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Preparation method of nano-iron catalyst for catalyzing hydrolysis and dehydrogenation of ammonia borane

A technology for catalyzing ammonia borane and nano-iron, which is applied in the field of hydrogen storage materials, can solve the problems of cumbersome methods, no high-efficiency catalytic performance of iron nano-particle catalysts, etc., and achieves the effects of high catalytic activity and excellent cycle stability.

Inactive Publication Date: 2019-04-26
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above catalysts are synthesized by first combining the metal salt with the carrier, then calcining the obtained sample in the air, and then introducing hydrogen into it for high-temperature reduction. This method is cumbersome and has not obtained an iron nanoparticle catalyst with high catalytic performance.

Method used

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  • Preparation method of nano-iron catalyst for catalyzing hydrolysis and dehydrogenation of ammonia borane
  • Preparation method of nano-iron catalyst for catalyzing hydrolysis and dehydrogenation of ammonia borane
  • Preparation method of nano-iron catalyst for catalyzing hydrolysis and dehydrogenation of ammonia borane

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take anhydrous ferrous chloride (0.5 mmol, 0.068 g) powder and place it in a 50 mL Schlenk reaction bottle, and carry out several pumping and ventilation of the reaction bottle at room temperature under a double-row tube to fill the reaction bottle with nitrogen, and add 10 mL The tetrahydrofuran stirred solution became white, and after ultrasonic dispersion for 10 min, continued stirring and added the reducing agent tetrahydrofuran borane solution (5 mL, c =1 mol / L), continue to sonicate for 30 min and stir the reaction overnight, the resulting black solid product is centrifuged and purified, and then washed with water for three times, and the black solid product obtained after washing is placed in a vacuum drying oven at 60 The nano-iron catalyst that catalyzes the hydrolytic dehydrogenation of ammonia borane was obtained by drying at ℃ overnight.

Embodiment 2

[0017] Take anhydrous ferric chloride (0.5 mmol, 0.081 g) powder and place it in a 50 mL Schlenk reaction flask, and carry out several pumping and ventilation of the reaction flask at room temperature under a double-row tube to fill the reaction flask with nitrogen, and add 10 mL of tetrahydrofuran Stir the solution to become white, and after ultrasonic dispersion for 10 min, continue to stir and add the reducing agent tetrahydrofuran borane solution (5 mL, c =1 mol / L), continue to sonicate for 30 min and stir the reaction overnight, the resulting black solid product is centrifuged and purified, and then washed with water for three times, and the black solid product obtained after washing is placed in a vacuum drying oven at 60 The nano-iron catalyst that catalyzes the hydrolytic dehydrogenation of ammonia borane was obtained by drying at ℃ overnight.

Embodiment 3

[0019] Anhydrous ferrous chloride (0.5 mmol, 0.068 g) powder was placed in a 50 mL Schlenk reaction flask, and the reaction flask was pumped and ventilated several times at 10 °C under a double row tube to fill the reaction flask with nitrogen, and 10 The stirred solution in mL tetrahydrofuran was white, and after ultrasonic dispersion for 10 min, continued stirring and added the reducing agent tetrahydrofuran borane solution (5 mL, c =1 mol / L), continue to sonicate for 30 min and stir the reaction overnight, the resulting black solid product is centrifuged and purified, and then washed with water for three times, and the black solid product obtained after washing is placed in a vacuum drying oven at 60 The nano-iron catalyst that catalyzes the hydrolytic dehydrogenation of ammonia borane was obtained by drying at ℃ overnight.

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Abstract

The invention discloses a preparation method of a nano-iron catalyst for catalyzing the hydrolysis and dehydrogenation of ammonia borane. The method comprises the following specific process: stirringa reducing agent, namely a borane complex, and ferric salt or ferrous salt for a reaction at 10-30 DEG C in the absence of water and oxygen by adopting a one-step chemical reduction method to obtain the nano-iron catalyst, wherein the borane complex is tetrahydrofuran borane THF.BH3 or dimethyl sulfoxide borane DMS.BH3, the ferric salt is ferric chloride, ferric sulfate or ferric nitrate, and theferrous salt is ferrous chloride, ferrous sulfate or ferrous nitrate. The nano-iron catalyst can be repeatedly used after catalyzing the hydrolysis and dehydrogenation of the ammonia borane. The nano-iron catalyst, provided by the invention, has higher catalytic activity than that of a similar iron-based catalyst obtained with a prior method, more effectively promotes the progress of the hydrolysis and dehydrogenation reaction of the ammonia borane, and has excellent cycle stability performance.

Description

technical field [0001] The invention belongs to the technical field of hydrogen storage materials, and in particular relates to a preparation method of a nano-iron catalyst that catalyzes the hydrolytic dehydrogenation of ammonia borane. Background technique [0002] The cleanest and most promising energy source today is hydrogen energy. With the rapid development of hydrogen energy, the primary task is to find safe and efficient hydrogen storage materials. Among the boron, nitrogen and hydrogen hydrogen storage materials that have been studied more, ammonia borane has attracted much attention due to its high hydrogen storage content (19.6% mass fraction), non-toxicity, stability at room temperature, and environmental friendliness. At room temperature, 1 mol of ammonia borane can be hydrolyzed under the action of a catalyst to produce 3 mol of hydrogen. Existing catalysts are mainly transition metal nanoparticles, including noble metals and non-noble metals. Noble metals ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/745B01J35/02C01B3/04B01J35/00
CPCC01B3/04B01J23/745C01B2203/1047B01J35/40Y02E60/36
Inventor 李慧珍张凯旋琚明月陈学年
Owner HENAN NORMAL UNIV