CN113308710B - Conductive cellulose filter paper loaded Ru nanoparticle composite catalyst and preparation method thereof - Google Patents

Conductive cellulose filter paper loaded Ru nanoparticle composite catalyst and preparation method thereof Download PDF

Info

Publication number
CN113308710B
CN113308710B CN202110566503.5A CN202110566503A CN113308710B CN 113308710 B CN113308710 B CN 113308710B CN 202110566503 A CN202110566503 A CN 202110566503A CN 113308710 B CN113308710 B CN 113308710B
Authority
CN
China
Prior art keywords
filter paper
cellulose filter
nanoparticle composite
composite catalyst
solution
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202110566503.5A
Other languages
Chinese (zh)
Other versions
CN113308710A (en
Inventor
张素风
魏宁
姚雪
王全胜
呼旭旭
周秋生
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shaanxi University of Science and Technology
Original Assignee
Shaanxi University of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shaanxi University of Science and Technology filed Critical Shaanxi University of Science and Technology
Priority to CN202110566503.5A priority Critical patent/CN113308710B/en
Publication of CN113308710A publication Critical patent/CN113308710A/en
Application granted granted Critical
Publication of CN113308710B publication Critical patent/CN113308710B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • 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
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/02—Hydrogen or oxygen
    • C25B1/04—Hydrogen or oxygen by electrolysis of water
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/054—Electrodes comprising electrocatalysts supported on a carrier
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)

Abstract

The invention provides a conductive cellulose filter paper loaded Ru nanoparticle composite catalyst and a preparation method thereof, belonging to the technical field of energy materials, and the method comprises the following steps: sequentially immersing qualitative filter paper into a nickel sulfate solution and a sodium borohydride solution, and then cleaning and drying to obtain the cellulose filter paper loaded with the nickel simple substance; soaking the cellulose filter paper loaded with the nickel simple substance into a mixed solution A of anhydrous sodium sulfate, sodium succinate, dimethyl ammonia borane, sodium hypophosphite and nickel sulfate for 0.5-1.5 h, and then cleaning and drying to obtain conductive cellulose filter paper; the conductive cellulose filter paper is used as a working electrode, the electrodeposition is carried out by using the aqueous solution of ruthenium chloride in a three-electrode system, the obtained product is dried after being cleaned, and the obtained conductive cellulose filter paper loaded Ru nanoparticle composite catalyst shows lower overpotential and good conductivity, and can be used as a self-supporting catalyst for the anodic oxygen evolution reaction of electrolyzed water.

