In-situ sulfur-doped mesoporous carbon supported palladium metal catalyst, and preparation method and application thereof

A metal catalyst, sulfur doping technology, applied in catalyst activation/preparation, metal/metal oxide/metal hydroxide catalyst, amino compound preparation, etc., can solve the problems of poor stability, poor selectivity, easy loss and so on , to achieve the effect of less catalyst dosage, long service life, not easy to agglomerate and run off

Inactive Publication Date: 2019-12-13
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, traditional Pd / C catalysts have problems such as poor selectivity and poor stability in the selective hydrogenation of halogenated aromatic nitro compounds to prepare halogenated aromatic amines.
Therefore, solving the problems of high activity, poor selectivity, easy loss or agglomeration of Pd / C catalyst is of great significance for the industrial production of halogenated aromatic amines

Method used

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  • In-situ sulfur-doped mesoporous carbon supported palladium metal catalyst, and preparation method and application thereof
  • In-situ sulfur-doped mesoporous carbon supported palladium metal catalyst, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] According to the ratio of about S to glucose mass ratio of 0.02:1, weigh 10g glucose and dissolve it in 60mL deionized water, add 0.7677g KHSO 3 , after dissolving, transferred to 150mL tetrafluoroethylene liner, placed in a sealed high-pressure hydrothermal kettle at 180°C for 30 hours, then cooled to room temperature, filtered, and the filter cake was vacuum-dried at 40°C for 15 hours to obtain preliminary carbonization in situ doped carbon materials. Subsequently, in an inert atmosphere, the temperature was raised to 700°C at a heating rate of 3°C / min, and roasted at a high temperature for 3 hours to obtain an in-situ sulfur-doped carbon material;

[0036] Palladium metal was supported by ultrasonic-assisted method. According to the palladium loading of 0.02wt%, the in-situ sulfur-doped carbon material prepared above was mixed evenly with 0.001g / mL palladium acetate aqueous solution, and ultrasonically treated for 5min at room temperature with ultrasonic power of 15...

Embodiment 2

[0038] According to the ratio of S to glucose mass ratio of 0.05:1, weigh 10g glucose and dissolve it in 60mL deionized water, add 1.9263g KHSO 3 , after dissolving, transferred to 150mL tetrafluoroethylene liner, placed in a sealed high-pressure hydrothermal kettle, hydrothermally reacted at 200°C for 24h, then cooled to room temperature, filtered, and the filter cake was vacuum-dried at 60°C for 12h to obtain preliminary carbonization in situ doped carbon materials. Subsequently, in an inert atmosphere, the temperature was raised to 600°C at a heating rate of 3°C / min, and roasted at a high temperature for 4 hours to obtain an in-situ sulfur-doped carbon material;

[0039] Palladium metal was supported by ultrasonic-assisted method. According to the palladium loading of 0.05wt%, the in-situ sulfur-doped carbon material prepared above was uniformly mixed with 0.005g / mL chloropalladium acid aqueous solution, and ultrasonically treated for 10min at room temperature, with ultras...

Embodiment 3

[0041] According to the ratio of S to glucose mass ratio of 0.1:1, weigh 10g glucose and dissolve it in 60mL deionized water, add KHSO 3 3. 8250g, dissolved and transferred to 150mL tetrafluoroethylene liner, placed in a sealed autoclave, hydrothermally reacted at 300°C for 20h, then cooled to room temperature, filtered, and the filter cake was vacuum-dried at 80°C for 8h to obtain Preliminary carbonization of in situ doped carbon materials. Subsequently, in an inert atmosphere, the temperature was raised to 800°C at a heating rate of 3°C / min, and roasted at a high temperature for 2 hours to obtain an in-situ sulfur-doped carbon material;

[0042] Palladium metal was supported by ultrasonic-assisted method. According to the palladium loading of 0.1wt%, the in-situ sulfur-doped carbon material prepared above was uniformly mixed with 0.005g / mL sodium chloropalladate aqueous solution, and ultrasonically treated for 2min at room temperature, with ultrasonic power of 150W and ultr...

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Abstract

The invention provides an in-situ sulfur-doped mesoporous carbon supported palladium metal catalyst, and a preparation method and application thereof. A required carrier material is directly obtainedby adopting a method of direct hydrothermal carbonization and calcination for further carbonization, so that sulfur can be doped into a skeleton of a carbon material and exists in a more stable form.In the sulfur-doped activated carbon supported noble metal catalyst, a large number of defects generated by doping are more beneficial to stable combination of palladium metal nanoparticles and the carrier, and strong interaction between sulfur and metal ensures high stability of the catalyst, so that metal nanoparticles are not easily agglomerated or lost in a hydrogenation reaction process, andthe service life of the catalyst is prolonged. Through the catalyst, halogenated nitrobenzene can be completely converted in a selective hydrogenation reaction of the halogenated nitrobenzene, and thehalogenated aniline selectivity can achieve 99.9%. In addition, the use condition is mild, stability is good, the use amount of the catalyst is less, and the service life of the catalyst is long.

Description

[0001] (1) Technical field [0002] The invention relates to an in-situ sulfur-doped carbon material supported palladium catalyst, a preparation method thereof, and an application in liquid-phase hydrogenation reaction of halogenated nitrobenzene. [0003] (2) Background technology [0004] Halogenated anilines are extremely important organic intermediates, which are widely used in medicine, dyes and other fields. Selective hydrogenation of halonitrobenzenes is the main method for the preparation of haloanilines. The traditional preparation methods of haloaniline include metal reduction method, electrolytic reduction method, alkali sulfide reduction method, hydrazine hydrate reduction method, etc. Because these traditional preparation methods have many wastes, high energy consumption and unsatisfactory product quality, the relatively advanced and more environmentally friendly catalytic hydrogenation process has begun to receive widespread attention in recent years. Among them...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/02B01J23/44B01J37/08B01J37/02B01J37/10C07C209/36
CPCB01J27/02B01J23/44B01J37/10B01J37/084C07C209/365B01J37/0207C07C211/52
Inventor 张群峰周媛张超杰马磊卢春山丰枫吕井辉李小年
Owner ZHEJIANG UNIV OF TECH
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