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A method for removing dibenzothiophene in oil by using co/kit-6 cubic mesoporous catalyst

A technology of KIT-6 and dibenzothiophene is applied in the field of removing dibenzothiophene in oil products, which can solve the problems of insufficient reaction and immiscibility.

Active Publication Date: 2018-09-11
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although hydrogen peroxide is a green oxidizing agent, it cannot be miscible with oil, which makes the reaction insufficient. In contrast, oil-soluble oxidizing agents can overcome this problem very well

Method used

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  • A method for removing dibenzothiophene in oil by using co/kit-6 cubic mesoporous catalyst
  • A method for removing dibenzothiophene in oil by using co/kit-6 cubic mesoporous catalyst
  • A method for removing dibenzothiophene in oil by using co/kit-6 cubic mesoporous catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 5g of KIT-6 molecular sieve to 100ml of absolute ethanol, add 25ml of cobalt nitrate solution dropwise, the concentration of cobalt is 0.25g / ml, magnetically stir for 2-3h, the obtained sample is centrifuged, washed with water and heated at 60°C Dry overnight at 550 DEG C for 6 h and dry to constant weight; take 0.1 g of the catalyst prepared above, add it to 20 ml of DBT-n-octane solution with a sulfur concentration of 400 ppm, and then add a certain amount of cyclohexanone peroxide oxidant, O / S=4, react in an oil bath at 100°C for 40min, take it out and cool to room temperature, filter to obtain a clear solution, transfer it to an extraction bottle, add 10ml of N,N-dimethylformamide for extraction twice, each Every time, it must be left to stand for 10 minutes after being fully shaken, then remove the lower layer solution, take out the oil phase, and then use gas chromatography to detect its sulfur content. The sulfur content in the solution is reduced to 5.28ppm<1...

Embodiment 2

[0018] Add 5g of KIT-6 molecular sieve to 100ml of absolute ethanol, add 25ml of cobalt nitrate solution dropwise, the concentration of cobalt is 0.25g / ml, magnetically stir for 2-3h, the obtained sample is centrifuged, washed with water and heated at 60°C Dry overnight under 550 DEG C of roasting 6h and dry to constant weight; Get the catalyst 0.1g of above-mentioned preparation, join in the DBT-n-octane solution that 20ml sulfur-containing concentration is 400ppm, add a certain amount of cyclohexanone peroxide oxidant ( O / S=6), react in an oil bath at 100°C for 40 minutes; take it out and cool to room temperature, filter to obtain a clear solution, transfer it to an extraction bottle, add 10ml of N,N-dimethylformamide to extract twice, Each time, it should be left to stand for 10 minutes after being fully shaken, then remove the lower layer solution, take out the oil phase, and then use gas chromatography to detect its sulfur content. The rate reaches 98.71%.

Embodiment 3

[0020] Add 5g of KIT-6 molecular sieve to 100ml of absolute ethanol, add 25ml of cobalt nitrate solution dropwise, the concentration of cobalt is 0.25g / ml, magnetically stir for 2-3h, the obtained sample is centrifuged, washed with water and heated at 60°C Dry overnight at 550°C for 6 hours until constant weight. Get 0.1g of the catalyst prepared above, add it into 20ml of DBT-n-octane solution with a sulfur concentration of 400ppm, then add a certain amount of cyclohexanone peroxide oxidant, O / S=4, in an oil bath at 100°C React in medium for 50min. Take it out and cool it to room temperature, filter to obtain a clear solution, transfer it to an extraction bottle, add 10ml of N,N-dimethylformamide for extraction twice, each time shake fully and let it stand for 10min, then remove the lower layer solution The oil phase is taken out, and its sulfur content is detected by gas chromatography, and the sulfur content in the solution is reduced to 4.12ppm<10ppm, which meets the Euro...

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Abstract

The invention relates to a method for removing dibenzothiophene from an oil product through utilization of a Co / KIT-6 cubic mesoporous catalyst. The method comprises: weighing a certain amount of P123, concentrated hydrochloric acid and deionized water in sequence, performing stirring at 35 DEG C, adding n-butanol, maintaining the temperature at 35 DEG C while performing stirring for 1h, adding tetraethoxysilane (TEOS), wherein the mole ratio of P123 to H2O to HCl to n-butanol to TEOS is 0.017:196.49:5.31:1.31:1, performing stirring for 24 h, and performing thermal treatment at 35 DEG C for 24 h; performing pumping filtration to the obtained white crystal, washing the obtained product, and performing calcination at 550 DEG C to obtain KIT-6; adopting an impregnation method to prepare a Co / KIT-6 catalyst; and adding a certain amount of the prepared Co / KIT-6 catalyst and cyclohexanone peroxide taken as an oxidant to a certain amount of a n-octane solution containing dibenzothiophene (DBT) to perform catalytic oxidation to dibenzothiophene, and performing extraction with N,N-dimethylformamide (DMF) for two times in sequence after the reaction, thereby removing dibenzothiophene from an oil product. The method is simple to operate, high in removal efficiency and mild in condition, the preparation technology of the catalyst is simple, and the catalyst is high in reuse rate.

Description

technical field [0001] The invention relates to a method for removing dibenzothiophene in oil products, in particular to using cubic mesoporous molecular sieve loaded cobalt as a catalyst, cyclohexanone peroxide as an oxidant, and catalytically oxidizing and removing dibenzothiophene in oil products under certain operating conditions. Benzothiophene (DBT) is finally removed by extraction. Background technique [0002] At present, there are two main problems caused by sulfur and nitrogen compounds in oil products: on the one hand, SOx, NOx and CO are released during combustion 2 It will form acid rain and photochemical smog, causing environmental pollution and endangering people's health. On the other hand, it poisons catalysts in hydrorefining process and automobile exhaust treatment, and causes problems such as corrosion of equipment, which increases equipment cost and investment. As a result, the ecological environment is deteriorating on a global scale, and countries al...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C10G53/14C10G53/04B01J29/03B01J29/04
CPCB01J29/0356B01J29/044B01J2229/183C10G53/04C10G53/14C10G2300/202
Inventor 杨春平魏赛楠钱慧朱灿耀仇璐康丽曾光明刘海洋
Owner HUNAN UNIV
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