Description

Conductive cellulose filter paper loaded Ru nanoparticle composite catalyst and preparation method thereof
Technical Field
The invention belongs to the technical field of energy materials, and particularly relates to a conductive cellulose filter paper loaded Ru nanoparticle composite catalyst and a preparation method thereof.
Technical Field
As the energy crisis and environmental problems caused by the excessive consumption of traditional fossil fuel systems have become more severe, numerous scholars have been devoted to find new energy systems. Hydrogen has a high calorific value and produces only water during use, is environmentally friendly and is considered to be the most promising clean energy source. The electrolysis of water to produce hydrogen has received much attention as a novel energy conversion technology. The water electrolysis comprises an anodic Oxygen Evolution Reaction (OER) and a cathodic hydrogen evolution reaction, wherein the anodic oxygen evolution reaction is a four-electron transfer process, and serious kinetic and thermodynamic retardation processes exist, so that the overpotential is large, the reaction efficiency is low, and the further development of the water electrolysis is seriously hindered. At present, the most active catalysts for OER are the noble metals ruthenium (Ru) and iridium (Ir) and their oxides. However, the expensive price and scarcity have limited the commercial use of precious metals. To overcome this difficulty, it is a preferred strategy to appropriately reduce the amount of noble metal in the catalyst.
The development of the nano-scale noble metal catalyst not only improves the OER performance, but also reduces the use cost of the noble metal. These catalysts require the use of stable supports to anchor the noble metal elements, thereby reducing agglomeration of the noble metal and substantially exposing the active sites of the catalyst. Common support materials are mainly nitrogen-doped carbon materials, metal oxides, metal organic frameworks and layered double hydroxides. The support materials are all powder materials, the electrochemical active area of the surface of the glassy carbon electrode is limited by adding a conductive adhesive in the using process, and the active materials are easy to peel off and have poor stability in the using process. In comparison, self-supported catalysts have the following advantages: (1) the use of binders and additional conductive additives can be avoided; (2) the agglomeration of the nano catalyst material is avoided; (3) the active sites of the catalyst are fully utilized. This has led to extensive attention being paid to self-supporting catalysts. Common support materials mainly include metal materials such as foamed nickel, titanium foil, copper foil and iron foil, and carbon materials such as carbon nanotubes, graphene oxide and carbon fibers. Although these substrates have good electrical conductivity and mechanical properties, they also have inherent disadvantages such as high cost, poor flexibility, heavy weight, etc. Therefore, the substrate is expanded into a cheap, abundant, flexible and environment-friendly substrate, and has great practical value and environmental benefit.
Cellulose is certainly the best candidate in terms of the ease with which the substrate can be obtained. Such materials are generally insulating and do not provide an electron-conducting path between the circuit and the electrocatalyst, severely limiting their application in the field of electrocatalysis.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the conductive cellulose filter paper loaded Ru nanoparticle composite catalyst and the preparation method thereof, and the obtained oxygen evolution reaction catalyst takes cellulose as a substrate, shows lower overpotential and good conductivity, and is a self-supporting catalyst capable of being used for the anodic oxygen evolution reaction of electrolyzed water.
The invention is realized by the following technical scheme:
the preparation method of the conductive cellulose filter paper loaded Ru nanoparticle composite catalyst comprises the following steps:
sequentially immersing qualitative filter paper into a nickel sulfate solution and a sodium borohydride solution, and then cleaning and drying to obtain the cellulose filter paper loaded with the nickel simple substance;
