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Method for preparing alkynylated graphene supported nano-palladium catalyst compound hydrogen absorption material

A hydrogen absorbing material and nano-palladium technology, applied in the field of hydrogen absorbing, can solve the problems such as the reduction of hydrogen elimination and hydrogen control ability, and achieve the effects of reducing steric hindrance, increasing mutual contact probability, and wide application range

Active Publication Date: 2018-10-12
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since this material is an organic hydrogen absorber, when its hydrogen absorption reaches saturation, the material's ability to eliminate hydrogen and hold hydrogen will be greatly reduced.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Accurately weigh 30 mg of graphene oxide, add it to 40 mL of N,N-dimethylformamide, ultrasonically disperse for 1 hour, and transfer to a 100 mL three-necked flask after full dispersion. Under water bath stirring conditions, add 1.5 g of sodium hydroxide weighed into it. After 1 hour, add 0.15 g of bromopropyne to it and react at 60°C for 24 hours. After the reaction is completed, the reaction suspension is washed with N,N-dimethylformamide, ethanol, and deionized water, centrifuged, and dried in vacuum to obtain alkynylated graphene.

[0040] Weigh 0.1g alkynylated graphene product, disperse it in 30mL DMF solution, sonicate for 1h, add 0.16g palladium acetate aqueous solution (10%), stir for 3min, then slowly drop in hydrazine hydrate while stirring at high speed ( 0.089mmoL) aqueous solution (0.2mL) and sonicated for 30min, reacted at 45℃ for 30min, then centrifuged the reacted suspension, and finally washed with N,N-dimethylformamide, ethanol, and deionized water. The...

Embodiment 2

[0042] Accurately weigh 30 mg of nitrogen-doped graphene oxide, add it to 40 mL of N,N-dimethylformamide, ultrasonically disperse for 1 hour, and transfer to a 100 mL three-necked flask after being fully dispersed. Under water bath stirring conditions, add 1.5 g of sodium hydroxide weighed into it. After 1 hour, add 0.15 g of propargylamine to it, and react at 60°C for 24 hours. After the reaction, the reaction solution is washed with N,N-dimethylformamide, ethanol, deionized water, centrifuged, and vacuum dried to obtain alkynylated graphene.

[0043] Weigh 0.1g of alkynylated graphene product, disperse it in 30mL DMF solution, ultrasonically disperse for 1h, add 0.014g sodium tetrachloropalladate solution (10%), stir for 3min, then ultrasonicate for 30min, then slowly drip Freshly prepared sodium borohydride (0.0885mmoL) aqueous solution (0.2mL) and vigorously stirred for 5min, reacted at 80℃ for 15min, and then centrifuged the reacted suspension, and finally used N,N-dimethylf...

Embodiment 3

[0045] Accurately weigh 30 mg of graphene, add it to 40 mL of N,N-dimethylformamide, ultrasonically disperse for 1 hour, and transfer to a 100 mL three-necked flask after full dispersion. Under the condition of water bath stirring, add 4.5g 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride EDC and 0.4g 4-dimethylaminopyridine DMAP to it, after all dissolved , And then add 0.15g propynol to it, and react at room temperature for 24 hours. After the reaction, the reaction solution was washed with N,N-dimethylformamide, ethanol, and deionized water, centrifuged, and vacuum dried to obtain alkynyl graphene.

[0046] Weigh 0.1g alkynylated graphene product and dissolve it in 30mL DMF solution. After fully dissolving, add 0.020g palladium chloride aqueous solution (10%), stir for 3min, then slowly drop in citric acid while stirring at high speed Sodium (0.09mmoL) aqueous solution (0.2mL) was stirred vigorously for 5min, reacted at 100℃ for 10min, and then the reacted suspensi...

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Abstract

The invention discloses a method for preparing an alkynylated graphene supported nano-palladium catalyst compound hydrogen absorption material. The method comprises the steps of performing alkynylating modification for graphene and compounding the modified graphene with nano-palladium, so that the alkynylated graphene can be used as a hydrogenating reactant or a stabilizer and carrier of a nano-palladium catalyst, so that two-in-one of a solid organic reactant and a solid catalyst carrier in an inorganic two-dimensional material catalytic hydrogenation system can be realized, steric hindrancebetween the solid reactant and the catalyst can be reduced, the mutual contact probability can be increased, and a higher catalytic hydrogenation efficiency can be obtained; and after the material issaturated in hydrogen absorption, the barrier performance for hydrogen is superior to that of an organic hydrogen absorption material, and hydrogen and isotopes thereof can be well controlled to penetrate into the environment. The inorganic two-dimensional material serving as filler is added into a polymer, and can be used for improving the mechanical performance, thermal performance, barrier performance and the like of the polymer. The nitrogen absorption material belongs to an irreversible hydrogen absorption material, and can reduce the content of hydrogen to a relatively low level in a closed environment at normal temperature normal pressure.

Description

Technical field [0001] The invention relates to the field of hydrogen absorption, in particular to the field of hydrogen absorbing materials and their preparation, in particular to a preparation method of alkynyl graphene loaded nano-palladium catalyst composite hydrogen absorbing material. Background technique [0002] Hydrogen has strong permeability and can hydrogenate with hydrogenated metal materials to generate brittle hydrides, which will lead to plastic loss and delayed cracking of the material, which will affect its performance; at the same time, in a closed environment, hydrogen accumulation still exists Risk of burning and explosion. In addition, if the radionuclide tritium in hydrogen isotope leaks, it will cause potential harm to human health and the environment. Therefore, it is necessary to effectively control the hydrogen content in the system to avoid hydrogen enrichment, which is of great significance for maintaining the stability of the material structure and ...

Claims

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Application Information

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IPC IPC(8): B01J31/02B01J37/02B01J37/16C01B3/58
CPCC01B3/58B01J31/0201B01J31/0235B01J37/0207B01J37/16B01J35/393
Inventor 李迎军周元林李银涛
Owner SOUTHWEAT UNIV OF SCI & TECH
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