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A kind of preparation method and application of bipyridyl ruthenium mof material

A bipyridine ruthenium and bipyridine technology, which is applied in the field of catalysts, can solve the problems of poor photocatalytic hydrogen production and achieve the effects of pore size tailorability, high porosity, and low requirements

Active Publication Date: 2021-06-22
CHONGQING TECH & BUSINESS UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The photocatalytic hydrogen production effect of existing metal organic framework materials is too poor. How to improve the existing metal organic framework materials so as to improve their photocatalytic hydrogen production effect is the research direction of those skilled in the art.

Method used

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  • A kind of preparation method and application of bipyridyl ruthenium mof material
  • A kind of preparation method and application of bipyridyl ruthenium mof material

Examples

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Effect test

Embodiment 1

[0024] Take 100mgZrCl 4 , 104mg biphenyl dicarboxylic acid (H 2 bpdc), 250 μL of glacial acetic acid dispersed in DMF (15 mL), sealed in a vial, and placed in an oven to maintain the temperature at 100 °C for 24 hours; after cooling to room temperature, the resulting solid was separated by centrifugation and washed with DMF and Methanol washed three times each, and then dried under vacuum to obtain the UIO-67MOF material.

Embodiment 2

[0026] (1) 780mg (3.76mmol) RuCl 3 .3H 2 O, 936mg (5.99mmol) bipyridine, 840mg (19.8mmol) LiCl in 5ml reagent grade DMF (dimethylformamide), heated at reflux at 110°C for 8h, during this period magnetic stirring; after the reaction mixture was reacted to room temperature , add 25ml of acetone and cool the resulting solution at 0°C overnight, filter to obtain a red to reddish-purple solution and dark green-black crystals; wash the solid with water first, then wash with ether, suction and then vacuum-dry to obtain solid A ;

[0027] (2) 320mg (0.66mmol) solid A, 203mg (0.84mmol) (2,2'-dipyridyl)-5,5'-dicarboxylic acid mixed in 20ml ethanol / water (v:v=1:1), in N 2 Reflux at 85°C for 12 hours, then concentrate with a rotary evaporator; then add methanol / diethyl ether mixture to the solid for recrystallization, then filter the solution and the solid with suction, and finally dry in vacuum to obtain solid B;

[0028] (3) 137.7mg hafnium chloride, 86.8mg biphenyl dicarboxylic aci...

Embodiment 3

[0031] (1) 780mg (3.76mmol) RuCl 3 .3H 2 O, 936mg (5.99mmol) bipyridine, 840mg (19.8mmol) LiCl in 5ml reagent grade DMF (dimethylformamide), heated at reflux at 110°C for 8h, during this period magnetic stirring; after the reaction mixture was reacted to room temperature , add 25ml of acetone and cool the resulting solution at 0°C overnight, filter to obtain a red to reddish-purple solution and dark green-black crystals; wash the solid with water first, then wash with ether, suction and then vacuum-dry to obtain solid A ;

[0032] (2) 320mg (0.66mmol) solid A, 203mg (0.84mmol) (2,2'-dipyridyl)-5,5'-dicarboxylic acid mixed in 20ml ethanol / water (v:v=1:1), in N 2 reflux at 85°C for 12 hours, then concentrate with a rotary evaporator; then add methanol / ether mixture to the solid for recrystallization, then filter the solution and the solid with suction, and finally dry in vacuum to obtain solid B;

[0033] (3) 100mgZrCl 4 , 86.8mg biphenyl dicarboxylic acid (H 2 bpdc), 60.8...

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Abstract

The invention discloses a preparation method and application of a bipyridine ruthenium MOF material. The preparation method of the bipyridyl ruthenium MOF material comprises the following steps: (1) Weighing RuCl 3 .3H 2 O, bipyridine and lithium chloride were dissolved in DMF reagent, heated to reflux, then added acetone to cool and filter to obtain solid A; (2) Combine solid A obtained in step (1) with (2,2'-bipyridine)-5 , 5'-dicarboxylic acid is mixed in ethanol / water solvent, concentrated under reflux, and then recrystallized to obtain solid B; (3) Disperse solid B, hafnium chloride, biphenyl dicarboxylic acid and glacial acetic acid obtained in step (2) In DMF, sealed in a reaction vessel and heated for reaction, then washed and dried to obtain the bipyridyl ruthenium MOF material. The bipyridyl ruthenium MOF material prepared by the invention can be used as a hydrogen production catalyst with high hydrogen production.

Description

technical field [0001] The invention relates to the field of catalysts, in particular to a preparation method and application of a bipyridyl ruthenium MOF material. Background technique [0002] With the rapid development of the economy, energy shortage and environmental problems have been paid more and more attention by people. As a clean, efficient, green and non-polluting energy, hydrogen energy is considered to be one of the most effective ways to solve energy and environmental problems. In the method of preparing hydrogen, it is an effective hydrogen production method to convert solar energy into hydrogen energy by using a solar light source and using semiconductor photocatalytic decomposition of water to produce hydrogen. [0003] Metal organic frameworks (MOFs) is a kind of porous material combined with organic and inorganic chemistry that has developed rapidly in recent years. It is a new type of porous material after graphene oxide and carbon nanotubes. MOFs is a ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00B01J31/22C01B3/04
CPCY02E60/36
Inventor 刘兴燕蒋瑶徐思俊唐镭
Owner CHONGQING TECH & BUSINESS UNIV