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 i

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0021] Example 1

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

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

[0024] Weigh sample A and place it in solution B. After stirring for 8 hours at 50°C, filter the mixture and use CHCl 3 It was washed, then vacuum-dried at 80°C for 3 hours, finally calcined at 600°C for 3 hours, ...

Example Embodiment

[0025] Example 2

[0026] Weigh 0.05g fluoroboric acid 1-butyl-3-(3-trimethoxysilyl)propylimidazole into the flask, add 10ml CHCl 3 Organic solvent, add 1.0g of MCM-48 obtained after drying at 120°C for 5 hours during the stirring process, and place in it, and heat the mixed system to reflux at 50°C for 24 hours; filter after the reaction and use CHCl 3 After washing and drying, MCM-48 (Sample A) containing ionic liquid was obtained. The loading amount of the ionic liquid is 1 wt% of the mass of the MCM-48 carrier.

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

[0028] Weigh sample A and place it in solution B. After stirring for 5 hours at 80°C, filter the mixture and use CHCl 3 It was washed, then vacuum-dried at 50°C for 5 hours, finally calcined at 400°C for...

Example Embodiment

[0029] Example 3

[0030] Weigh 0.7g of fluorinated 1-butyl-3-(3-trimethoxysilyl)propylimidazole into the flask, add 10ml CHCl 3 Organic solvent, add 1.0g of SBA-15 obtained after drying at 130°C for 4 hours in the stirring process, and place the mixed system under reflux at 60°C for 20 hours; filter after the reaction and use CHCl 3 After washing and drying, SBA-15 immobilized with ionic liquid (sample A) 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 cooled to room temperature under nitrogen protection, and dissolved in 5ml CHCl containing 20ml of tripropylamine 3 In an organic solvent, solution B was obtained after stirring at 60°C for 7 hours.

[0032] Weigh sample A and place it in solution B. After stirring for 7 hours at 60°C, filter the mixture and use CHCl 3 It is washed, then vacuum-dried at 60°C for 4 hours, finally calcined at 500°C for 5 hours, a...

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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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