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Production method and application of trisruthenium MOF material

A technology of ruthenium bipyridine and bipyridine, applied in the field of catalysts, can solve problems such as poor photocatalytic hydrogen production effect, and achieve the effects of great popularization value, low requirements and convenient operation.

Active Publication Date: 2019-06-07
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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  • Production method and application of trisruthenium MOF material
  • Production method and application of trisruthenium MOF material

Examples

Experimental program
Comparison scheme
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 which 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 acid (H ...

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 which 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 mg of...

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Abstract

The invention discloses a production method of a trisruthenium MOF material and application of the trisruthenium MOF material. The production method of the trisruthenium MOF material comprises the following steps of (1) weighing RuCl3.3H2O, dipyridyl and lithium chloride, dissolving the RuCl3.3H2O, the dipyridyl and the lithium chloride in a DMF agent, conducting heating reflux on a mixture, and then adding acetone for cooling and filtering to obtain solid A; (2) mixing the solid A obtained in the step (1) and 2,2'-bipyridine-5,5'-dicarboxylicacid in an ethyl alcohol / water solvent, and conducting reflux concentration and then recrystallization on a mixture to obtain solid B; and (3) dispersing the solid B Obtained in the step (2), hafnium tetrachloride, biphenyldicarboxylic acid and glacial acetic acid in DMF, sealing a mixture in a reaction kettle for heating reaction, and washing and drying a product to obtain the trisruthenium MOF material. The trisruthenium MOF material produced through the production method can be used as a hydrogen production catalyst, and the hydrogen production capability is high.

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 Applications(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