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Preparation method and application of immobilized catalyst for hydrocarbon oxidation

A technology of immobilized catalysts and hydrocarbons, which is applied in the direction of oxidation reaction preparation, organic compound preparation, physical/chemical process catalysts, etc. It can solve the problem that catalysts are difficult to separate and recycle, and achieve many steps in the immobilization process and simple preparation methods , the complex effect of the preparation process

Active Publication Date: 2014-11-19
XIANGTAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

Inventions described earlier were able to improve the efficiency of producing certain types of organopolysiloxanes called polydiorganosilsiloxanes(PDOS). These organopolymers consist mainly of repeating units that contain different functionalities like amine moieties and alkynols. By reacting an acid chloroformate derivative onto each unit's surface, they become chemically bound together without losing their functionality. They may even include substituents at specific positions within one unit instead of just combining multiple atoms into rings. Overall, these technical improvements lead to improved properties and applications related thereto.

Problems solved by technology

This technical problem addressed in this patents relates to improving the efficiency of producing industrially useful compounds while minimizing environmental impact caused by combustion processes involving direct oxidative addition of unsaturated hydrogen atoms onto specific positions within certain types of substances like alcohol groups. Current methods involve expensive noble metals and complex procedures, making it difficult to reuse them after their usage.

Method used

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  • Preparation method and application of immobilized catalyst for hydrocarbon oxidation
  • Preparation method and application of immobilized catalyst for hydrocarbon oxidation
  • Preparation method and application of immobilized catalyst for hydrocarbon oxidation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The immobilized N,N'-dihydroxypyrylenetetracarboximide catalyst was prepared according to the following procedure.

[0032]

[0033] 1.34g (19.2mmol) of hydroxylamine hydrochloride and 2.6mL (19mmol) of triethylamine were dissolved in 60mL of ethanol, stirred for 10min, and 2.18g (9.8mmol) of 1,2,4,5-benzenetetracarboxylic anhydride [formula (5 )], stirred and refluxed under nitrogen atmosphere for 8h, cooled to room temperature, added 100ml deionized water, stirred evenly and precipitated a yellow solid. The solid filtered out with suction was washed several times with deionized water, and dried under vacuum to obtain N,N'-dihydroxypyrolitetetridine (NDHPI) [formula (6)].

[0034] After activation treatment, 4.00g of commercially available SBA-15 (Nanjing Jicang Nano Technology Co., Ltd.) was suspended in 120ml of toluene, and 0.012mol (2.83g) of γ-(2,3 glycidyl oxide) was added while fully stirring. Base) propyltrimethoxysilane, 110 ° C nitrogen protection reflux ...

Embodiment 2

[0037] In a 100ml passivated autoclave, add 1.37g of immobilized N,N'-dihydroxypyrylenetetracarboximine prepared in Example 1, 0.0036g of N,N-disalicylaldehyde ethylenediamine cobalt complex (Cosalen) , 4.00g of acetonitrile, 5.00g of toluene, 1.60MPa oxygen gas was introduced to react at one time, the reaction temperature was 90°C, after 7h, the reaction kettle was taken out and cooled rapidly, and the reaction solution was taken out after pressure relief, analyzed by gas chromatography, and cyclohexanone was used as The internal standard was used for quantification, and the conversion rate of toluene was measured to be 12.74%, and the selectivities of benzaldehyde, benzyl alcohol and benzoic acid were 40.31%, 9.25% and 50.43%, respectively.

Embodiment 3

[0039] In a 100ml passivated autoclave, add 1.37g of immobilized N,N'-dihydroxypyrylenetetracarboximine prepared in Example 1, 0.0036g of N,N-disalicylaldehyde ethylenediamine cobalt complex (Cosalen) , 4.00g of acetonitrile, 5.00g of toluene, 1.60MPa oxygen was introduced into the reaction at one time, the reaction temperature was 110°C, after 4h, the reaction kettle was taken out and cooled rapidly, and the reaction solution was taken out after pressure relief, analyzed by gas chromatography, and cyclohexanone was used as The internal standard was used for quantification, and the conversion rate of toluene was measured to be 52.25%, and the selectivities of benzaldehyde, benzyl alcohol and benzoic acid were 17.81%, 5.16% and 77.02%, respectively.

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Abstract

The invention discloses a preparation method and application of an immobilizedcatalyst which is applied to a hydrocarbon-oxidizing system, is easily separated from a reaction liquid and can be recycled. The preparation method for the immobilized catalyst is realized in such a way that two or more N-hydroxyphthalimide (NHPI ) derivatives are immobilized on a silicon-based mesoporous material through a silane coupling agent containing an epoxygroup by adopting a covalent chemical grafting method. The immobilized catalyst can be used for catalyzing hydrocarbon molecule oxygen to generate an oxidizing reaction under a mild condition and has higher activity and selectivity.

Description

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Claims

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Application Information

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Owner XIANGTAN UNIV
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