the temperature to obtain a clear solution B.
Further, collecting the product of the copper foam taken out in the step (5) after 3 times of water washing and 3 times of alcohol alternate washing.
Further, collecting the product after cleaning in the step (5), and drying the product for 10-14 hours at 50-70 ℃ to obtain NH4V4O10a/CF composite water cracking catalyst.
The invention has the following beneficial effects:
(1) the method adopts one-step hydrothermal reaction to directly synthesize the final product, has simple and efficient process, low synthesis temperature, easy operation, no harsh reaction conditions, common and cheap raw materials, low cost and no need of post-treatment.
(2) NH prepared by the method4V4O10the/CF composite water cracking catalyst forms regular nano-sheets on the foam copper, and the thickness of the nano-sheets is about 40 nm. The nano sheet is favorable for free access of ions and is also favorable for electrolyte and NH4V4O10Sufficient contact of/CF nanoplates, in turn, enables improvement of NH4V4O10Electrochemical performance of (1), change of pure NH by compounding with copper foam4V4O10The structure provides more reaction sites.
(3) The product prepared by the method is foam copper loaded NH4V4O10The nano-sheet has high purity and good crystallinity, can show good electrochemical performance when being used as an electrolytic water electrode material, and has the electrochemical performance of 10mA/cm2The overpotential of (2) is about 513mV at the current density of (1).
Drawings
FIG. 1 shows NH prepared in example 2 of the present invention4V4O10Powder of/CF (powder scraped from copper foam) X-ray diffraction (XRD) pattern
FIG. 2 shows NH prepared in example 2 of the present invention4V4O10Scanning Electron Microscope (SEM) photograph of/CF
FIG. 3 shows NH prepared in example 2 of the present invention4V4O10Per CF Linear Sweep Voltammetry (LSV) performance test chart
Detailed Description
The present invention will be described in further detail with reference to the following examples, which are not intended to limit the invention thereto.
Example 1:
(1) 10mL of solution A containing complexing agent triethylamine is prepared, and the concentration is kept at 0.001 mol/L.
(2) Soaking the foamy copper into a pure acetone solution for ultrasonic oscillation cleaning for 5min, soaking the foamy copper into 2mol/L hydrochloric acid for ultrasonic oscillation cleaning for 5min, and finally alternately washing the foamy copper with ethanol and deionized water for 3 times respectively to obtain the foamy copper which is temporarily stored in an aqueous solution with introduced nitrogen.
(3) Weighing NH4VO3C3H6O3 and CO (NH)2)2Simultaneously adding the mixture into 50mL of deionized water, and controlling NH4VO3:C3H6O3:CO(NH2)2At a molar ratio of 3:2:3, in which case NH4VO3The concentration of the mixed solution is 0.06mol/L, the concentration of the lactic acid is 0.04mol/L, the concentration of the urea is 0.06mol/L, and the clear solution B is obtained by ultrasonic oscillation for 10min at room temperature.
(4) Mixing the solution A obtained in the step (1) and the solution B obtained in the step (3), wherein NH in the mixed solution4VO3The concentration of the sodium lactate is 0.05mol/L, the concentration of the lactic acid is 0.03mol/L, the concentration of the urea is 0.05mol/L, the concentration of the triethylamine is 0.00017mol/L, the newly processed foam copper sheet is added, the foam copper sheet is transferred into a reaction lining and sealed, then the lining is arranged in an outer kettle and fixed, then the inner kettle is arranged in a homogeneous reactor, and then the reaction is carried out for 24 hours at the temperature of 100 ℃.
(5) After the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, then taking out the cooled foamy copper product after the reaction, collecting the product after 3 times of water washing and 3 times of alcohol alternate washing, and drying for 10 hours at 50 ℃ to obtain NH4V4O10a/CF composite water cracking catalyst.
Example 2:
(1) 10mL of solution A containing a complexing agent triethylamine is prepared, and the concentration is kept at 0.003 mol/L.
