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Regeneration method of hydrogenation catalyst used for preparing aromatic amine antioxidant

A technology of hydrogenation catalyst and antioxidant, which is applied in the direction of catalyst regeneration/reactivation, chemical instruments and methods, physical/chemical process catalysts, etc. It can solve the problems of catalyst activity degradation, loss of active components, harsh reaction conditions, etc. Achieve the effects of reducing consumption costs, increasing application times, and mild conditions

Active Publication Date: 2019-05-03
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst is actually "borrowing" CO low-temperature shift catalysts such as B204 and C207 in the ammonia synthesis industry, and its main component is CuO-ZnO-Al 2 o 3 , its initial research and development and later evolution and development are not tailored for the preparation of aromatic amine rubber antioxidants, and it is even more difficult to match the characteristics of reductive alkylation reactions. The main problems are: (1) poor catalyst selectivity, The side reaction of ketone carbonyl hydrogenation is serious; (2) The low catalytic activity leads to harsh reaction conditions; (3) The loss of active components leads to serious "copper damage"
However, due to the high cost of noble metal-supported catalysts, their service life is directly related to the production cost of antioxidants
As the number of catalyst cycles increases, the catalyst activity continues to deteriorate, and the catalytic performance gradually decreases.

Method used

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  • Regeneration method of hydrogenation catalyst used for preparing aromatic amine antioxidant
  • Regeneration method of hydrogenation catalyst used for preparing aromatic amine antioxidant
  • Regeneration method of hydrogenation catalyst used for preparing aromatic amine antioxidant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1: the Pt / C catalyst regeneration of antioxidant IPPD preparation comprises the following steps:

[0027] (1) Disperse 1kg of the catalyst to be treated (denoted as Pt / C-1U, with an isoelectric point of 7.2) into 50kg of N-methylpyrrolidone to form a suspension, and transport it into the 2 In the replaced 100L regeneration kettle 1, heat up to 120°C for stirring and washing; after washing, the mixed material liquid is sent to a precision filter for filtration, and then 50kg of methanol is used to backflush the catalyst into the regeneration kettle 1, and the temperature is raised to 60°C for stirring again Wash and filter.

[0028] (2) Use 50kg of deionized water to recoil the catalyst to pre-use N 2 In the replaced 100L high-pressure regeneration kettle 2, the temperature was raised to 230°C for hydrothermal treatment; after the hydrothermal treatment, the mixed material liquid was sent to a precision filter for filtration to obtain the regenerated catalyst...

Embodiment 2

[0032] Embodiment 2: comparative experiment of regeneration method

[0033]Only the method of step (1) in Example 1 was used to wash and regenerate Pt / C-1U, and the treated catalyst was recorded as Pt / C-2R, and its isoelectric point was determined to be 7.

[0034] Perform performance evaluation on the regenerated Pt / C-2R: the evaluation experiment and analysis method are the same as in Example 1. The result is as follows.

[0035]

[0036] As can be seen from the experimental results in the table above, using the treated Pt / C-2R, after 6.2 hours of reaction, about 10% of 4-aminodiphenylamine was not converted, and the purity of the product by IPPD chromatographic analysis was only 88.7%. There is a slight improvement before, but the catalyst activity recovery effect is not obvious. It shows that the ideal regeneration effect cannot be achieved only by simple washing treatment.

Embodiment 3

[0038] The Pt / C-1U and Pt / C-1R before and after regeneration in Example 1 were respectively used as ketone-amine condensation reaction catalysts to evaluate the acid-catalyzed Schiff base formation performance: the molar ratio of acetone to 4-aminodiphenylamine was 5:1 , the mass ratio of catalyst dosage on dry basis to 4-aminodiphenylamine is 1:100, the reaction temperature is 90°C, and the kettle is replaced with nitrogen.

[0039] Samples were taken from the sampling port every 30 minutes, and the amount of Schiff base generated in the reaction solution was analyzed by gas chromatography. The specific analysis conditions were as follows: vaporization temperature 300°C, FID detector temperature 300°C, initial column temperature 80°C, initial column temperature The maintenance time is 2min, the heating rate is 15°C / min, the final column temperature is 300°C, the final column temperature is maintained for 5min, and the capillary column type is HP-5 (30m×0.32mm×0.25μm). Pt / C-1U...

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Abstract

The invention relates to the technical field of catalysts, and particularly discloses a regeneration method of a hydrogenation catalyst used for preparing an aromatic amine antioxidant. The method adopts a solvent having better solubility for macromolecular organic substances (polyanilines) which block catalyst pore channels as a hot detergent, and realizes the effects of cleaning coking and unblocking the pore channels; and the washed catalyst is further subjected to hydrothermal treatment to reconstitute weakly-acidic sites (mainly based on phenolic hydroxyl groups) on the carbon surface toeffectively restore acid catalytic performance of a ketoamine condensation reaction. The method provided by the invention has the characteristics of simple operation, mild conditions, environmental protection and high efficiency, the method does not destroy a structure of a carbon carrier and a loading state of active metal nanoparticles while unblocking the pore structure of the catalyst and reconstituting the acidic sites, and the treatment method is highly compatible with the characteristics of a ketoamine reductive amination reaction, and can effectively restore the activity of the catalyst.

Description

(1) Technical field [0001] The invention relates to the technical field of catalysts, in particular to a method for regenerating a hydrogenation catalyst used in the preparation of aromatic amine antioxidants. (2) Background technology [0002] Aromatic amine rubber antioxidant is an important rubber antioxidant category, mainly including IPPD, 6PPD, 7PPD, 77PD and many other varieties, widely used in rubber and tire industries. At present, aromatic amine rubber antioxidants are mainly produced from aromatic amine and aliphatic ketone through reductive amination reaction. In the production technology of traditional reductive amination method to prepare aromatic amine rubber antioxidants, copper-based catalysts are generally used as hydrogenation catalysts. The catalyst is actually "borrowing" CO low-temperature shift catalysts such as B204 and C207 in the ammonia synthesis industry, and its main component is CuO-ZnO-Al 2 o 3 , its initial research and development and late...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J38/52C07C209/78C07C211/54
CPCY02P20/584
Inventor 丁军委于文龙刘福胜程秋振单玉领于世涛
Owner QINGDAO UNIV OF SCI & TECH
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