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A kind of PDNI alloy nano-catalyst of ammonia borane water interpretation hydrogen and preparation method thereof

An alloy nanometer and alloy nanoparticle technology are applied in the field of titanium dioxide hollow sphere-supported PdNi alloy nanocatalyst and its preparation, and the field of catalyzing hydrolysis hydrogenation catalyst to achieve the effects of improving anti-toxicity, increasing loading and simple process

Active Publication Date: 2020-01-03
HUBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] According to literature research, in TiO 2 The study of loading PdNi alloy nanoparticles in hollow spheres and using them to catalyze the hydrolysis of ammonia borane has not been reported

Method used

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  • A kind of PDNI alloy nano-catalyst of ammonia borane water interpretation hydrogen and preparation method thereof
  • A kind of PDNI alloy nano-catalyst of ammonia borane water interpretation hydrogen and preparation method thereof
  • A kind of PDNI alloy nano-catalyst of ammonia borane water interpretation hydrogen and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1: TiO 2 Hollow sphere (TiO 2 HS), PdNi / TiO 2 Preparation of HS supported catalyst

[0030] (1) Weigh 1.8g of potassium titanium oxalate K 2 TiO(C 2 o 4 ) 2 2H 2 O, it is added in the beaker of 100mL, the deionized water of 37.5mL is added in the beaker, magnetic stirring is until forming colorless transparent solution. Then add 37.5mL H 2 o 2 and 5mL of hydrochloric acid, stirred for about 5min, then added to a 100mL stainless steel reaction kettle lined with polytetrafluoroethylene, reacted at 160°C for 12h, cooled naturally, filtered, washed, and dried under vacuum at 80°C overnight to obtain a titanium dioxide hollow ball (TiO 2 HS) white powder. where the H 2 o 2 The mass fraction of hydrochloric acid is 30%, and the mass fraction of said hydrochloric acid is 37%.

[0031] (2) Weigh 70.93mg of PdCl 2Add it into a small beaker containing a small amount of concentrated hydrochloric acid, stir at room temperature until the solid is completely...

Embodiment 2

[0035] Embodiment two: single metal load mixed type (Pd / TiO 2 HS+Ni / TiO 2 HS) catalyst preparation

[0036] Weigh 100mg of TiO prepared in the above-mentioned embodiment one 2 Add HS to 30mL deionized water, then add 2.5mL0.04mol / L H 2 PdCl 4 , after ultrasonication for 10 min, stirring was continued for 5 h to obtain a suspension. Then weigh 50.0 mg of reducing agent NaBH 4 The solid was dissolved in 10 mL of deionized water, and the solution was added dropwise to the above suspension to reduce the metal ions in the solution, and the stirring was continued for 3 h after the dropwise addition was completed. The product was filtered, washed, and vacuum dried overnight to yield Pd / TiO 2 HS catalyst.

[0037] Take by weighing the TiO of 100mg above-mentioned embodiment one 2 Add HS to 30mL deionized water, then add 1.5mL0.04mol / L Ni(NO 3 ) 2 ·6H 2 O, continue stirring for 5 h after ultrasonication for 10 min to obtain a suspension. Then weigh 50.0 mg of reducing agent...

Embodiment 3

[0039] Embodiment three: the preparation of unsupported PdNi nanoparticles

[0040] Measure 2.5mL 0.04mol / L H 2 PdCl 4 and 1.5mL 0.04mol / L Ni(NO 3 ) 2 ·6H 2 O was added to 30 mL of deionized water, and a uniformly dispersed solution was obtained after ultrasonication for 10 minutes. Then, 50.0 mg of NaBH 4 The solid was dissolved in 10 mL of deionized water, and the solution was added dropwise to the above solution, and stirring was continued for 3 h after the dropwise addition was completed. The product was filtered, washed, and vacuum-dried overnight at 80 °C to obtain the PdNi NPs catalyst.

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Abstract

The invention provides a titanium dioxide hollow sphere PdNi-loaded alloy nanometer catalyst as well as a preparation method and application thereof. The catalyst is prepared from an active ingredient and a carrier, wherein the active ingredient is PdNi alloy nanometer particles; the particle diameter of the PdNi alloy nanometer particles is 4.1 to 5.5nm; the carrier is a titanium dioxide hollow sphere; the diameter of the titanium dioxide hollow sphere is 2.1 to 3.0mu m, and the hole diameter is 0.33 to 0.5mu m. The specific surface area of the prepared catalyst disclosed by the invention is large; the PdNi alloy nanometer particles are embedded evenly inside and outside holes; the loading quantity is increased; the particle diameter of the PdNi alloy nanometer particles is small; the catalytic activity sites are many; the activity and the stability of the catalyst can be obviously improved; when the catalyst is used for hydrogen release through hydrolysis of ammonia borane, at room temperature, the maximum hydrogen release speed can reach 105.36mol H2min<-1>(mol Pd) <-1>; the reaction activation energy is 24.86kJ mol<-1>. The preparation method has the advantages that the process is simple; the raw materials are easily to obtain; the cost is low; the implementation is easy; the preparation method is suitable for industrial production; the application prospects are wide.

Description

technical field [0001] The invention relates to the technology of catalytic water-interpretation hydrogen catalyst, in particular to a PdNi alloy nano-catalyst supported by titanium dioxide hollow spheres and its preparation method and application, belonging to the field of hydrogen storage materials. Background technique [0002] Hydrogen energy is considered as a new type of clean energy and a green energy with broad application prospects. How to safely and efficiently produce and store hydrogen is a great challenge for researchers. In recent years, chemical hydrides have become the most promising hydrogen storage materials due to their high hydrogen content and low molecular weight. Among them, ammonia borane (NH 3 BH 3 , referred to as AB) has a low molecular weight (30.87g / mol) and a high mass hydrogen storage density (19.6wt%) and has become the most promising solid hydrogen storage material. Ammonia borane has stable performance and can be hydrolyzed to produce hyd...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/89C01B3/06
CPCB01J23/892C01B3/068C01B2203/1052C01B2203/1064C01B2203/1082Y02E60/36
Inventor 周立群李悦马浩宁红辉彭薇薇徐宏坤刘红英
Owner HUBEI UNIV