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Regeneration method of Pd/C catalyst and application of regenerated Pd/C catalyst

A catalyst and reaction technology, applied in the field of regeneration of Pd/C catalyst, can solve problems such as easy combustion

Inactive Publication Date: 2013-07-10
ZHEJIANG UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, for activated carbon-supported catalysts, the activated carbon support will also be oxidized and easily combustible under high-temperature oxidation conditions, so activated carbon-supported catalysts cannot be regenerated by high-temperature oxidation, and no activated carbon-supported catalysts have ever been used. Published reports on regeneration by oxidation

Method used

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  • Regeneration method of Pd/C catalyst and application of regenerated Pd/C catalyst
  • Regeneration method of Pd/C catalyst and application of regenerated Pd/C catalyst
  • Regeneration method of Pd/C catalyst and application of regenerated Pd/C catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In the reaction of catalyzing the hydrogenation of m-nitrobenzenesulfonic acid to synthesize m-aminobenzenesulfonic acid, add 200g of industrial grade m-nitrobenzenesulfonic acid solution with a mass concentration of 60wt% in a 500mL autoclave, and use a mass concentration of 30wt % NaOH solution to adjust the pH to 7, and add 1g of 5wt% Pd / C catalyst. The hydrogenation reaction temperature is 75°C and the reaction pressure is 1MPa. Among them, the Pd / C catalyst is selected from fresh catalyst, catalyst recovered by filtration after reaction, and catalyst recovered by filtration after reaction and then regenerated by air oxidation. The catalyst regeneration method is as follows: the deactivated Pd / C catalyst is dried and oxidized under air atmosphere, the drying temperature is 120° C., and the drying time is 4 hours.

[0027]

[0028]

Embodiment 2

[0030] In the reaction of catalyzing the hydrogenation of m-nitrobenzenesulfonic acid to synthesize m-aminobenzenesulfonic acid, add 200g of industrial-grade m-nitrobenzenesulfonic acid solution with a mass concentration of 50wt% in a 500mL autoclave, and use a mass concentration of 20wt % KOH solution to adjust the pH to 6.5, add 1g3wt%Pd / C catalyst. The reaction temperature is 95° C., and the reaction pressure is 0.8 MPa. Among them, the Pd / C catalyst is selected from fresh catalyst, catalyst recovered by filtration after reaction, and catalyst recovered by filtration after reaction and then regenerated by air oxidation. The catalyst regeneration method is as follows: the deactivated Pd / C catalyst is dried and oxidized under air atmosphere, the drying temperature is 70° C., and the drying time is 10 h.

[0031]

Embodiment 3

[0033] In the reaction of catalyzing the hydrogenation of m-nitrobenzenesulfonic acid to synthesize m-aminobenzenesulfonic acid, add 200g of industrial-grade m-nitrobenzenesulfonic acid solution with a mass concentration of 55wt% in a 500mL autoclave, and use a mass concentration of 25wt % NaOH solution to adjust the pH to 7, and add 1g of 5wt% Pd / C catalyst. The reaction temperature is 85° C., and the reaction pressure is 1 MPa. Among them, the Pd / C catalyst is recovered by filtration after the reaction, and then regenerated by air oxidation to continue to be used in the next reaction. The catalyst regeneration method is as follows: the deactivated Pd / C catalyst is dried and oxidized under the air atmosphere, the drying temperature is 110° C., and the drying time is 8 hours. A total of 80 applied experiments were carried out, wherein a small amount of fresh catalyst was added after every several reactions.

[0034]

[0035]

[0036]

[0037]

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Abstract

The invention discloses a regeneration method of a Pd / C catalyst and an application of the regenerated Pd / C catalyst. The Pd / C catalyst is inactivated due to poisoning by sulfur-containing substances during the process of catalyzing the hydrogenation synthesis of m-aminobenzenesulfonic acid from m-nitrobenzenesulfonic acid; and the regeneration method comprises the steps of drying and oxidizing the inactivated Pd / C catalyst in an air atmosphere at the temperature of 50-140 DEG C to obtain the regenerated Pd / C catalyst. The Pd / C catalyst obtained by regeneration according to the regeneration method disclosed by the invention can be applied to the reaction of catalyzing the hydrogenation synthesis of the m-aminobenzenesulfonic acid from the m-nitrobenzenesulfonic acid. The method disclosed by the invention is environment-friendly and pollution-free, can effectively restore the activity of the Pd / C catalyst which is inactivated due to the positioning of the sulfur-containing substances during the process of catalyzing the hydrogenation synthesis of the m-aminobenzenesulfonic acid from the m-nitrobenzenesulfonic acid, can ensure that the catalyst can be mechanically used for more than 80 times in a circulating manner, and can keep the activity of the catalyst and the selectivity of the target product unchanged.

Description

(1) Technical field [0001] The invention relates to a method for regenerating a Pd / C catalyst. More specifically, it relates to a process of catalyzing the hydrogenation of m-nitrobenzenesulfonic acid to synthesize m-aminobenzenesulfonic acid. A small amount of sulfur-containing organic compounds in the industrial raw material m-nitrobenzenesulfonic acid poison the Pd / C catalyst. Active regeneration method; In addition, the present invention also relates to the application of the regenerated Pd / C catalyst in the reaction of catalyzing m-nitrobenzenesulfonic acid hydrogenation to synthesize m-aminobenzenesulfonic acid. (2) Background technology [0002] Palladium-carbon (Pd / C) catalysts have excellent catalytic performance in (liquid phase) hydrogenation reactions, and are widely used in the synthesis of petrochemicals, pharmaceuticals, and agrochemicals. However, during these reactions, deactivation of Pd / C catalysts is often observed due to poisons, carbon (or organic mole...

Claims

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Application Information

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IPC IPC(8): B01J23/96C07C309/46C07C303/22
CPCY02P20/584
Inventor 李小年张群峰丰枫卢春山李良梁秋霞徐铁勇马磊朱秀全
Owner ZHEJIANG UNIV OF TECH
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