soaking the cellulose filter paper loaded with the nickel simple substance into a mixed solution A of anhydrous sodium sulfate, sodium succinate, dimethyl ammonia borane, sodium hypophosphite and nickel sulfate for 0.5-1.5 h, and then cleaning and drying to obtain conductive cellulose filter paper;
and taking the conductive cellulose filter paper as a working electrode, performing electrodeposition by using an aqueous solution of ruthenium chloride in a three-electrode system, and drying the cleaned product to obtain the conductive cellulose filter paper loaded Ru nanoparticle composite catalyst.
Preferably, the qualitative filter paper is firstly subjected to ultrasonic treatment in deionized water, then transferred to acetone for dipping, dried and then dipped into a nickel sulfate solution and a sodium borohydride solution.
Preferably, the concentration of the nickel sulfate solution is 0.15-0.35M.
Preferably, the concentration of the sodium borohydride solution is 0.4-0.6M.
Preferably, the qualitative filter paper is sequentially and circularly immersed into the nickel sulfate solution and the sodium borohydride solution, and is washed after 3-5 times of circulation.
Preferably, the washing in the step is washing with deionized water and absolute ethyl alcohol in sequence.
Preferably, the ratio of anhydrous sodium sulfate, sodium succinate, dimethyl ammonia borane, sodium hypophosphite, nickel sulfate and deionized water in the mixed solution A is (1.0-2.0) g: (2.0-3.0) g: (0.70-0.74) g: (0.090-0.098) g: (2.0-3.0) g: (80-120) mL.
Preferably, the cellulose filter paper loaded with the nickel simple substance is immersed into the mixed solution A at the temperature of 8-12 ℃.
Preferably, the conductive cellulose filter paper is electrodeposited for 5-20 min under the voltage of-0.6-1.2V.
The conductive cellulose filter paper loaded Ru nanoparticle composite catalyst is prepared by the preparation method of the conductive cellulose filter paper loaded Ru nanoparticle composite catalyst.
Compared with the prior art, the invention has the following beneficial technical effects:
the preparation method of the conductive cellulose filter paper loaded Ru nanoparticle composite OER catalyst comprises the steps of sequentially immersing qualitative filter paper into a nickel sulfate solution and a sodium borohydride solution, the surface of the cellulose can firstly absorb nickel ions, then the nickel ions are reduced by sodium borohydride to form the cellulose filter paper loaded with the nickel simple substance, then the cellulose filter paper is taken as a substrate to be immersed into the mixed solution of anhydrous sodium sulfate, sodium succinate, dimethyl ammonia borane, sodium hypophosphite and nickel sulfate, through a chemical plating mode, amorphous divalent nickel, a small amount of boron and phosphorus are formed on the surface of the substrate to obtain conductive cellulose filter paper, the conductive cellulose filter paper is converted into a working electrode, the method can carry out electrodeposition by means of aqueous solution of ruthenium chloride in a three-electrode system, finally grow the electrocatalyst in situ, can prepare the high-activity oxygen evolution reaction catalyst, and can be used for electrolyzing water to evolve oxygen.
Drawings
FIG. 1 is an SEM image of the material obtained in step 3 of example 2 of the present invention at 200 nm.
FIG. 2 is an SEM photograph of the catalyst obtained in example 2 of the present invention at 200 nm.
FIG. 3 is an XRD spectrum of the catalyst obtained in example 2 of the present invention.
FIG. 4 is a polarization curve of the catalyst obtained in example 2 of the present invention.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
The preparation method of the conductive cellulose filter paper loaded Ru nanoparticle composite OER catalyst comprises the following steps:
step 1, cutting qualitative filter paper into 1 x 2cm 2 And placing the filter paper in deionized water, carrying out ultrasonic treatment for 20min, then transferring the filter paper subjected to ultrasonic treatment to acetone, soaking for 3h, and drying at room temperature to finish cleaning of the qualitative filter paper.
And 2, circularly immersing the dried filter paper into 0.15-0.35M nickel sulfate solution and 0.4-0.6M sodium borohydride solution which are prepared in situ in sequence, washing the filter paper by using deionized water and absolute ethyl alcohol in sequence after circulating for 3-5 times, drying the filter paper at room temperature, and reducing the cellulose surface by using sodium borohydride after absorbing nickel ions to form the active cellulose filter paper loaded with the nickel simple substance.
