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Inorganic-organic core-shell framework loaded low-dose precious metal palladium material and preparation thereof and application in electro-catalytic dechlorination hydrogenation reaction

A low-dose, precious metal technology, applied in electrolytic organic production, electrodes, electrolysis process, etc., can solve the problems of thermodynamic instability of precious metal nanoparticles, reducing effective reactive sites, reducing reaction efficiency, etc., to achieve high activity per unit mass, Atomic economy, the effect of reducing usage

Active Publication Date: 2021-12-28
ZHEJIANG UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the thermodynamic instability of noble metal nanoparticles, they are easy to agglomerate into large particles during the preparation process, reducing the effective reactive active sites and reducing the reaction efficiency, resulting in low activity per unit mass. The current highest mass activity of the catalyst is 8.5min -1 g -1 So, inventing a highly dispersed low-dose noble metal catalyst is the key to realize the industrialization of dechlorination by electrocatalytic reduction

Method used

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  • Inorganic-organic core-shell framework loaded low-dose precious metal palladium material and preparation thereof and application in electro-catalytic dechlorination hydrogenation reaction
  • Inorganic-organic core-shell framework loaded low-dose precious metal palladium material and preparation thereof and application in electro-catalytic dechlorination hydrogenation reaction
  • Inorganic-organic core-shell framework loaded low-dose precious metal palladium material and preparation thereof and application in electro-catalytic dechlorination hydrogenation reaction

Examples

Experimental program
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Effect test

Embodiment 1

[0035] 1. Preparation of TiO with nano-array structure 2 vertical nanorods. Immerse the FTO conductive glass into the hydrochloric acid aqueous solution of tetrabutyl titanate (the content of tetrabutyl titanate is 2.8%, and the solvent is 37wt% hydrochloric acid aqueous solution), react with hydrothermal reaction at a constant temperature of 150°C for 5 hours, then wash it, and keep it in the air at a constant temperature of 450°C. Calcined for 3h to prepare FTO / TiO 2 Material. figure 2 For FTO / TiO 2 From the SEM image, it can be seen that TiO 2 It has a one-dimensional nanorod array structure and grows vertically on the surface of FTO. The average diameter of the nanorods is about 160nm.

[0036] 2. FTO / TiO 2 Preparation of @PDA. The above FTO / TiO 2 placed vertically containing 1.21g L -1Tris-HCl and 0.5gL -1 In the dopamine solution, stir at a constant temperature of 15°C for 12 hours, then wash with deionized water, and dry to obtain FTO / TiO 2 @PDA. image 3 In...

Embodiment 2

[0043] 1. FTO / TiO 2 Preparation of Vertical Nanorods. The preparation method and process are the same as in Example 1, and TiO with an array structure is vertically grown on the FTO surface. 2 One-dimensional nanorods.

[0044] 2. FTO / TiO 2 Preparation of @PDA. The preparation method and process are the same as in Example 1, except that the concentration of dopamine is 1.0 g L -1 , the resulting FTO / TiO 2 The thickness of the polydopamine thin layer of the one-dimensional nanorod is 12.15 nm, which is higher than 5.23 nm in Example 1.

[0045] 3. FTO / TiO 2 Preparation of @PDA / Pd. The preparation method and process are the same as in Example 1, except that the carrier adopts FTO / TiO with a polydopamine layer thickness of 12.15nm 2 @PDA, the resulting FTO / TiO 2 The particle size of palladium nanoparticles on @PDA / Pd is about 2.0nm, and the loading of Pd is calculated to be 0.60%.

[0046] 4. With FTO / TiO 2 The @PDA / Pd material is used as the cathode for electrocatalyt...

Embodiment 3

[0048] 1. Preparation of cathode materials. The preparation method and process are the same as in Example 1, and the results obtained are the same as in Example 1.

[0049] 2. With FTO / TiO 2 The @PDA / Pd material is used as the cathode for electrocatalytic dechlorination and hydrogenation of 3,6-dichloropicolinic acid. H-type electrode reaction tank is used, N117 cationic membrane is used to separate the cathode and anode electrolyte, the anode is made of graphite rod material, and the cathode is made of FTO / TiO prepared above. 2 @PDA / Pd material. The electrolyte in the anode reaction tank is sodium hydroxide buffer solution (pH=10); the catholyte is 1mmol L -1 3,6-dichloropicolinic acid solution, adjust its pH to 10.0 with sodium hydroxide buffer. The electrolyte was kept at 30°C in a water bath, and the electrolysis current was controlled at 5.0mA cm -2 , electrolyzed for 4 hours under constant stirring.

[0050] The high-performance liquid chromatography is used for d...

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Abstract

The invention discloses an inorganic-organic core-shell framework loaded low-dosage precious metal palladium material and preparation thereof and application of the material in electro-catalytic dechlorination hydrogenation reaction. The preparation method comprises the following steps: polymerizing dopamine around a TiO2 one-dimensional nanorods which vertically grow on the surface of FTO and have an array structure by utilizing an in-situ auto-polymerization effect of the dopamine to form an inorganic-organic core-shell structure of TiO2 nanorod wrapped by the dopamine; and uniformly dispersing and loading an extremely low amount of palladium nanoparticles on the core-shell framework by adopting a chemical impregnation method to obtain an electrode material, wherein the loading capacity of precious metal palladium in the electrode material is only 0.29%, when the electrode material is used as a cathode to be applied to electro-catalysis of a dechlorination reaction of a chlorinated organic compound, the mass activity reaches up to 44.39 min<-1>g<-1>, the conversion rate of dechlorination of the chlorinated organic compound can reach up to 94%, very high electro-catalytic reaction activity is shown, and a relatively large application prospect is achieved in electro-catalytic hydrodechlorination.

Description

technical field [0001] The invention relates to a low-dose noble metal electrode material loaded with an inorganic-organic core-shell framework and its preparation method and application, in particular to a TiO 2 @PDA is a carrier-loaded low-dose metal palladium electrode material and its preparation method, as well as its application in electrocatalytic dechlorination and hydrogenation reactions. Background technique [0002] Chlorinated organic compounds (chlorophenol, polychlorpyralid, polychlorinated biphenyls, etc.) are widely used in chemical, pharmaceutical, pesticide and other fields. Chlorinated organic compounds have the characteristics of high toxicity, persistence, and bioaccumulation. It is extremely difficult to transform through biodegradation, and improper disposal can easily lead to pollution of water bodies, soil and groundwater systems. Therefore, how to effectively dispose of chlorinated organic pollutants is an urgent problem related to the long-term de...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B11/054C25B11/069C25B11/081C25B3/01C25B3/25C03C17/36
CPCC25B11/054C25B11/069C25B11/081C25B3/01C25B3/25C03C17/36C03C17/3649
Inventor 赵浙菲俞丽郑华均
Owner ZHEJIANG UNIV OF TECH
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