(2) Soaking the foamy copper into a pure acetone solution for ultrasonic oscillation cleaning for 10min, soaking the foamy copper into 3mol/L hydrochloric acid for ultrasonic oscillation cleaning for 10min, and finally alternately washing the foamy copper with ethanol and deionized water for 4 times respectively to obtain the foamy copper which is temporarily stored in an aqueous solution with introduced nitrogen.
(3) Weighing NH4VO3C3H6O3 and CO (NH)2)2Simultaneously adding the mixture into 50mL of deionized water, and controlling NH4VO3:C3H6O3:CO(NH2)2At a molar ratio of 4.5:3:4, in which case NH4VO3The concentration of the mixed solution is 0.09 mol/L, the concentration of the lactic acid is 0.05mol/L, the concentration of the urea is 0.08mol/L, and the clear solution B is obtained by ultrasonic oscillation at room temperature for 20 min.
(4) Mixing the solution A obtained in the step (1) and the solution B obtained in the step (3), wherein NH in the mixed solution4VO3The concentration of the sodium hydrogen carbonate is 0.075mol/L, the concentration of the lactic acid is 0.05mol/L, the concentration of the urea is 0.067mol/L, the concentration of the triethylamine is 0.0005mol/L, and the newly processed foam copper sheet is added, and is transferred into a reaction lining and sealed, then the lining is arranged in an outer kettle and is fixed, and then the inner kettle is arranged in a homogeneous phase reactor, and then the reaction is carried out for 20 hours at 120 ℃.
(5) After the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, then taking out the cooled foamy copper product after the reaction, collecting the product after 3 times of water washing and 3 times of alcohol alternate washing, and drying for 12 hours at 60 ℃ to obtain NH4V4O10a/CF composite water cracking catalyst.
It can be seen from FIG. 1 that relatively pure NH was synthesized4V4O10The diffraction peak of nickel foam was observed in the powder. The sample shows NH of (001), (110) and (020) at diffraction angles of 9.2 degrees, 25.5 degrees and 49.7 degrees respectively4V4O10Diffraction peaks of the crystal planes, illustrating NH4V4O10the/CF catalyst was successfully prepared.
From the SEM image of fig. 2, it can be seen that the morphology of the sample is nanosheet grown on copper foam, and the thickness of the nanosheet is about 40nm or so.
As can be seen from the linear scanning voltammogram of FIG. 3, the sample has a current density of 10mA/cm2When the hydrogen storage battery is used, the overpotential of the overpotential is 513mV, and the overpotential shows that the overpotential has certain electrocatalytic hydrogen evolution activity.
Example 3:
(1) 10mL of solution A containing complexing agent triethylamine is prepared, and the concentration is kept at 0.005 mol/L.
(2) Soaking the foamy copper into a pure acetone solution for ultrasonic oscillation cleaning for 15min, soaking the foamy copper into 4mol/L hydrochloric acid for ultrasonic oscillation cleaning for 15min, and finally alternately washing the foamy copper with ethanol and deionized water for 5 times respectively to obtain the foamy copper which is temporarily stored in an aqueous solution with introduced nitrogen.
(3) Weighing NH4VO3C3H6O3 and CO (NH)2)2Simultaneously adding the mixture into 50mL of deionized water, and controlling NH4VO3:C3H6O3:CO(NH2)2At a molar ratio of 6:4:5, in which case NH4VO3The concentration of the mixed solution is 0.12mol/L, the concentration of the lactic acid is 0.8mol/L, the concentration of the urea is 0.1mol/L, and the clear solution B is obtained by ultrasonic oscillation for 30min at room temperature.
