Production of lactams and carboxylic acid amides by beckman rearrangement of oximes in the presence of nb catalysts

A technology of Beckmann rearrangement and catalyst, which is applied in the field of preparing lactam and carboxylic acid amide through Beckmann rearrangement of oxime in the presence of Nb catalyst, which can solve the problems of salt pollution, catalyst deactivation, etc.

Inactive Publication Date: 2012-03-21
DSM IP ASSETS BV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] The main problem of the above-mentioned method in the presence of B-MFI catalyst is that after about 2 hours of reaction time, the catalyst starts to deactivate because carbonaceous spe

Method used

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  • Production of lactams and carboxylic acid amides by beckman rearrangement of oximes in the presence of nb catalysts
  • Production of lactams and carboxylic acid amides by beckman rearrangement of oximes in the presence of nb catalysts
  • Production of lactams and carboxylic acid amides by beckman rearrangement of oximes in the presence of nb catalysts

Examples

Experimental program
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Embodiment 1

[0065] Example 1: Catalyst A

[0066] SiO 2 The Nb on the support is prepared by the impregnation method. The catalyst is synthesized by the following method: DAVICAT SP 550-10021 (surface area = ~ 300m 2 / g) is used as a silica carrier. By using NbCl 5 Impregnation to prepare Nb / SiO 2 . During its preparation, first add an appropriate amount of NbCl 5 Dissolve in 100ml isopropanol. Add 10g SiO to this solution 2 Carrier material. The mixture obtained therefrom was stirred at 110°C until the isopropanol had evaporated. After impregnation, the sample was dried at 110°C for 4 hours and calcined in an air stream at 400°C for 4 hours.

Embodiment 2

[0067] Example 2: Catalyst B

[0068] SiO 2 -Al 2 O 3 The Nb on the support material was prepared by the same synthesis method as in Example 1. In this embodiment, SiO 2 -Al 2 O 3 (60:40) SASOL SIRAL-40 (BET area = 520m 2 / g) is used as a carrier material.

Embodiment 3

[0069] Example 3: Catalyst C

[0070] TiO 2 The Nb on the support material was also prepared by the impregnation method as in Example 1, except that TiO 2 Instead of SiO 2 As a carrier material. Hombicat II type from Sachtleben company is used as TiO 2 Source, its BET surface area is m 2 / g.

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Abstract

The present invention relates to processes for the production of lactams such as e-Caprolactam, w-Laurolactam, or of carboxylic acid amides such as acetaminophenol and benzanilide by Beckman rearrangement from the corresponding oximes in the presence of Nb-impregnated catalysts, such as Nb on SiO2, preferably in the gaseous phase but also in the liquid phase. The reactions in the gaseous phase can be performed in various reactors, such as fixed bed reactors, plate reactors, fluidized bed reactors, fluidized bed reactors having continuous regeneration in a second fluidized bed at temperatures between 200 DEG C and 500 DEG C and a pressure of 0.01 bar to 10 bar. In the liquid phase, the reactions can take place in different reactors such as autoclaves, stirred reactors, loop reactors, and trickle bed reactors at temperatures from 20 DEG C to 200 DEG C and a pressure between 0.5 and 20 bar. The invention further relates to the method of regeneration of said Nb-containing catalysts in oxidizing and non-oxidizing media at 200 DEG C to 600 DEG C.

Description

Technical field [0001] The present invention relates to a catalyst impregnated with Nb (such as SiO 2 In the presence of Nb) above, the preparation of lactams such as ε-caprolactam and ω-laurolactam or acetaminophen (acetaminophen with analgesic effect) and The method of the carboxylic acid amide of benzanilide, which is preferably carried out in the gas phase, but can also be carried out in the liquid phase. [0002] In addition, the present invention describes a method for regenerating these Nb-containing catalysts in oxidizing media and non-oxidizing media at 200°C to 600°C. Background technique [0003] Nb-containing materials show extraordinary activity in the heterogeneous catalysis process, and can also be used to synthesize fine chemicals (Chem. Rev., 99 (1999) 3603-3624, Cat. Today 8 (1990) 1). The patent (US 5618512) further discloses that niobium-containing zeolites can be used for the oxidation of hydrocarbons (such as olefins). [0004] In Journal of Catalysis 260 (200...

Claims

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Application Information

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IPC IPC(8): C07D201/04C07C231/10
CPCC07D201/04C07C231/10
Inventor 沃尔夫冈·郝尔德里奇阿尼库玛·麦图耐瑞博尔·斯瑞梅哈弗桑
Owner DSM IP ASSETS BV
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