Preparation method of hydrogen elimination material

A technology of hydrogen elimination and nanomaterials, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of poor hydrogen elimination effect and low hydrogen absorption capacity, reduce agglomeration, increase contact probability, and improve hydrogen elimination reaction rate. Effect

Active Publication Date: 2019-03-12

SOUTHWEAT UNIV OF SCI & TECH

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Problems solved by technology

The hydrogen absorbing materials prepared in the prior art have lo...

Abstract

The invention discloses a preparation method of a hydrogen elimination material. The method comprises the following steps: 1, oxidizing a carbon nanomaterial, and then activating and alkynylating to obtain an alkynylated carbon nanomaterial having a hydrogen storage function; 2, dispersing the alkynylated carbon nanomaterial in a solvent, adding a precious metal salt solution, heating and stirring; then, adding a reducing agent solution, and continuing to stir to obtain an alkynylated carbon nanomaterial-loaded nano-precious metal hydrogen elimination material. According to the preparation method, the carbon nanomaterial having a hydrogen storage function is firstly oxidized, and is then subjected to activation and alkynylation, so that the alkynylated carbon nanomaterial having the hydrogen storage function is obtained; the alkynylated carbon nanomaterial-loaded nano-precious metal hydrogen elimination material is then prepared by using an in-situ reduction method. In the alkynylatedcarbon nanomaterial-loaded nano-precious metal hydrogen elimination material, the carbon nanomaterial has the hydrogen storage function, and the nano-precious metal acts as a catalyst and can enable the unsaturated alkyne group to react with hydrogen at the normal temperature, so that a hydrogen elimination function is realized.

Application Domain

Other chemical processes

Technology Topic

SolventPrecious metal +11

Examples

Experimental program(13)

Example Embodiment

[0021] Example 1:

[0022] A preparation method of a hydrogen-eliminating material, comprising the following steps:

[0023] Step 1. By weight, add 1 part of carbon nanotubes to 200 parts of fuming nitric acid, stir and react for 3 hours at a temperature of 50°C, then add 30 parts of 4-ethynylaniline, 50 parts of barium nitrite and 2 parts of azo Diisobutyl cyanide, stirred at 150°C, condensed and refluxed for 5 hours, then diluted with distilled water, purified by centrifugation, washed 5 times with organic solvent, and dried under vacuum to obtain alkynylated carbon nanotubes; the centrifugal separation and purification The rotating speed is 10000r/min, the temperature is 15°C, and the time is 10min; the organic solvent used for the organic solvent washing is toluene; the vacuum drying conditions are: temperature 120°C, vacuum degree-0.05MPa, drying time 24 hours;

[0024] Step 2: Disperse 1 part of alkynyl carbon nanotubes in 20 parts of N,N-dimethylformamide by weight, add 5 parts of sodium chloroplatinate solution, and stir at a temperature of 100 ° C for 10 min; then add 3 parts of diethylenetriamine solution, continue to stir for 20min, to obtain alkynyl carbon nanotube-loaded nano-platinum hydrogen-eliminating material; the preparation method of the sodium chloroplatinate solution is: by weight, take 0.1 part of chloroplatinic acid Sodium is prepared by dissolving 5 parts of distilled water; the preparation method of the diethylenetriamine solution is as follows: by weight, 0.1 part of diethylenetriamine is dissolved in 3.0 parts of distilled water to prepare;

[0025] The hydrogen absorption performance test of the alkynyl carbon nanotube-supported nano-platinum hydrogen elimination material prepared in this example was carried out, and the hydrogen absorption capacity was 8.5 mol/kg.

Example Embodiment

[0026] Example 2:

[0027] A preparation method of a hydrogen-eliminating material, comprising the following steps:

[0028] Step 1. By weight, add 1 part of carbon nanotubes to 500 parts of fuming nitric acid, stir and react for 3 hours at a temperature of 50°C, and then add 50 parts of dimethylpropargylamine, 30 parts of sodium nitrite and 3 parts of isocyanide. Propylbenzene hydroperoxide, stirring at 150°C, condensing and refluxing for 5 hours, then diluting with distilled water, centrifuging and purifying, washing 5 times with an organic solvent, and vacuum drying to obtain alkynylated carbon nanotubes; the centrifugal separation The rotational speed of purification is 12000r/min, the temperature is 15°C, and the time is 10min; the organic solvent used for the organic solvent washing is xylene; the vacuum drying conditions are: temperature 120°C, vacuum degree-0.05MPa, drying time 24 Hour;

[0029] Step 2: Disperse 1 part of alkynyl carbon nanotubes in 30 parts of toluene by weight, add 4 parts of sodium chloroplatinate solution, stir at a temperature of 100 ° C for 10min; then add 2 parts of 1,4-butanedi amine solution, and continue stirring for 20 min to obtain alkynyl carbon nanotube-supported nano-platinum hydrogen-eliminating material; the preparation method of the sodium chloroplatinate solution is as follows: by weight, 0.1 part of sodium chloroplatinate is dissolved in 3 parts of distilled water prepared; the preparation method of the 1,4-butanediamine solution is as follows: by weight, 0.1 part of 1,4-butanediamine is dissolved in 2 parts of distilled water to prepare;

[0030] The hydrogen absorption performance of the alkynyl carbon nanotube-supported nano-platinum hydrogen-absorbing material prepared in this example was tested, and the hydrogen absorption capacity was 8.6 mol/kg.

Example Embodiment

[0031] Example 3:

[0032] A preparation method of a hydrogen-eliminating material, comprising the following steps:

[0033] Step 1. By weight, take 1 part of fullerene and add it to 300 parts of fuming sulfuric acid, stir and react for 5 hours at a temperature of 60 ° C, then add 50 parts of dimethylpropargyl amine, 30 parts of magnesium nitrite and 3 parts of bicarbonate. Nitriles were stirred at a temperature of 150°C, condensed and refluxed for 5 hours, then diluted with distilled water, purified by centrifugation, washed 5 times with an organic solvent, and dried in vacuo to obtain alkynylated fullerenes; the centrifugal separation The rotational speed of purification is 12000r/min, the temperature is 25°C, and the time is 10min; the organic solvent used for the organic solvent washing is xylene; the vacuum drying conditions are: temperature 100°C, vacuum degree -0.05MPa, drying time 24 Hour;

[0034] Step 2: Disperse 1 part of alkynylated fullerene in 50 parts of tetrahydrofuran by weight, add 5 parts of sodium chloroplatinate solution, and stir at a temperature of 100 ° C for 10min; then add 2 parts of stannous chloride solution, Continue to stir for 20 min to obtain alkynylated fullerene supported nano-platinum hydrogen-eliminating material; the preparation method of the sodium chloroplatinate solution is as follows: by weight, 0.1 part of sodium chloroplatinate is dissolved in 3 parts of distilled water to prepare; The preparation method of the stannous chloride solution is as follows: by weight, 0.1 part of stannous chloride is dissolved in 2 parts of distilled water to prepare.

[0035] The hydrogen absorption performance test of the alkynylated fullerene-supported nano-platinum hydrogen elimination material prepared in this example was carried out, and the hydrogen absorption capacity was 8.8 mol/kg.

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