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Regeneration method for supported noble metal catalyst

A precious metal catalyst and supported technology, which is applied in the regeneration field of supported precious metal catalysts, can solve certain problems in stability control and amplification, no reports of industrial application, influence on catalyst stability, etc. Sulfur-containing impurities, the effect of reducing catalyst cost

Inactive Publication Date: 2018-05-08
SHENYANG RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Although the current patent literature reports that the noble metal catalyst regeneration method has certain effects, it only targets certain single specific hydrogenation reactions and corresponding deactivated noble metal catalysts, and fails to effectively solve the regeneration of noble metal catalysts for the hydrogenation of aromatic nitro compounds containing sulfonic acid groups. question
Patent CN 101817766A uses hydrogen peroxide for regeneration, which can oxidize low-valence sulfur adsorbed on the catalyst to high-valence sulfur, making it lose its "toxicity". However, long-term hydrogen peroxide treatment will also cause a certain degree of damage to the activated carbon carrier. Affect catalyst stability; patent CN 103191759 A adopts hot air method to regenerate Pd / C catalyst, and there may be certain problems in the stability control and amplification of the regeneration process
Patent CN 103657683 A realizes the effective regeneration of Pt / C catalyst through steps such as hydrogen peroxide oxidation, Soxhlet extraction, immersion reduction to replenish platinum, and then immersion to replenish zinc, but the process is relatively cumbersome and the treatment cost is high
In these three patents, although the regenerated catalyst can be used many times, there are no industrial application reports
In addition, the first two patents are limited to the regeneration of Pd / C catalysts, and the third is limited to the regeneration of Pt / C catalysts, which has limitations

Method used

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  • Regeneration method for supported noble metal catalyst
  • Regeneration method for supported noble metal catalyst
  • Regeneration method for supported noble metal catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] In a 2L hydrogenation autoclave, add 1400g of nitro T acid with a mass concentration of 20% and 0.28g of a Pd / C catalyst with a loading rate of 5%. Put on the autoclave, and use nitrogen and hydrogen to exhaust the air in the autoclave 3 times each , Fill with hydrogen, start stirring, and carry out hydrogenation reaction. The reaction temperature is 60°C and the pressure is 1.5MPa. Use a hydrogen mass flow meter to monitor the end of the reaction. When the hydrogen is not consumed, stop stirring, close the hydrogen inlet valve, cool down, discharge the residual gas in the kettle, open the kettle, the reaction mother liquor is filtered out of the catalyst, and the filtrate is analyzed by liquid chromatography. Calculate raw material conversion rate and product selectivity; the catalyst is directly used without any treatment. The results are shown in Table 1:

[0028] Table 1 Application of the catalyst in Example 1

[0029]

[0030]

Embodiment 2

[0032] Filter out the Pd / C catalyst from the reaction mother liquor in the above-mentioned embodiment set 9 and add all of it to a 100 mL autoclave, and then add 30 g of Na with a mass concentration of 0.25% 2 CO 3 Aqueous solution, put on the kettle to ensure that there is no leakage, first replace the air in the kettle with nitrogen three times, and then use CO 2 Replace the nitrogen in the kettle three times, and finally fill with CO with a total pressure of 0.8MPa and a volume ratio of 2:1 2 With O 2 Start stirring, heat to 140°C, and continue stirring at this temperature for 3.5 hours, turn off stirring and heating, wait to cool to room temperature, filter, and wash the filter cake with deionized water to neutral;

[0033] Transfer the catalyst treated in the above steps to a 50mL flask, add 20g of tetrahydrofuran solvent, stir, heat to 40°C, and add 0.8g N dropwise 2 H 4 .H 2 O, after dripping, continue to stir for 2.0h, filter, first wash with tetrahydrofuran, and then wash t...

Embodiment 3

[0038] The Pd / C catalyst in the reaction mother liquor of the set 9 of Example 2 was filtered out as described above, and the catalyst was regenerated using the same method as that of Example 2, and the regenerated catalyst was applied. The experimental method was the same as that of Example 1. The results are shown in Table 3:

[0039] Table 3 Application of the catalyst in Example 3

[0040]

[0041]

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Abstract

The invention relates to a catalyst, in particular to a regeneration method for a supported noble metal catalyst. According to the regeneration method, a deactivated supported noble metal catalyst isoxidized by a mixed gas of CO2 and O2, and then is reduced by a reducing agent in a tetrahydrofuran solvent after oxidation, so as to obtain the regenerated catalyst. The method has the advantages that the problems that an existing regeneration method for a noble metal catalyst for hydrogenation of a sulfonic-acid-group-containing aromatic nitro compound is poor in stability, industrial amplification is unfeasible, the application range is narrow and the like can be solved, meanwhile, the regeneration method can aim at deactivated noble metal catalysts corresponding to hydrogenation of varioussulfonic-acid-group-containing aromatic nitro compounds, in addition, the regeneration mode is efficient, the regenerated catalyst has relatively high activity and selectivity on the hydrogenation ofthe multiple sulfonic-acid-group-containing aromatic nitro compounds, the service life of the catalyst can be remarkably prolonged, the cost of the catalyst can be lowered, and the method has an industrial application prospect.

Description

Technical field [0001] The invention relates to a catalyst, in particular to a method for regenerating a supported precious metal catalyst. Background technique [0002] The hydrogenation of aromatic nitro compounds containing sulfonic acid groups is an important unit reaction in dye synthesis. Supported noble metal catalysts are usually used, which have the advantages of mild reaction conditions and good product quality. However, this type of catalyst is easy to deactivate in the hydrogenation process and is difficult to apply, which greatly increases the investment cost of the catalyst and hinders its industrial application. In order to avoid frequent replacement of the catalyst, it is necessary to regenerate the deactivated catalyst to restore its activity and realize multiple reuse, which can save costs and reduce waste emissions, and has good economic and environmental benefits. [0003] There are two main reasons for the deactivation of precious metal catalysts for hydrogena...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/42B01J23/44B01J23/96B01J38/12B01J38/52B01J38/64B01J38/70C07C303/22C07C303/32C07C309/46C07C309/47
CPCB01J23/42B01J23/44B01J23/96B01J38/12B01J38/52B01J38/64B01J38/70C07C303/22C07C303/32C07C309/47C07C309/46Y02P20/584
Inventor 鄢冬茂龚亚军闫士杰龚党生
Owner SHENYANG RES INST OF CHEM IND
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