And 3, weighing 1.0-2.0 g of anhydrous sodium sulfate, 2.0-3.0 g of sodium succinate, 0.70-0.74 g of dimethyl ammonia borane, 0.090-0.098 g of sodium hypophosphite and 2.0-3.0 g of nickel sulfate hexahydrate, dissolving the sodium succinate, the dimethyl ammonia borane, the sodium hypophosphite and the nickel sulfate hexahydrate in 80-120 mL of deionized water, magnetically stirring to form a uniform solution, placing the uniform solution in a water bath at 8-12 ℃, soaking the filter paper obtained in the step 2 as a substrate into the substrate, reacting for 0.5-1.5 h, sequentially washing the obtained product with deionized water and anhydrous ethanol, forming amorphous divalent nickel on the surface of the substrate through chemical plating, and forming a small amount of boron and phosphorus to obtain the conductive cellulose filter paper.
And step 4, weighing 12-20 mg of ruthenium chloride hydrate and dissolving in 30mL of deionized water to form the electrodeposition solution. And (3) carrying out electrodeposition for 5-20 min by using a Chenghua CHI760E electrochemical workstation under a three-electrode system and by using a platinum electrode as a counter electrode, a saturated calomel electrode as a reference electrode and the material obtained in the step (3) as a working electrode under the condition that the applied voltage is-0.6 to-1.2V. And washing the obtained product with deionized water and absolute ethyl alcohol in sequence, and drying at 60 ℃ to obtain the conductive cellulose filter paper loaded Ru nanoparticle composite OER catalyst.
Example 1
The preparation method of the conductive cellulose filter paper loaded Ru nanoparticle composite OER catalyst comprises the following steps:
step 1, cutting qualitative filter paper into 1 x 2cm 2 Placed in deionized water, sonicated for 20min, then the filter paper was transferred to acetone, soaked for 3h, and dried at room temperature.
And 2, repeatedly immersing the dried filter paper into 0.2M nickel sulfate and the prepared 0.6M sodium borohydride solution, washing the filter paper by using deionized water and absolute ethyl alcohol after 3 times of immersion, and drying the filter paper at room temperature.
And 3, weighing 1.5g of anhydrous sodium sulfate, 2.5g of sodium succinate, 0.72g of dimethyl ammonia borane, 0.094g of sodium hypophosphite and 2.5g of nickel sulfate hexahydrate, dissolving in 100mL of deionized water, magnetically stirring to form a uniform solution, placing in a water bath at 10 ℃, soaking the filter paper obtained in the step 2 as a substrate in the uniform solution, reacting for 1h, and washing the obtained product with deionized water and anhydrous ethanol.
And 4, weighing 16mg of ruthenium chloride hydrate solution into 30mL of deionized water to form the electrodeposition solution. And (3) performing electrodeposition for 10min by using a Chenghua CHI760E electrochemical workstation under a three-electrode system and by using a platinum electrode as a counter electrode, a saturated calomel electrode as a reference electrode and the material obtained in the step (3) as a working electrode under the condition that the applied voltage is-0.6V. The obtained product is washed by deionized water and absolute ethyl alcohol and dried at 60 ℃.
Example 2
The preparation method of the conductive cellulose filter paper loaded Ru nanoparticle composite OER catalyst comprises the following steps:
step 1, cutting qualitative filter paper into 1 x 2cm 2 Placed in deionized water, sonicated for 20min, then the filter paper was transferred to acetone, soaked for 3h, and dried at room temperature.
And 2, repeatedly immersing the dried filter paper into 0.2M nickel sulfate and the prepared 0.4M sodium borohydride solution, washing the filter paper by using deionized water and absolute ethyl alcohol after 3 times of immersion, and drying the filter paper at room temperature.
And 3, weighing 1.5g of anhydrous sodium sulfate, 2.5g of sodium succinate, 0.72g of dimethyl ammonia borane, 0.094g of sodium hypophosphite and 2.5g of nickel sulfate hexahydrate, dissolving in 100mL of deionized water, magnetically stirring to form a uniform solution, placing in a water bath at 10 ℃, soaking the filter paper obtained in the step 2 as a substrate in the uniform solution, reacting for 1h, and washing the obtained product with deionized water and anhydrous ethanol.
