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Preparation method of alkynylated graphene-supported nano-palladium catalyst composite hydrogen-absorbing material

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

Active Publication Date: 2021-07-23
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 into 40 mL of N,N-dimethylformamide, ultrasonically disperse for 1 hour, transfer to a 100 mL three-neck flask after fully dispersed. Under the condition of stirring in a water bath, 1.5 g of sodium hydroxide weighed was added thereto, and after 1 hour, 0.15 g of propyne bromide was added thereto, and reacted at 60° C. for 24 hours. After the reaction, the reaction suspension was washed and centrifuged with N,N-dimethylformamide, ethanol, and deionized water, and vacuum-dried to obtain alkynylated graphene.

[0040] Take by weighing 0.1g alkynylated graphene product, be dispersed in 30mL DMF solution, ultrasonic 1h, then add the palladium acetate aqueous solution (10%) of 0.16g, stir 3min, then while stirring at a high speed, slowly drip hydrazine hydrate ( 0.089mmoL) aqueous solution (0.2mL) and sonicated for 30min, reacted at 45°C for 30min, then processed the reacted suspension by centrifugation, and finally washed the...

Embodiment 2

[0042] Accurately weigh 30 mg of nitrogen-doped graphene oxide, add to 40 mL of N,N-dimethylformamide, ultrasonically disperse for 1 hour, and transfer to a 100 mL three-necked flask after fully dispersed. Under the condition of stirring in a water bath, 1.5 g of sodium hydroxide weighed was added thereto, and after 1 hour, 0.15 g of propargylamine was added thereto, and reacted at 60° C. 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 the alkynylated graphene.

[0043]Weigh 0.1g of alkynylated graphene product, disperse in 30mL DMF solution, ultrasonically disperse for 1h, add 0.014g of sodium tetrachloropalladate aqueous solution (10%), stir for 3min, then treat with ultrasonic for 30min, then slowly drop into Freshly prepared sodium borohydride (0.0885mmoL) aqueous solution (0.2mL) was vigorously stirred for 5min, reacted at 80°C for 15min, and then treated t...

Embodiment 3

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

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

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Abstract

The invention discloses a method for preparing a composite hydrogen-absorbing material supported by alkynylated graphene supported by nano-palladium catalyst. The hydrogen reactant is used as the stabilizer and carrier of the nano-palladium catalyst to realize the two-in-one combination of the solid organic reactant and the solid catalyst carrier in the catalytic hydrogenation system of inorganic two-dimensional materials, and reduce the steric hindrance between the solid reactant and the catalyst , increase the probability of mutual contact, and obtain higher catalytic hydrogenation efficiency; and when the material reaches hydrogen absorption saturation, its barrier performance to hydrogen is better than that of organic hydrogen absorption materials, and it can well control the penetration of hydrogen and its isotopes into the environment. Such inorganic two-dimensional materials are added to polymers as fillers, which can improve the mechanical properties, thermal properties, and barrier properties of polymers. The hydrogen-absorbing material of the invention belongs to the irreversible hydrogen-absorbing material, and can reduce the hydrogen content in a closed environment under normal temperature and pressure to a relatively low level.

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, and in particular to a method for preparing a composite hydrogen-absorbing material supported by alkynylated graphene with a nano-palladium catalyst. Background technique [0002] Hydrogen has a strong penetrating ability, and can hydrogenate with hydrogenated metal materials to form brittle hydrides, which will lead to plastic loss and hysteresis cracking of materials, affecting their performance; at the same time, in a closed environment, the accumulation of hydrogen still exists. Fire and explosion hazard. In addition, once the radionuclide tritium in the 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 the enrichment of hydrogen, which is of great significance for maintaining ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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帅茂兵
Owner SOUTHWEAT UNIV OF SCI & TECH
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