MXene(Ti3C2)-loaded palladium catalyst and preparation method and application thereof

A palladium catalyst and loading capacity technology, which is applied in the direction of physical/chemical process catalysts, chemical instruments and methods, and the preparation of organic compounds, can solve pollution and other problems, and achieve the effects of simple operation, simple process flow, and low price

Active Publication Date: 2018-01-05
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the price of 4-methylguaiacol remains high, industrially developed 4-methylguaiacol with higher purity through the bromination and oxidation of p-cresol. The environment is highly polluted, so the industry urgently needs to develop a process route suitable for industrialization to expand the source of 4-methylguaiacol

Method used

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  • MXene(Ti3C2)-loaded palladium catalyst and preparation method and application thereof
  • MXene(Ti3C2)-loaded palladium catalyst and preparation method and application thereof
  • MXene(Ti3C2)-loaded palladium catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: loading is 5% MXene (Ti 3 C 2 ) The preparation method of supported palladium catalyst is as follows:

[0029] Weigh 3.0g of Ti 3 AlC 2 As the raw material, put it in a 50 mL polytetrafluoroethylene cannula, then add 30 mL of 40wt.% HF solution dropwise into the cannula under stirring, and etch at room temperature for 24 hours; the etched powder Rinse with a large amount of deionized water until neutral, then put it into a freeze dryer, set the temperature of the cold well at -40°C, and freeze-dry for 20 hours to obtain MXene (Ti 3 C 2 ), weigh the dried MXene (Ti 3 C 2 ) powder 2.0g and 0.213g of palladium acetate were placed in a 100mL round-bottomed flask, and an excess amount of deionized water was added under low-speed stirring, stirred at a low speed in an oil bath at 60°C, and immersed for 12 hours. Evaporate to dryness under reduced pressure at 55°C, then dry in vacuum at 60°C overnight, roast in a muffle furnace at 250°C for 3 hours to remo...

Embodiment 2

[0030] Embodiment 2: loading is 2% MXene (Ti 3 C 2 ) The preparation method of supported palladium catalyst is as follows:

[0031] Weigh 3.0g of Ti 3 AlC 2 As the raw material, put it in a 50 mL polytetrafluoroethylene cannula, then add 30 mL of 40wt.% HF solution dropwise into the cannula under stirring, and etch at room temperature for 24 hours; the etched powder Rinse with a large amount of deionized water until neutral, then put it into a freeze dryer, set the temperature of the cold well at -40°C, and freeze-dry for 20 hours to obtain MXene (Ti 3 C 2 ). Weigh the dried MXene (Ti 3 C 2 ) powder 2.0g and 0.085g of palladium acetate were placed in a 100mL round-bottomed flask, and an excess amount of deionized water was added under low-speed stirring, stirred at a low speed in an oil bath at 60°C, and immersed for 12 hours. Evaporate to dryness under reduced pressure at 55°C, then dry in vacuum at 60°C overnight, roast in a muffle furnace at 250°C for 3 hours to rem...

Embodiment 3

[0033] Get the MXene (Ti) prepared in Example 1 3 C 2 ) 0.0425g of palladium catalyst with a loading capacity of 5%, 67 mL of water, and 0.3g of vanillin were added to the reactor, and the air in the reactor was replaced by hydrogen for 5 times, then the temperature was set at 100°C, the pressure was 0.3 MPa, and the reactor was sealed. , stirring speed 900 rpm, reacted for 0.5h, cooled to room temperature with cold water, took out the reaction solution, filtered, the filter cake was used as a catalyst, and could be recycled and applied mechanically. Add 15 mL of ethyl acetate to the filtrate, fully extract and separate, and take the organic phase Atmospheric pressure distillation, take 200 ~ 220 ℃ distillate, get 4-methyl guaiacol. The results of gas chromatography-mass spectrometry analysis showed that the conversion rate of vanillin was 100%, and the selectivity of 4-methylguaiacol was 98%.

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Abstract

The invention discloses a MXene(Ti3C2)-loaded palladium catalyst and a preparation method and application thereof. The MXene(Ti3C2)-loaded palladium catalyst is prepared from a MXene(Ti3C2) carrier and palladium which is carried on the MXene(Ti3C2) carrier, the carried quantity of palladium accounts for 2-6 wt.% of the mass of the carrier, and the prepared MXene(Ti3C2)-loaded palladium catalyst isused for vanillic aldehyde catalytic hydrogenation to prepare 2-methoxy-4-methylphenol. According to the MXene(Ti3C2)-loaded palladium catalyst, after the palladium catalyst is carried, precious metal particles are small, the dispersity degree of the metal particles is high, the cost is low, the mechanical strength of the MXene(Ti3C2)-loaded palladium catalyst is good, and the stability of a catalytic cycle is good; the MXene(Ti3C2)-loaded palladium catalyst is used for the vanillic aldehyde catalytic hydrogenation to prepare 2-methoxy-4-methylphenol simply by using water as solvent of reaction, the cost is low, the preparation method is environmentally friendly, the toxicity is low, the yield of high, the technological processes are simple, and the operation is easy, which is conducive to industrial production; by using a gas chromatography mass spectrometer for qualitative and quantitive analysis, it is indicated that the conversion rate of vanillic aldehyde is 98%-100%, and the selectivity of 2-methoxy-4-methylphenol is 98%-100%.

Description

technical field [0001] The invention belongs to the technical field of material preparation, in particular to a kind of MXene (Ti 3 C 2 ) supported palladium catalyst and its preparation method and application, specifically a method for preparing 4-methylguaiacol by catalytic hydrogenation of vanillin. Background technique [0002] MXene material is a new type of two-dimensional material prepared by etching based on MAX ceramics. MAX phase (such as Ti 3 AlC 2 ) is a kind of ternary layered material, which has some characteristics of ceramics and metals, good thermal stability and oxidation resistance; it also has excellent thermal and electrical conductivity of metals. The MXene material obtained by etching is a two-dimensional material synthesized by using hydrofluoric acid to selectively etch away the Al in the MAX phase, and in order to show its similar structure to graphene (Graphene). named MXene. At present, it is mainly used in electrochemistry (supercapacitors,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/22C07C41/18C07C43/23
CPCY02P20/584
Inventor 王建国刘天柱张世杰韩冰冰周虎
Owner ZHEJIANG UNIV OF TECH
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