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Preparation method of composite hydrogen-absorbing material supported by alkyne-rich polymer supported nano-palladium catalyst and hydrogen-absorbing material

A polymer-loaded, hydrogen-absorbing material technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of reduced hydrogen elimination performance and difficulty in fully contacting and other issues to achieve the effect of improving hydrogen absorption efficiency

Active Publication Date: 2018-09-04
MATERIAL INST OF CHINA ACADEMY OF ENG PHYSICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to: the existing DEB and DPB and other hydrogen elimination materials are often used in solid form and belong to the gas-solid hydrogenation system. In practical applications, these hydrogen elimination materials are directly or mixed with powder It is used after secondary compounding with other materials, and the alkyne-containing reactants (DEB and DPB, etc.) and the carbon black-supported catalyst Pd are in a static state, and it is difficult to achieve sufficient contact between the solid reactant and the catalyst Pd, making it dehydrogenate To solve the problem of performance degradation, a method for preparing a composite hydrogen-absorbing material supported by an alkyne-rich polymer supported nano-palladium catalyst and the hydrogen-absorbing material thereof are provided

Method used

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  • Preparation method of composite hydrogen-absorbing material supported by alkyne-rich polymer supported nano-palladium catalyst and hydrogen-absorbing material
  • Preparation method of composite hydrogen-absorbing material supported by alkyne-rich polymer supported nano-palladium catalyst and hydrogen-absorbing material
  • Preparation method of composite hydrogen-absorbing material supported by alkyne-rich polymer supported nano-palladium catalyst and hydrogen-absorbing material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Example 1 Preparation of Alkyne Functionalized Polyvinyl Alcohol

[0052] Under the protection of nitrogen, 20 mL DMF and 1.0648 g PVA (20 mmol) were added into a three-necked flask, stirred in an oil bath at 85 °C until the PVA was completely dissolved, cooled to room temperature, and placed under N 2 Under protection, add 3.243 g CDI (20 mmol) and react at room temperature for 3 h; then, add 1.54 mL propargylamine (24 mmol) to the three-necked flask and react at room temperature for 20 h; then slowly pour the reaction solution in the three-necked flask into a container Stir in a beaker with 100 mL of ethanol solution until all the product is precipitated, repeatedly wash with ethanol solution, filter, and vacuum-dry the filter residue for 24 h to constant weight to obtain a white flocculent solid.

[0053] The results of structural confirmation are as follows: 1 H NMR (400 MHz, DMSO) δ 4.73 (m, 1H), 4.4-4.37 (m, 1H), 3.75 (s, 2H), 3.03 (s, 1H), 1.97-1.93 (m, 3H), 1.7...

Embodiment 2

[0054] Example 2 Preparation of Alkyne Functionalized Polyacrylic Acid

[0055] Add 1.44 g of PAA (20 mmol) into a three-necked flask containing 20 mL of DMF, stir for 2 h, heat until PAA is completely dissolved, and cool to room temperature; then, add 4.6 g of EDCI and 1.46 g of DMAP to the three-necked flask, After stirring for a period of time, add 1.54 mL of propargylamine (24 mmol), and after stirring for 20 h, stop the reaction to obtain a reaction solution; concentrate the prepared reaction solution to about 8 mL, pour it into a solution containing 100 mL of dichloromethane , stirred until all the products were precipitated, washed repeatedly with acetone and dichloromethane solutions, filtered, and the filter residue was vacuum-dried for 24 h to constant weight to obtain a yellow solid.

[0056] The results of structural confirmation are as follows: 1 H NMR (300 MHz, DMSO) δ3.31(s, 2H), 2.99(s, 1H), 2.56(s, 1H), 1.74-1.77(m, 2H); 13 C NMR (300 MHz, DMSO) δ169.82, 79....

Embodiment 3

[0057] Example 3 Preparation of Alkyne-rich Polyvinyl Alcohol-supported Nano Palladium Catalyst Composite Hydrogen Absorbing Material

[0058] Weigh 0.5 g of alkyne-functionalized polyvinyl alcohol product and dissolve it in 50 mL of DMF solution. After fully dissolving, add 0.0651 g (0.2212 mmoL) of sodium tetrachloropalladate aqueous solution (5 mL) and stir for 3 min; then While stirring at a high speed, a fresh sodium borohydride (0.4425 mmol) aqueous solution (0.5 mL) was slowly added dropwise and stirred vigorously for 5 min to obtain a tan alkyne-rich PVA-PdNPs suspension.

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Abstract

The invention discloses a preparation method of an alkyne-rich polymer supported nano palladium catalyst compound hydrogen absorption material and a prepared hydrogen absorption material and aims at solving the problems that an existing hydrogen eliminating material is used in a solid-state form, sufficient contact of a solid-state reactant and a catalyst Pd is difficult to realize in practical application and the hydrogen eliminating performance is reduced. The preparation method disclosed by the invention has the advantages that firstly alkyne-rich polymers are synthesized and then are compounded with nano palladium, so that the alkyne-rich polymers can serve as a hydrogenation reactant and also can serve as a stabilizer and a carrier of the nano palladium catalyst, two-in-one of a solid-state organic reactant and a solid-state catalyst carrier in a catalytic hydrogenation system is realized by controlling reaction conditions, the steric hindrance between the solid-state reactant and the catalyst is effectively reduced, the mutual contact probability is increased, and the higher catalytic hydrogenation efficiency can be obtained; and the prepared hydrogen absorption material belongs to an irreversible hydrogen absorption material, the hydrogen content in a closed environment at normal temperature and normal pressure can be reduced to a lower level, and a new material and a new method for controlling hydrogen are provided for the field of hydrogen elimination.

Description

technical field [0001] The invention relates to the field of hydrogen elimination, in particular to the field of hydrogen elimination materials and their preparation, in particular to a preparation method of a composite hydrogen absorption material supported by an alkyne-rich polymer loaded with nano-palladium catalyst and the hydrogen absorption material. Background technique [0002] Hydrogen has a strong penetrating ability, and can hydrogenate with hydrogenated metal materials to form brittle hydrides, which will lead to the loss of plasticity and hysteresis cracking of materials. At the same time, in a closed environment, the accumulation of hydrogen also presents the danger of combustion and explosion. In a nuclear power plant, if a coolant loss failure occurs, a large amount of hydrogen will be released and enter the containment of the nuclear power plant; if no corresponding measures are taken, the hydrogen content in the containment atmosphere will gradually increas...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/06C01B3/58
CPCB01J31/06C01B3/58
Inventor 帅茂兵常凤雯黄德顺赵鹏翔杨晓娇岳国宗朱婧
Owner MATERIAL INST OF CHINA ACADEMY OF ENG PHYSICS
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