And 4, weighing 16mg of ruthenium chloride hydrate solution into 30mL of deionized water to form the electrodeposition solution. And (3) performing electrodeposition for 10min by using a Chenghua CHI760E electrochemical workstation under a three-electrode system and by using a platinum electrode as a counter electrode, a saturated calomel electrode as a reference electrode and the material obtained in the step (3) as a working electrode under the condition that the applied voltage is-0.8V. The obtained product is washed by deionized water and absolute ethyl alcohol and dried at 60 ℃.
As shown in FIG. 1, it can be seen that the cellulose surface is wrapped by the nanoparticles to give the cellulose filter paper good conductivity, which is about 40 s/cm. (ii) a
As shown in FIG. 2, it can be seen that the amorphous divalent nickel coated on the surface of the cellulose is nanospheres with a size of 200-500 nm, and ruthenium nanoparticles with smaller size are distributed on the surface of the divalent nickel.
As shown in fig. 3, the XRD spectrum of example 2 can be seen, which shows a characteristic peak of cellulose at 22.8 ° and a characteristic peak of amorphous Ni at 46.4 °, and no characteristic peak of Ru is found, indicating that the introduction of Ru does not change the crystallization property of the conductive cellulose.
As shown in FIG. 4, the polarization curve of example 2, 100mA/cm, can be seen 2 Corresponding to 1.6V, 1.6-1.23V is 0.37V, so the current density of the anodic oxygen evolution reaction can be driven to reach 100mA/cm by only 370mV of overpotential 2 Thus showing that the catalyst has excellent electrocatalytic performance.
Example 3
The preparation method of the conductive cellulose filter paper loaded Ru nanoparticle composite OER catalyst comprises the following steps:
step 1, cutting qualitative filter paper into 1 x 2cm 2 Placed in deionized water, sonicated for 20min, then the filter paper was transferred to acetone, soaked for 3h, and dried at room temperature.
And 2, repeatedly immersing the dried filter paper into 0.15M nickel sulfate and the prepared 0.5M sodium borohydride solution, washing the filter paper by using deionized water and absolute ethyl alcohol after immersing for 4 times, and drying the filter paper at room temperature.
And 3, weighing 1.0g of anhydrous sodium sulfate, 2.0g of sodium succinate, 0.70g of dimethyl ammonia borane, 0.090g of sodium hypophosphite and 2.0g of nickel sulfate hexahydrate, dissolving the materials in 80mL of deionized water, magnetically stirring the materials to form a uniform solution, placing the uniform solution in a water bath at the temperature of 8 ℃, immersing the filter paper obtained in the step 2 as a substrate in the uniform solution, reacting for 1.5h, and washing the obtained product with deionized water and anhydrous ethanol.
And 4, weighing 12mg of ruthenium chloride hydrate solution in 30mL of deionized water to form the electrodeposition solution. And (3) performing electrodeposition for 10min by using a Chenghua CHI760E electrochemical workstation under a three-electrode system and by using a platinum electrode as a counter electrode, a saturated calomel electrode as a reference electrode and the material obtained in the step (3) as a working electrode under the condition that the applied voltage is-1.0V. The obtained product is washed by deionized water and absolute ethyl alcohol and dried at 60 ℃.
Example 4
The preparation method of the conductive cellulose filter paper loaded Ru nanoparticle composite OER catalyst comprises the following steps:
step 1, cutting qualitative filter paper into 1 x 2cm 2 Placed in deionized water, sonicated for 20min, then the filter paper was transferred to acetone, soaked for 3h, and dried at room temperature.
And 2, repeatedly immersing the dried filter paper into 0.2M nickel sulfate and the prepared 0.6M sodium borohydride solution, washing the filter paper by using deionized water and absolute ethyl alcohol after 3 times of immersion, and drying the filter paper at room temperature.
And 3, weighing 1.5g of anhydrous sodium sulfate, 2.5g of sodium succinate, 0.72g of dimethyl ammonia borane, 0.094g of sodium hypophosphite and 2.5g of nickel sulfate hexahydrate, dissolving in 100mL of deionized water, magnetically stirring to form a uniform solution, placing in a water bath at 10 ℃, soaking the filter paper obtained in the step 2 as a substrate in the uniform solution, reacting for 1h, and washing the obtained product with deionized water and anhydrous ethanol.
