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Method for preparing heterogeneous catalyst used for epoxy cyclohexane and application thereof

A heterogeneous catalyst, epoxy cyclohexane technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of precious metal loss, catalyst activity decline, easy to agglomerate, etc., to achieve high activity and selectivity, avoid easy runoff, prevent the effect of agglomeration

Inactive Publication Date: 2012-02-08
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, with the gradual deepening of research, it is found that these catalysts are difficult to control the coordination state of the active center so that the catalytic performance of the catalyst is seriously affected.
In addition, the active components (metal ions) in these mesoporous molecular sieve catalysts are easy to fall off during the reaction, resulting in the loss of precious metals
At the same time, metal ions are easy to agglomerate at a certain reaction temperature, resulting in a decrease in catalyst activity.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Weigh 0.5g of 1-methyl-3-(3-trimethoxysilyl)propylimidazole chloride in a flask, add 10ml of CHCl 3 As an organic solvent, add 1.0 g of MCM-41 obtained after drying at 150°C for 3 hours during stirring, and heat the mixed system at 80°C to reflux for 12 hours; filter after the reaction, and use CHCl 3 After washing and drying, MCM-41 (sample A) loaded with ionic liquid was obtained. The loading amount of the ionic liquid is 20wt% of the mass of the MCM-41 carrier.

[0023] 0.03g titanocene was dried under vacuum at 120°C for 1 hour, then naturally cooled to room temperature under nitrogen protection and dissolved in 5ml CHCl containing 1.7ml triethylamine 3 Solution B was obtained after stirring at 50°C for 8 hours in an organic solvent.

[0024] Weigh sample A and place it in solution B, stir at 50°C for 8 hours, filter the mixture, and wash with CHCl 3 Washing, then vacuum drying at 80°C for 3 hours, and finally calcination at 600°C for 3 hours, and natural cooling...

Embodiment 2

[0026] Weigh 0.05g of 1-butyl-3-(3-trimethoxysilyl)propylimidazole fluoborate in a flask, add 10ml of CHCl 3 As an organic solvent, add 1.0 g of MCM-48 obtained after drying at 120°C for 5 hours during stirring, and heat the mixed system at 50°C to reflux for 24 hours; filter after the reaction, and use CHCl 3 After washing and drying, MCM-48 (sample A) loaded with ionic liquid was obtained. The loading amount of the ionic liquid is 1wt% of the mass of the MCM-48 carrier.

[0027] 0.6g of ferrocene was vacuum-dried at 80°C for 3 hours, then naturally cooled to room temperature under nitrogen protection and dissolved in 5ml of CHCl containing 30ml of triethanolamine 3 Solution B was obtained after stirring at 80° C. for 5 hours in an organic solvent.

[0028] Weigh sample A and place it in solution B, stir at 80°C for 5 hours, filter the mixture, and wash with CHCl 3 Wash, then vacuum-dry at 50°C for 5 hours, and finally calcined at 400°C for 6 hours, and naturally cool to r...

Embodiment 3

[0030] Weigh 0.7g of 1-butyl-3-(3-trimethoxysilyl)propylimidazole fluoride in a flask, add 10ml of CHCl 3 Organic solvent, add 1.0 g of SBA-15 obtained after drying at 130°C for 4 hours during stirring, and heat the mixed system at 60°C for 20 hours; filter after the reaction, and use CHCl 3 After washing and drying, SBA-15 (sample A) loaded with ionic liquid was obtained. The loading amount of the ionic liquid is 50wt% of the mass of the SBA-15 carrier.

[0031] 0.3g of ferrocene was dried under vacuum at 100°C for 2 hours, then naturally cooled to room temperature under nitrogen protection and dissolved in 5ml of CHCl containing 20ml of tripropylamine 3 Solution B was obtained after stirring at 60° C. for 7 hours in an organic solvent.

[0032] Weigh sample A and place it in solution B, stir at 60°C for 7 hours, filter the mixture, and wash with CHCl 3Wash, then vacuum-dry at 60°C for 4 hours, and finally calcined at 500°C for 5 hours, and cool naturally to room temperatu...

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PUM

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Abstract

The invention relates to a preparation method of a heterogeneous catalyst, and particularly relates to a preparation method of a heterogeneous catalyst used for epoxy cyclohexane and an application thereof. The catalyst takes SiO2-based mesopore molecular sieve as a carrier, the method comprises the following steps: forming a metal organic complex by organic metal salt and a complex in advance, then combing with an ionic liquid phase, highly dispersed and loaded on a tunnel surface of a porous SiO2 material by a grafting method. So that the catalyst has good catalysis performance in the application of cyclohexene on catalytic oxidation preparation of epoxy cyclohexane, in addition, the catalyst has the characteristics of controllable structure, good stability, easy separation, easy recovery and the like.

Description

Technical field: [0001] The invention belongs to the technical field of fine chemical industry and catalyst preparation, and in particular relates to a preparation method of a heterogeneous catalyst for preparing epoxycyclohexane by catalytic oxidation of cyclohexene. Background technique: [0002] Epoxycyclohexane is an important fine chemical raw material and organic intermediate. Because of its active epoxy group in its molecular structure, it can react with ammonia, amine, phenol, alcohol and carboxylic acid in industrial and agricultural production. While generating high value-added chemical products, it is also a highly soluble organic solvent. With the continuous development of the use of epoxycyclohexane, the demand for it has also increased in recent years. [0003] Using cyclohexene as a raw material, the preparation of epoxycyclohexane by catalytic oxidation reaction is an important process route at present. According to the catalyst used, it can be divided into...

Claims

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Application Information

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IPC IPC(8): B01J29/70B01J29/76B01J29/03B01J29/78C07D303/04C07D301/19
CPCY02P20/50
Inventor 孙继红胡新涛任博张丽张黄高琳
Owner BEIJING UNIV OF TECH
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