Deep desulfurization method for diesel by coupling of oxidation and extraction

A diesel and hydrogen peroxide technology, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, chemical/physical processes, etc., can solve the problem of increased operating costs, high desulfurization costs and impact on oil yield rate and other problems, to achieve the effect of low cost, high oil yield, high economic and social benefits

Inactive Publication Date: 2010-06-02
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] To sum up, most of the existing oxidative desulfurization technologies need to separate and remove sulfoxide and sulfone oxidation products from fuel oil through extraction and other methods after the catalytic oxidation reaction. Yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In a 250ml Erlenmeyer flask, add 100ml of mixed straight-run diesel oil with a sulfur content of 1703 μg / g, 10ml of a 30% (percentage by weight) aqueous solution of hydrogen peroxide and 100ml of N, N-dimethylformamide (DMF) extractant and 2g homemade WO 3 / ZrO 2 Solid superacid catalyst, at an ultrasonic frequency of 50-70kHz, preferably 59kHz, and an ultrasonic power of 350-450W, preferably 350W, under the action of ultrasound at 40-80°C, preferably 60°C, for 30-70min, preferably 60min. . After the reaction was finished, cool to room temperature, separate the solid catalyst and recycle it, and then put it into stratification. The upper layer was analyzed to obtain desulfurized diesel oil with a sulfur content of 28.5 μg / g, the desulfurization rate was 98.3%, and the oil yield was 98.7%. It is recycled after regeneration.

Embodiment 2

[0028] In a 250ml Erlenmeyer flask, adding 100ml sulfur content is 1703 μg / g mixed straight-run diesel oil, 20ml concentration is 30% (weight percent) hydrogen peroxide aqueous solution and 100ml N, N-dimethylformamide (DMF) extractant and 2g homemade WO 3 / ZrO 2 Solid superacid catalyst, all the other operations are the same as Example 1, and the desulfurized diesel oil with a sulfur content of 26.8 μg / g is obtained, the desulfurization rate is 98.4%, and the oil yield is 98.2%.

Embodiment 3

[0030] In a 250ml Erlenmeyer flask, add 50ml of mixed straight-run diesel oil with a sulfur content of 1703 μg / g, 10ml of a 30% (percentage by weight) hydrogen peroxide solution and 100ml of N, N-dimethylformamide (DMF) extractant And 2g self-made catalyst, the rest of the operations are the same as in Example 1 to obtain desulfurized diesel oil with a sulfur content of 23.8 μg / g, a desulfurization rate of 98.6%, and an oil yield of 93.1%.

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PUM

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Abstract

The invention relates to a deep desulfurization method for diesel by coupling of oxidation and extraction, that is a catalyzed oxidation desulfurization method for diesel in petroleum refining technologies. The method comprises the following steps of crushing and fine grinding a zirconium hydroxide carrier, dipping into impregnation liquid formed by aqueous ammonium meta-tungstate solution, placing the impregnation liquid in an ultrasonic generator to carry out ultrasonic facilitating impregnation, boiling off water after the impregnation is finished, drying and baking at high temperature to obtain a WO3/ZrO2 super solid acidic catalyst; adding aqueous hydrogen peroxide solution, extraction solvent and the WO3/ZrO2 super solid acidic catalyst in diesel containing sulfur, carrying out catalyzed oxidation desulfurization reaction under the action of power ultrasonics, cooling to the room temperature after the reaction is finished, separating and recycling the solid catalyst, standing and layering, wherein the upper layer is desulfurized diesel and the lower layer can be reused after regeneration. The invention has simple process, mild condition, high desulfurization degree and gasoline recovery, low cost and no pollution to environment and can obtain ultra-low sulfur clean diesel products.

Description

technical field [0001] The invention relates to a method for catalytic oxidation desulfurization of diesel oil in petroleum refining process. Background technique [0002] With the enhancement of people's awareness of environmental protection and the improvement of vehicle fuel exhaust emission standards, many countries in the world have set increasingly strict restrictions on the sulfur content of fuel oil, and the production and use of ultra-low sulfur fuel oil has become imperative. Therefore, it is of great practical significance to study the environment-friendly deep desulfurization technology of diesel oil and meet the new opportunities and challenges of clean fuel production. [0003] In terms of deep desulfurization, the traditional hydrodesulfurization (HDS) method has harsh reaction conditions, high equipment investment and operating costs, and it is difficult to remove dibenzothiophene (DBT) series sulfides with large steric hindrance, so it is difficult to meet t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10G53/14B01J23/30B01J37/34B01J37/02
Inventor 张存王洪娟王峰
Owner YANGZHOU UNIV
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