And 4, weighing 16mg of ruthenium chloride hydrate solution into 30mL of deionized water to form the electrodeposition solution. And (3) performing electrodeposition for 5min by using a Chenghua CHI760E electrochemical workstation under a three-electrode system and by using a platinum electrode as a counter electrode, a saturated calomel electrode as a reference electrode and the material obtained in the step (3) as a working electrode under the condition that the applied voltage is-0.8V. The obtained product is washed by deionized water and absolute ethyl alcohol and dried at 60 ℃.
Example 5
The preparation method of the conductive cellulose filter paper loaded Ru nanoparticle composite OER catalyst comprises the following steps:
step 1, cutting qualitative filter paper into 1 x 2cm 2 Placed in deionized water, sonicated for 20min, then the filter paper was transferred to acetone, soaked for 3h, and dried at room temperature.
And 2, repeatedly immersing the dried filter paper into 0.2M nickel sulfate and the prepared 0.5M sodium borohydride solution, washing the filter paper by using deionized water and absolute ethyl alcohol after immersing for 4 times, and drying the filter paper at room temperature.
And 3, weighing 1.5g of anhydrous sodium sulfate, 2.5g of sodium succinate, 0.72g of dimethyl ammonia borane, 0.094g of sodium hypophosphite and 2.5g of nickel sulfate hexahydrate, dissolving in 100mL of deionized water, magnetically stirring to form a uniform solution, placing in a water bath at 10 ℃, soaking the filter paper obtained in the step 2 as a substrate in the uniform solution, reacting for 1h, and washing the obtained product with deionized water and anhydrous ethanol.
And 4, weighing 16mg of ruthenium chloride hydrate solution into 30mL of deionized water to form the electrodeposition solution. And (3) performing electrodeposition for 15min by using a Chenghua CHI760E electrochemical workstation under a three-electrode system and by using a platinum electrode as a counter electrode, a saturated calomel electrode as a reference electrode and the material obtained in the step (3) as a working electrode under the condition that the applied voltage is-1.2V. The obtained product is washed by deionized water and absolute ethyl alcohol and dried at 60 ℃.
Example 6
The preparation method of the conductive cellulose filter paper loaded Ru nanoparticle composite OER catalyst comprises the following steps:
step 1, cutting qualitative filter paper into 1 x 2cm 2 Placed in deionized water, sonicated for 20min, then the filter paper was transferred to acetone, soaked for 3h, and dried at room temperature.
And 2, repeatedly immersing the dried filter paper into 0.35M nickel sulfate and the prepared 0.4M sodium borohydride solution, washing the filter paper by using deionized water and absolute ethyl alcohol after 5 times of immersion, and drying the filter paper at room temperature.
And 3, weighing 2.0g of anhydrous sodium sulfate, 3.0g of sodium succinate, 0.74g of dimethyl ammonia borane, 0.098g of sodium hypophosphite and 3.0g of nickel sulfate hexahydrate, dissolving in 120mL of deionized water, magnetically stirring to form a uniform solution, placing in a water bath at 12 ℃, soaking the filter paper obtained in the step 2 as a substrate in the uniform solution, reacting for 0.5h, and washing the obtained product with deionized water and anhydrous ethanol.
And 4, weighing 20mg of ruthenium chloride hydrate solution into 30mL of deionized water to form the electrodeposition solution. And (3) performing electrodeposition for 20min by using a Chenghua CHI760E electrochemical workstation under a three-electrode system and by using a platinum electrode as a counter electrode, a saturated calomel electrode as a reference electrode and the material obtained in the step (3) as a working electrode under the condition that the applied voltage is-0.8V. The obtained product is washed by deionized water and absolute ethyl alcohol and dried at 60 ℃.
The catalyst performance characterization in the above examples is to be understood as being illustrative of the present invention and not limiting, and appropriate modifications and improvements within the meaning and range of equivalents may be made by those skilled in the art and are intended to be included within the scope of the present invention.

