Preparation of a highly active and extremely low loading ruthenium catalyst ru@zif-8 and its application in catalytic hydrogenation

A ruthenium catalyst, catalytic hydrogenation technology, applied in the preparation of organic compounds, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve low activity, high loading capacity, poor stability, etc. problems, achieve good application prospects, simple preparation, and good stability

Active Publication Date: 2022-01-21
CHINA UNIV OF MINING & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional nickel and cobalt-based catalysts have low activity, while ruthenium and palladium-based catalysts prepared by impregnation method have high activity, but the loading capacity is generally high, the stability is poor and the cost is high, so it is difficult to realize conversion and application in industry

Method used

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  • Preparation of a highly active and extremely low loading ruthenium catalyst ru@zif-8 and its application in catalytic hydrogenation
  • Preparation of a highly active and extremely low loading ruthenium catalyst ru@zif-8 and its application in catalytic hydrogenation
  • Preparation of a highly active and extremely low loading ruthenium catalyst ru@zif-8 and its application in catalytic hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: Preparation of Ru@ZIF-8 catalyst

[0025] 0.3g ruthenium acetylacetonate (Ru(acac) 3 ) and 5g zinc nitrate hexahydrate (Zn(NO 3 ) 2 ·6H 2 O) The precursor was dissolved in 50 mL of methanol to obtain solution A. 10 g of 2-methylimidazole was dissolved in 60 mL of methanol to obtain solution B, and solution B was added to the above precursor solution A under vigorous stirring. Then, the mixed solution was stirred at room temperature for 24 h. The product obtained was centrifuged and washed with methanol until the solution was colorless. The solid product was dried under vacuum at 80 °C overnight and labeled as Ru(acac) 3 @ZIF-8. Subsequently, the prepared Ru(acac) 3 @ZIF-8 is placed in a tube furnace and heated to 900°C at a rate of 5°C / min. In nitrogen (N 2 ) atmosphere at 900°C for 3h, the tube furnace was naturally cooled to room temperature. The resulting powder, labeled as Ru@ZIF-8, was directly used as a catalyst without further treatment. ...

Embodiment 2

[0040] Embodiment 2: the catalytic reaction of benzyl phenyl ether (BPE)

[0041] (1) Put 50mg of the reaction substrate benzyl phenyl ether, 10mg of the catalyst Ru@ZIF-8 and 10mL of isopropanol into a 100mL stainless steel autoclave, seal it and pass in hydrogen to remove the residual air in the reactor;

[0042] (2) Continuously feed hydrogen or argon at room temperature to pressurize the reactor to 1MPa, then raise the temperature to the required reaction temperature, and stir the reaction for 2h at a vigorous stirring speed of 800rpm;

[0043](3) After the reaction, the reaction system was naturally cooled to room temperature and the pressure was released, the catalyst was removed by filtration, and the obtained organic phase was analyzed by GC-MS and GC.

[0044] The catalyst that comparative example 1-2 makes is carried out the catalytic reaction of benzyl phenyl ether respectively, and reaction condition is the same as embodiment 2, and product is analyzed simultaneous...

Embodiment 3

[0051] Example 3: C-O bond cleavage reactions of other lignin model compounds

[0052] (1) Put 50mg of reactants, 10mg of catalyst Ru@ZIF-8 and 10mL of isopropanol into a 100mL stainless steel autoclave, seal it and pass in hydrogen to remove the residual air in the reactor;

[0053] (2) Continue to feed hydrogen at room temperature to pressurize the reactor to 1MPa, then stir and react at a certain temperature for 2-7h, and the stirring speed is 800rpm;

[0054] (3) After the reaction, the reaction system was naturally cooled to room temperature and the pressure was released, the catalyst was removed by filtration, and the organic phase obtained was analyzed by GC-MS and GC. The results are shown in Table 3.

[0055] Table 3 C-O bond cleavage of different lignin model compounds on Ru@ZIF-8 catalyst

[0056]

[0057] Reaction conditions: (a) 190°C, 2h, (b) 230°C, 5h, (c) 250°C, 7h.

[0058] It can be seen from Table 3 that the catalyst Ru@ZIF-8 prepared by the present inv...

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Abstract

The invention discloses the preparation of a highly active and extremely low loading ruthenium catalyst Ru@ZIF‑8 and its application in catalytic hydrogenation. The catalyst uses ruthenium acetylacetonate as a precursor and synthesizes a highly active ruthenium catalyst by a carbonization reduction method Ru@ZIF‑8; when the catalyst uses isopropanol as a solvent, it can efficiently catalyze the hydrocracking of C‑O bonds of various reactants under mild conditions, the conversion rate of reactants is 100%, and the yield of products is high . The catalyst of the invention has simple preparation, low active metal ruthenium load, low cost and good application prospect.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, and relates to the preparation and application of a ruthenium catalyst, in particular to the preparation of a highly active and extremely low loading ruthenium catalyst Ru@ZIF-8 and its application in catalytic hydrogenation. Background technique [0002] Lignin contains a large number of natural phenolic biopolymers that can be used in the chemical industry to produce high value-added aromatics, fuels and other intermediates for sustainable chemicals. However, the presence of stable C-O bonds in the structure of biomass-derived model compounds such as lignin makes depolymerization difficult. The hydrogenolysis reaction of C-O bonds in aryl ethers is crucial for the reduction catalysis of biomass such as lignin, and it is still a difficult problem so far. The cleavage of C-O bonds in lignin structural units is well known, especially the catalytic hydrogenolysis reaction that has been...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/60C07C29/10C07C35/08C07C37/055C07C39/04
CPCB01J23/60C07C29/10C07C37/055C07C35/08C07C39/04Y02P20/52
Inventor 曹景沛江玮赵小燕解金旋赵亮张创
Owner CHINA UNIV OF MINING & TECH
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