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Method for preparing nanometer Pd electrocatalyst

An electrocatalyst and nanotechnology, applied in the field of electrocatalyst preparation, can solve the problems of difficult control of reaction conditions, difficult industrial production, uneven products, etc., achieve controllable shape and size, realize shape and size regulation, overcome Instruments and equipment require higher effects

Inactive Publication Date: 2013-01-16
ANHUI UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0007] However, there are still some imperfections in this technology at present, such as the stability of hybrids, the interaction between nanoparticles and templates, a large amount of reducing agent must be added in the preparation process, the reaction conditions in the preparation process are not easy to control, or the preparation process The use of ultrasonic, microwave or electrochemical workstations or high-energy radiation sources and other test conditions results in higher costs, uneven products and difficulties in industrial production, etc.

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  • Method for preparing nanometer Pd electrocatalyst
  • Method for preparing nanometer Pd electrocatalyst
  • Method for preparing nanometer Pd electrocatalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Embodiment 1: Preparation of nano-Pd electrocatalyst for 8h reaction in dark conditions

[0044] 1. Preparation of hexagonal lyotropic liquid crystals

[0045] Weigh 2.4013g sodium lauryl sulfate, 0.0374g NaCl, 0.103g PdCl 2 Mix with 6mL of water, heat up to 35°C under airtight conditions to dissolve, then add 8.88mL of cyclohexane dropwise under stirring, and then add 1.29mL of n-pentanol dropwise under stirring to obtain a stable gel, namely component A;

[0046] 2. Reduction of Pd salt precursor

[0047] Put component A in a dark box to react for 8 hours, and the yellow-brown stable gel reacts to dark brown to obtain component B;

[0048] 3. Post-processing

[0049] Add 10mL of isopropanol to component B to obtain a black suspension, ultrasonically disperse for 7min, centrifuge and wash for 30min, wash repeatedly 3 times, add 8mL of ethanol and disperse evenly, then put it in a vacuum oven at 40°C for 24h to obtain nano Pd electrocatalyst.

[0050] The microscop...

Embodiment 2

[0051] Embodiment 2: Preparation of nano-Pd electrocatalyst for 72h reaction under dark conditions

[0052] The preparation method of this example is the same as that of Example 1, except that in step 2, component A was reacted in a dark box for 72 hours to obtain component B.

[0053] The microscopic morphology of the nano-Pd electrocatalyst prepared in this example is as follows: figure 2 As shown, the particles have regular shapes such as quadrilaterals, pentagons, and decahedrons, and the particle size is 30-35nm. Compared with the microscopic shape and size of nano-Pd prepared by reacting for 8 hours, the regularity of the particles is significantly improved, and the size of the particles is also large. Significantly increased, indicating that with the extension of the reaction time, the morphology and size of nano-Pd can be regulated. The electrocatalytic activity of nano-Pd electrocatalysts for formaldehyde oxidation is as follows: Figure 6 As shown in (b), in the p...

Embodiment 3

[0054] Embodiment 3: the preparation of 40W incandescent lamp radiation 24h nanometer Pd electrocatalyst

[0055] 1. Preparation of hexagonal lyotropic liquid crystals

[0056] Weigh 0.8g sodium dodecyl sulfate (SDS), 0.012gNaCl, 0.01gPdCl 2 and 2mL of water in a reaction vessel, sealed and dissolved in a water bath at 35°C to obtain a yellow-brown viscous liquid, add 3mL of cyclohexane dropwise under magnetic stirring to obtain a yellow-brown unstable emulsion, and then add dropwise 0.43mL n-amyl alcohol, to obtain a translucent tan stable gel, component A;

[0057] 2. Reduction of Pd salt precursor

[0058] Put component A in a self-made light box, and use an incandescent lamp to irradiate and react for 24 hours. The wattage of the incandescent lamp is 40W. The yellow-brown stable gel reacts to dark brown, and component C is obtained;

[0059] 3. Post-processing

[0060] Add 10mL of isopropanol to component C to obtain a black suspension, ultrasonically disperse for 7min...

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Abstract

The invention discloses a method for preparing a nanometer Pd electrocatalyst. The method comprises a hexagonal phase lyotropic liquid crystal preparation process, a Pd salt precursor reduction process and a unit aftertreatment process; and the shape of the generated nanometer Pd can be regulated and controlled by changing reaction time, illumination intensity and the like. By the method, the shape and the size of the prepared nanometer Pd electrocatalyst can be controlled and regulated; nanometer Pd electrocatalysts with controllable sizes and shapes are obtained according to different reaction time and bulb power; and the method is suitable for preparing electro-catalysis formaldehyde and other organic small molecular electrocatalysts. The preparation method is mild in condition, simple in process, short in production period and uniform in product and makes the nanometer Pd electrocatalyst easily produced on a large scale.

Description

1. Technical field [0001] The invention relates to a method for preparing an electrocatalyst, in particular to a method for preparing a nanometer Pd electrocatalyst. 2. Background technology [0002] In recent years, the synthesis and characterization of inorganic nanocrystal clusters have received extensive attention. As a heterogeneous catalyst, nano-palladium (Pd) is widely used in industry for the synthesis of C–C bonds in Suzuki, Heck, and Stille coupling reactions and the hydrogenation of unsaturated hydrocarbons. Moreover, because nanoparticles have excellent properties such as large specific surface area, many surface active centers, and high catalytic efficiency, nanomaterials can be introduced into modified electrodes to study their application in the field of electrocatalysis. [0003] In the study of structure-activity relationship of nanocatalysts, the morphology-activity relationship is an advanced research topic. Studies have shown that the catalytic or elec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J37/03B22F9/24
Inventor 王艳丽谭德新张明旭彭勇军华龙杰吴天华方熙卫伟
Owner ANHUI UNIV OF SCI & TECH
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