(4) Mixing the solution A obtained in the step (1) and the solution B obtained in the step (3), wherein NH in the mixed solution4VO3The concentration of the sodium lactate is 0.1mol/L, the concentration of the lactic acid is 0.7mol/L, the concentration of the urea is 0.08mol/L, the concentration of the triethylamine is 0.00083mol/L, the newly processed foam copper sheet is added, the foam copper sheet is transferred into a reaction lining together and sealed, then the lining is arranged in an outer kettle and fixed, then the inner kettle is placed in a homogeneous phase reactor, and then the reaction is carried out for 12 hours at 150 ℃.
(5) After the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, then taking out the cooled foamy copper product after the reaction, collecting the product after 3 times of water washing and 3 times of alcohol alternate washing, and drying for 14 hours at 70 ℃ to obtain NH4V4O10a/CF composite water cracking catalyst.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the above embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the embodiments of the invention without departing from the spirit and scope of the invention, which is to be covered by the claims.

Claims (6)

1. Synthesis of NH4V4O10The preparation method of the/CF water cracking catalyst is characterized by comprising the following steps:
(1) preparing 10mL of solution A containing complexing agent triethylamine, wherein the concentration is 0.001-0.005 mol/L;
(2) immersing the foamy copper into a pure acetone solution for ultrasonic oscillation cleaning, immersing the foamy copper into hydrochloric acid for ultrasonic oscillation cleaning, finally alternately flushing the foamy copper for a plurality of times by using ethanol and deionized water respectively, and temporarily storing the foamy copper in an aqueous solution with introduced nitrogen;
(3) weighing NH according to the molar ratio of (3-6) to (2-4) to (3-5)4VO3、C3H6O3And CO (NH)2)2Simultaneously adding the mixture into 50mL of deionized water to ensure NH in the solution4VO3The concentration is 0.06-0.12 mol/L, the concentration of lactic acid is 0.04-0.8 mol/L, the concentration of urea is 0.06-0.1 mol/L, and the clear solution B is obtained by ultrasonic oscillation and uniform mixing at room temperature;
(4) mixing the solution A obtained in the step (1) and the solution B obtained in the step (3), wherein NH in the mixed solution4VO3The concentration of the sodium lactate is 0.05-0.1 mol/L, the concentration of the lactic acid is 0.03-0.7 mol/L, the concentration of the urea is 0.05-0.08 mol/L, the concentration of the triethylamine is 0.00017-0.00083 mol/L, the copper foam sheets processed in the step (2) are added, the copper foam sheets are transferred into the reaction lining together and then sealed, then the lining is arranged in an outer kettle and fixed, then the inner kettle is placed in a homogeneous phase reactor, and then the reaction is carried out for 12-24 hours at the temperature of 100-150 ℃;
(5) after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, taking out the cooled foamy copper product after the reaction, then alternately cleaning the foamy copper product with water and alcohol, collecting the product, and drying the collected product to obtain NH4V4O10Water splitting of/CF compositeAnd (4) decomposing the catalyst.
2. The method of claim 1, wherein: and (3) immersing the foamy copper into a pure acetone solution for ultrasonic oscillation cleaning for 5-15 min, immersing the foamy copper into 2-4 mol/L hydrochloric acid for ultrasonic oscillation cleaning for 5-15 min, and finally alternately washing with ethanol and deionized water for several times.
3. The method of claim 2, wherein: and (3) alternately washing the obtained product for 3-5 times by using ethanol and deionized water respectively in the step (2).
4. The method of claim 1, wherein: weighing NH in the step (3)4VO3、C3H6O3And CO (NH)2)2And simultaneously adding the mixed solution into 50mL of deionized water, and performing ultrasonic oscillation at room temperature for 10-30 min to obtain a clear solution B.
5. The method of claim 1, wherein: and (4) collecting the product of the foam copper taken out in the step (5) after washing the product of the foam copper by 3 times of water and alternately washing the product of the foam copper by 3 times of alcohol.
6. The method of claim 5, wherein: collecting the product after cleaning in the step (5), and drying at 50-70 ℃ for 10-14 h to obtain NH4V4O10a/CF composite water cracking catalyst.
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