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Ultrasonic-oxidation extraction desulphurization method of sulfur-containing diesel

An ultrasonic and diesel technology, applied in the direction of multi-stage series refining process treatment, etc., can solve the problems of limited large-scale application, long desulfurization reaction time, complex process flow, etc. The effect of simple reaction time and process flow

Inactive Publication Date: 2013-04-10
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The above techniques use O 2 As an oxidant, the treatment method of oxidative desulfurization of sulfur-containing diesel oil, although the oxidation effect is better and the desulfurization rate is higher, but there are also the following shortcomings: the desulfurization reaction time is long (16h), the temperature (100 ° C ~ 250 ° C) and the pressure (1atm ~ 150atm, of which the desulfurization rate of 1atm ~ 50atm is less than 51.6%) has high requirements and complicated process, resulting in high cost, which limits large-scale application
[0009] At present, the oxidative desulfurization of diesel oil under the action of ultrasonic is the use of oxidant H 2 o 2 , which exists H 2 o 2 High price, large consumption, difficult regeneration and discharge of sulfur-containing wastewater

Method used

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  • Ultrasonic-oxidation extraction desulphurization method of sulfur-containing diesel

Examples

Experimental program
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Effect test

Embodiment 1

[0035] with O 2As a gas oxidant, in a 250mL three-necked flask, dissolve 0.5mL of dibenzoyl peroxide radical initiator and 4mL of n-octanal in 15mL of acetonitrile solvent, and magnetically stir the reaction solution at a temperature of 30°C and a pressure of 0.1MPa , Bubble O into the reaction solution 2 The amount is 390mL, reacted for 20min; then according to the above-mentioned reaction solution (containing aldehyde, free radical initiator and solvent) and diesel oil volume ratio 1: 4 mix, add 78mL diesel oil in the three-necked flask, V(O 2 Total consumption, standard condition): V (sulfur-containing diesel oil) = 10:1, place the ultrasonic reactor probe (ultrasonic frequency 20kHz) in the reaction mixture, the sound intensity is 5×10 3 W·m -2 , magnetically stirred the mixture, and continued to feed O into the reaction mixture by bubbling. 2 The volume is 390mL, the temperature and pressure are kept constant, and the oxidation reaction is performed under the action of...

Embodiment 2

[0038] Other conditions are the same as Example 1, change operating conditions: 0.5mL cyclohexanone peroxide free radical initiator, 20mL acetonitrile solvent, reaction temperature 60 DEG C, pass into O in the reaction solution by bubbling method 2 Amount is 1470mL, reacts 30min; Reaction liquid and diesel oil are mixed by volume ratio 1: 6, add 147mL diesel oil in the there-necked flask, V(O 2 Total consumption, standard condition): V (sulfur-containing diesel oil) = 20: 1, the three-necked flask is placed in a tank-type ultrasonic generator (ultrasonic frequency 28kHz), and the ultrasonic sound intensity is 5 × 10 3 W·m -2 , the paddle stirred the mixed solution, and the bubbling method continued to pass O into the reaction mixed solution. 2 The volume is 1470mL, and the ultrasonic action time is 30min. The oil phase water washing process is carried out under the conditions of a temperature of 15°C and a pressure of 0.3MPa, using Na 2 CO 3 Solution and water; Diesel oil ...

Embodiment 3

[0040] Other conditions are the same as in Example 1, and the operating conditions are changed: 0.7mL isobutyl hydroperoxide free radical initiator, 3mL isobutyraldehyde, 20mL N, N-dimethylformamide solvent, reaction temperature 20°C, bubbling normal reaction O 2 The volume is 950mL, and the reaction is 20min; the reaction solution and diesel oil are mixed in a volume ratio of 1:3, and 71.1mL diesel oil is added to the three-necked flask, V(O 2 Total consumption, standard condition): V (sulfur diesel) = 30:1, ultrasonic sound intensity 2×10 3 W·m -2 , the bubbling method continued to pass O into the reaction mixture 2 The volume is 1183mL, and the ultrasonic action time is 20min. The oil phase water washing process is carried out under the conditions of a temperature of 30°C and a pressure of 0.1MPa, using NaHCO 3 Solution and water; Diesel oil after washing with 0.6g anhydrous CaCl 2 After drying for 4 hours, refined diesel oil with a sulfur content of 34 μg / g was obtain...

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Abstract

The invention discloses an ultrasonic-oxidation extraction desulphurization method of sulfur-containing diesel, which is characterized in that oxygen or air is adopted as an oxidant during the oxidation process. The method integrates the ultrasonic effect, the catalyzing oxidation process and the extraction desulphurization process, so the sulfur content of the diesel reaches the quality standardof national class-V diesel (less than 15 micrograms per gram) within a short time under the condition of the normal pressure and the atmospheric temperature, and the desulphurization rate reaches more than 96 percent. Compared with the conventional desulphurization technology, the method not only has remarkable desulphurization effect and short reaction time, and improves the production efficiency, but also has moderate reaction conditions, has low equipment investment and operation cost, simple process flow procedures and low production cost, and is an energy-saving, high-efficient and environment-friendly desulphurization process route.

Description

technical field [0001] The invention relates to an oxidative extraction desulfurization method of diesel oil in a petroleum refining process, in particular to an ultrasonic-oxidative extraction desulfurization method of sulfur-containing diesel oil. Background technique [0002] With the increasingly stringent environmental protection regulations, the quality requirements of fuel oil are becoming more stringent worldwide, and the production of low-sulfur "clean fuel" has become an inevitable trend. Therefore, in the face of increasingly stringent restrictions on diesel sulfur content and the huge market demand for low-sulfur clean diesel, the improvement and innovation of diesel desulfurization methods have very important practical significance. [0003] The sulfides in diesel are mainly alkylbenzothiophene and alkyldibenzothiophene; the existence of these sulfides not only causes SOx pollution to the environment during the use of diesel, but also significantly affects the e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C10G53/14
Inventor 吕效平王成勇郭伟林朋韩萍芳
Owner NANJING TECH UNIV