Claims (9)

1. The preparation method of the conductive cellulose filter paper loaded Ru nanoparticle composite catalyst is characterized by comprising the following steps of:
sequentially immersing qualitative filter paper into a nickel sulfate solution and a sodium borohydride solution, and then cleaning and drying to obtain the cellulose filter paper loaded with the nickel simple substance;
soaking the cellulose filter paper loaded with the nickel simple substance into a mixed solution A of anhydrous sodium sulfate, sodium succinate, dimethyl ammonia borane, sodium hypophosphite and nickel sulfate for 0.5-1.5 h, and then cleaning and drying to obtain conductive cellulose filter paper;
taking conductive cellulose filter paper as a working electrode, performing electrodeposition for 5-20 min at-0.6 to-1.2V by using an aqueous solution of ruthenium chloride in a three-electrode system, and drying an obtained product after cleaning to obtain the conductive cellulose filter paper loaded Ru nanoparticle composite catalyst.
2. The preparation method of the conductive cellulose filter paper-supported Ru nanoparticle composite catalyst according to claim 1, wherein the qualitative filter paper is subjected to ultrasonic treatment in deionized water, then transferred to acetone for dipping, dried and then dipped in a nickel sulfate solution and a sodium borohydride solution.
3. The preparation method of the conductive cellulose filter paper supported Ru nanoparticle composite catalyst according to claim 1, wherein the concentration of the nickel sulfate solution is 0.15-0.35M.
4. The preparation method of the conductive cellulose filter paper supported Ru nanoparticle composite catalyst according to claim 1, wherein the concentration of the sodium borohydride solution is 0.4-0.6M.
5. The preparation method of the conductive cellulose filter paper loaded Ru nanoparticle composite catalyst according to claim 1, wherein the qualitative filter paper is sequentially and circularly immersed into a nickel sulfate solution and a sodium borohydride solution, and is cleaned after being circulated for 3-5 times.
6. The method for preparing the conductive cellulose filter paper supported Ru nanoparticle composite catalyst according to claim 1, wherein the cleaning in the step is washing with deionized water and absolute ethyl alcohol in sequence.
7. The preparation method of the conductive cellulose filter paper supported Ru nanoparticle composite catalyst according to claim 1, wherein the ratio of anhydrous sodium sulfate, sodium succinate, dimethyl ammonia borane, sodium hypophosphite, nickel sulfate and deionized water in the mixed solution A is (1.0-2.0) g: (2.0-3.0) g: (0.70-0.74) g: (0.090-0.098) g: (2.0-3.0) g: (80-120) mL.
8. The preparation method of the conductive cellulose filter paper-supported Ru nanoparticle composite catalyst according to claim 1, wherein the cellulose filter paper loaded with the nickel simple substance is immersed in the mixed solution A at a temperature of 8-12 ℃.
9. The conductive cellulose filter paper-supported Ru nanoparticle composite catalyst obtained by the preparation method of the conductive cellulose filter paper-supported Ru nanoparticle composite catalyst according to any one of claims 1 to 8.
CN202110566503.5A 2021-05-24 2021-05-24 Conductive cellulose filter paper loaded Ru nanoparticle composite catalyst and preparation method thereof Active CN113308710B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110566503.5A CN113308710B (en) 2021-05-24 2021-05-24 Conductive cellulose filter paper loaded Ru nanoparticle composite catalyst and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110566503.5A CN113308710B (en) 2021-05-24 2021-05-24 Conductive cellulose filter paper loaded Ru nanoparticle composite catalyst and preparation method thereof

