Manganese-base catalyst for synthesizing alpha-tetralone from tetrahydronaphthalene and preparation method thereof

A technology of manganese-based catalyst and tetralone, which is applied in the field of manganese-based catalyst and its preparation, can solve the problems of difficulty in recycling, high reaction temperature, and high catalyst toxicity of α-tetralone, and achieve low temperature, high The effect of high catalytic activity and good industrial application prospects

Inactive Publication Date: 2013-01-23
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0005] The object of the present invention is to provide a high low-temperature activity, environment-friendly and recyclable catalyst for the existing tetralone oxidatio

Method used

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  • Manganese-base catalyst for synthesizing alpha-tetralone from tetrahydronaphthalene and preparation method thereof
  • Manganese-base catalyst for synthesizing alpha-tetralone from tetrahydronaphthalene and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Embodiment 1: with 0.2396 grams of Mn (NO 3 ) 2 4H 2 O and 0.0581 g of Zr(NO 3 ) 4 ·5H 2 Immerse 1 gram of activated alumina with a particle size of 0.10 mm in an equal volume at room temperature for 24 h in an aqueous solution prepared with O, dry at 60 °C for 4 h in an air atmosphere, and then roast at 400 °C for 6 h to obtain zirconium-modified manganese The base catalyst is recorded as Cat-A, and its composition is shown in Table 1.

Embodiment 2

[0015] Embodiment 2: with 0.4468 gram of Mn (NO 3 ) 2 4H 2 O and 0.1734 g Co(NO 3 ) 2 ·6H 2 O impregnate 1 gram of activated alumina with a particle size of 0.15 mm in an equal volume at room temperature for 36 h in the prepared aqueous solution. After impregnation, dry at 80 °C for 4 h and roast at 550 °C for 4 h in an air atmosphere to obtain cobalt-modified manganese The base catalyst is recorded as Cat-B, and its composition is shown in Table 1.

Embodiment 3

[0016] Embodiment 3: with 0.5991 gram of Mn (NO 3 ) 2 4H 2 O and 0.2109 g Fe(NO 3 ) 3 9H 2 The aqueous solution prepared by O was impregnated with an equal volume of 1 gram of activated alumina with a particle size of 0.50 mm for 24 h at room temperature. After the impregnation was completed, it was dried at 100 °C for 3 h and calcined at 600 °C for 3 h in an air atmosphere to obtain iron-modified manganese-based The catalyst is recorded as Cat-C, and its composition is shown in Table 1.

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Abstract

The invention provides a manganese-base catalyst for synthesizing alpha-tetralone from tetrahydronaphthalene and a preparation method thereof, belonging to the technical field of catalyst preparation. The manganese-base catalyst provided by the invention uses active aluminum oxide as a supporter; and Mn oxide is used as the main active component of the catalyst, and oxide of Zr, Co, Fe, Cu or Ce is used as the auxiliary active component of the manganese-base catalyst. The preparation method comprises the following steps: impregnating the active aluminum oxide supporter in a mixed solution of Mn nitrate and nitrate of Zr, Co, Fe, Cu or Ce, drying, and roasting to obtain the catalyst. The manganese-base catalyst provided by the invention has the outstanding advantage of high low-temperature activity, has the characteristic of low cost, can completely substitute toxic chrome-containing catalyst, and has favorable industrial application prospects. For example, after the reaction is carried out at 90 DEG C for 8 hours by using oxygen as an oxidizer, the conversion rate of tetrahydronaphthalene is up to 51.67%; and after the reaction is circulated four times, the activity of the catalyst is basically unchanged, and the peroxide content in the product is very low.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, and in particular relates to a manganese-based catalyst used for synthesizing alpha-tetralone from tetralin and a preparation method thereof. Background technique [0002] α-tetralone is an important pharmaceutical intermediate, mainly used for dehydrogenation of methylnaphthol; in the pharmaceutical industry for the synthesis of 18-methyl norethindrone (contraceptives), insecticide methylnaphthylamine , is also an important intermediate for the synthesis of benazepril. In addition, it can be used as a solvent and softener for plastics. [0003] At present, the synthetic methods of tetralone mainly include the following two kinds: (1) Friedel-Crafts reaction method, using benzene and γ-butyrolactone as raw materials, synthesized by Friedel-Crafts acylation reaction; Acid anhydride is used as a raw material through multi-step synthesis such as acylation, reduction and cyclization. ...

Claims

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Application Information

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IPC IPC(8): B01J23/34B01J23/889C07C49/67C07C45/36
Inventor 许立信李培杰刘巍崔平王知彩贾志刚
Owner ANHUI UNIVERSITY OF TECHNOLOGY
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