Regeneration method and application of chloronitro aromatic hydrocarbon selective hydrogenation catalyst

[0033] Embodiment 1: The 5w% Pt / C catalyst deactivated in the selective hydrogenation of o-chloronitrobenzene to prepare 2,2'-dichlorohydroazobenzene is regenerated, comprising the following steps:

[0034] (1) Take 10g of deactivated catalyst (referred to as Cat1-U) and disperse it into 50g of methanol solution containing 5% n-butyl titanate and 5% terephthalaldehyde, stir and impregnate at 50°C, and the impregnation is completed Afterwards, the catalyst was filtered and transferred to a tube atmosphere furnace under N 2 Under the protection of 2°C / min, the heating rate was increased to 500°C and then maintained for 2h for carbonization treatment. The product obtained after carbonization (denoted as N&Ti@Cat1-U) was cooled and stored for later use.

[0035] (2) Add 10g of N&Ti@Cat1-U and 250g of Cat1-U to a 10L regenerating kettle equipped with an ultraviolet light irradiation device and a microwave generating device, add 2.5kg of an aqueous solution containing 5% sodium pero...

[0049] Embodiment 2: The 3w% Pd / C catalyst deactivated in the selective hydrogenation of o-chloronitrobenzene to prepare 2,2'-dichlorohydroazobenzene is regenerated, comprising the following steps:

[0050] (1) Take 10g of deactivated catalyst (Cat2-U) and disperse it into 50g of methanol solution containing 15% n-butyl p-titanate and 15% terephthalaldehyde, and stir and impregnate it at 80°C. The catalyst was filtered and transferred to a tube atmosphere furnace under N 2 Under the protection of the temperature rising rate of 5 ℃ / min to 800 ℃ and then maintained for 2 hours for carbonization treatment, the product obtained after carbonization (denoted as N&Ti@Cat2-U) was cooled and stored for later use.

[0051] (2) Add 10g of N&Ti@Cat2-U and 300g of Cat2-U to a 10L regenerating kettle equipped with an ultraviolet light irradiation device and a microwave generating device, and add 3kg of an aqueous solution containing 5% potassium peroxodisulfate. The regeneration treatmen...

[0057] Embodiment 3: comparative experiment of regeneration method

[0058] (1) Add 250g of Cat1-U directly to a 10L regeneration kettle equipped with a UV irradiation device and a microwave generator, add 2.5kg of an aqueous solution containing 5% sodium peroxodisulfate, and irradiate it with ultraviolet light with a wavelength of 200nm Regeneration treatment is carried out under the action, the treatment temperature is 50°C, and the microwave power is 1000W. The processed material liquid is filtered by nitrogen pressure into the precision filter.

[0059] (2) Carry out subsequent regeneration experiments according to steps (3) and (4) of Example 1. Catalyst performance evaluation is carried out to the regenerated catalyst (referred to as Cat1-U-R1): evaluation method and analysis method are the same as embodiment 1. The result is as follows:

[0060]

[0061] As can be seen from the experimental results in the above table, compared with the catalyst regenerated in Examp...