Publications (2)

Publication Number Publication Date
CN113308710A CN113308710A (en) 2021-08-27
CN113308710B true CN113308710B (en) 2022-08-09

Family

ID=77374285

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110566503.5A Active CN113308710B (en) 2021-05-24 2021-05-24 Conductive cellulose filter paper loaded Ru nanoparticle composite catalyst and preparation method thereof

Country Status (1)

Country Link
CN (1) CN113308710B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116083952B (en) * 2023-03-28 2023-06-13 西南石油大学 Cu (copper) alloy 3 Ti nano-sheet loaded Ti-doped CuO/Ru hydrogen evolution reaction catalyst and preparation method thereof

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB201416062D0 (en) * 2014-09-11 2014-10-29 Univ The Glasgow Hydrogen generation
JP6889446B2 (en) * 2016-09-09 2021-06-18 デノラ・ペルメレック株式会社 Manufacturing method of anode for alkaline water electrolysis and anode for alkaline water electrolysis
EP3296431A1 (en) * 2016-09-15 2018-03-21 Ecole Polytechnique Fédérale de Lausanne (EPFL) Method of synthesis of an electrode for use as a catalyst of oxygen evolution reaction
CN110280271B (en) * 2019-06-06 2022-09-09 中南林业科技大学 Preparation method of OER composite electrocatalyst
JP2021012863A (en) * 2019-07-08 2021-02-04 正視 後藤 Power generation system using oxygen extracted from water
CN111129522A (en) * 2019-12-06 2020-05-08 同济大学 Preparation and application of nickel-iron alloy/nitrogen-doped carbon fiber serving as zinc-air battery oxygen electrocatalyst
CN112609205B (en) * 2020-11-30 2021-10-26 陕西科技大学 Nitrogen-doped carbon fiber loaded zirconium-induced transition metal phosphide and preparation method thereof

Also Published As

Publication number Publication date
CN113308710A (en) 2021-08-27

Similar Documents

Publication Publication Date Title
CN108080034B (en) Preparation method and application of nickel-based three-dimensional metal organic framework catalyst
CN110711596B (en) Efficient full-hydrolysis water catalyst IPBAP/Ni2P@MoOx/NF and preparation method thereof
CN112108163A (en) Preparation of CoFe-LDH nanosheet coated CoP nanowire core-shell nano array water oxidation electrocatalyst
CN109433234B (en) Nickel-iron phosphide/carbon nanotube composite material and preparation method and application thereof
CN109321933B (en) Preparation method and application of MOF/carbon dot nanocomposite catalyst
CN113652707B (en) Nickel telluride hydrogen evolution catalyst and preparation method and application thereof
CN112791736A (en) WP2/Cu3Application of P composite nano-structure catalyst in aspect of hydrogen production by electrolyzing water
CN112853374B (en) Nickel-iron oxygen evolution electrochemical catalyst for seawater electrolysis and preparation method and application thereof
CN112808274A (en) High-performance iron-doped nickel or cobalt-based amorphous oxyhydroxide catalyst prepared by room temperature method and research on efficient water electrolysis hydrogen production thereof
CN112481656B (en) Bifunctional catalyst for high-selectivity electrocatalysis of glycerin oxidation conversion to produce formic acid and high-efficiency electrolysis of water to produce hydrogen, preparation method and application thereof
CN113957456A (en) Nickel-based alkaline electrolytic water catalyst with co-doped combination heterostructure and preparation method thereof
CN111841598B (en) S-doped Co @ NC composite material with high oxygen evolution catalytic activity and preparation method thereof
CN113308710B (en) Conductive cellulose filter paper loaded Ru nanoparticle composite catalyst and preparation method thereof
CN109876846B (en) Three-dimensional self-supporting Cu3Preparation method of PNW @ CoFeP composite material
CN109926095B (en) Cobalt-based oxygen evolution catalyst based on eutectic solvent, preparation method and electrocatalytic oxygen evolution application thereof
CN109097788B (en) Double-carbon coupling transition metal nickel-based quantum dot electrocatalyst and preparation method thereof
CN114045509B (en) Seawater electrolysis device with sodium ion conduction and application thereof
CN113368878B (en) MnCoP catalyst, preparation and application
CN109402654A (en) A kind of MoS with substrate protective function2/Ni3Se2Compound Electrocatalytic Activity for Hydrogen Evolution Reaction agent and preparation method thereof
CN114622243A (en) Fe-doped Ni3S2Preparation method and application of electrode material
CN110227467B (en) Three-layer coaxial oxygen production electrocatalyst and preparation method thereof
CN114164451A (en) Phosphide heterogeneous nanosheet and preparation method thereof
CN113774425A (en) Preparation method and application of Ru-modified FeCo @ NF electrocatalyst
CN111118564A (en) Nickel-nickel oxide ultrathin nanosheet material and electrodeposition preparation method and application thereof
CN113026049B (en) Two-step solvothermal method for preparing NiFe (CN)5NO-Ni3S2-NF composite catalyst and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant