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Fuel oxidation adsorption desulfurization technology and device thereof

An adsorption desulfurization and oxidative desulfurization technology, which is applied in the petroleum industry, multi-stage series refining process treatment, hydrocarbon oil treatment, etc., can solve the problems of high liquid recovery loss, complicated separation process, and difficulty in demulsification and dehydration.

Active Publication Date: 2018-07-10
DALIAN UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

This process can oxidize some sulfur compounds, and the process cost caused by separation is relatively high
[0007] CN1660498A and CN1534082A proposed microemulsion catalytic oxidation in diesel catalytic oxidation, which improved mass transfer efficiency, but at the same time brought new difficulties for demulsification and dehydration in the separation process
[0008] To sum up, in the existing fuel oil oxidative desulfurization technology, the use of oil-soluble oxidants brings difficulties and increases the cost of subsequent product separation, and some processes introduce highly corrosive peracetic acid or peroxyformic acid, which requires high equipment requirements. High; in a two-phase reaction system, enhanced mass transfer is the key
The addition of phase transfer agent makes the separation process complicated; the reaction process of continuous operation is less, and the subsequent removal of sulfone adopts the extraction method, which has a high loss of liquid yield and subsequent separation is difficult

Method used

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  • Fuel oxidation adsorption desulfurization technology and device thereof
  • Fuel oxidation adsorption desulfurization technology and device thereof
  • Fuel oxidation adsorption desulfurization technology and device thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The preparation of metal peroxide refers to literature W.Winter, C.Mark, V.Schurig, Inorganic Chemistry 1980,19,2045-2048.,

[0035] 1) MoO(O 2 ) 2 (molybdenum peroxide) preparation: take by weighing 50g MoO 3 and 150ml 30% H 2 o 2 Transfer the aqueous solution into a 500ml round bottom flask, stir overnight at 60°C, filter and separate, add N,N'-dimethylformamide (DMF) solvent to the collected filtrate, refrigerate and crystallize in the refrigerator for 2 days, and the precipitated crystals are pumped filtered and dried to obtain MoO(O 2 ) 2 • 2DMF (43.8g).

[0036] 2)WO(O 2 ) 2 (Tungsten peroxide) Preparation of hydrogen peroxide solution: Weigh tungstic acid (100g), dissolve in 500ml H 2 o 2 solution, stirred at room temperature for 24h, centrifuged, and the liquid product was collected as WO(O 2 ) 2 of hydrogen peroxide solution.

[0037] The preparation method of the catalyst refers to the literature S.E.Jacobson, R.Tang, F.Mares, Inorg Chem1978,17,30...

Embodiment 2

[0040] Set up test groups 1, 2, and 3, and take 1000ml of raw fuel oil hydrogen (diesel, kerosene or hydrogenated gasoline) and 1000ml of working fluid into the T-shaped microreactor respectively. The preparation method of described working liquid is: in embodiment 1, molybdenum-based catalyst MoO(O 2 ) 2 Me 2 The concentration of bpy is 2.5 mg / L, the oxidizing agent is ammonium persulfate, and the solvent is a methanol-water mixed solution with a volume percentage of methanol of 10%. The oxygen-sulfur molar ratio of the oxidant to the fuel oil is 12. The volume space velocity is 10h -1 , the reaction temperatures were 60, 40, and 30°C, and the reaction pressures were 0.2, 0.2, and 0.25 MPa. After separation, centrifugation, and desulfone adsorption through Y-type molecular sieves, the sulfur content analysis results before and after the reaction are shown in Table 1.

[0041] Table 1

[0042]

Embodiment 3

[0044] Set test group 4~9, take diesel oil, kerosene or hydrogenated gasoline respectively as raw material fuel oil (as table 2) and pump into straight pipe static mixer with working fluid mixing, the preparation method of described working fluid is: the tungsten in embodiment 1 The concentration of the base catalyst bipyridyl tungsten peroxide complex is 2.5 mg / L, the solvent is water, and the oxidant is hydrogen peroxide. The molar ratio of oxygen to sulfur is 20, and the volumetric space velocity is 4h -1 , the reaction temperatures were 60, 40, and 30°C, and the reaction pressures were 0.35, 0.35, and 0.4MPa.

[0045] The oil volume ratio in test groups 4 to 6 is 1:1, and the oil volume ratio in test groups 7 to 9 is 1:2. After separation, coalescer dehydration, and acidic alumina bed adsorption to remove sulfone, the sulfur content analysis results of fuel oil mixture samples before and after the reaction are shown in Table 2.

[0046] Table 2

[0047]

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Abstract

The invention relates to a fuel oxidation adsorption desulfurization technology and a device thereof. A fuel and a water-soluble oxidant are subjected to an oxidation desulfurization reaction in an interface mass transfer enhanced reactor in the presence of a catalyst in order to oxidize most sulfur-containing compounds into sulfone products. The reaction products undergo oil-water separation, thesulfone products are removed by selective adsorption to achieve the purpose of desulfurization, and an adsorbent and the catalyst can be recycled. The technology can realize ultra-deep desulfurization of the fuel under mild conditions, and the octane number and the cetane number of the fuel before and after desulfurization are not significantly changed. The technology has the advantages of cleanprocess, high desulfurization efficiency, and suitableness for large-scale industrial production. The technology can be combined with an existing hydrodesulfurization technology to produce a clean fuel that meets national V sulfur index requirements. The method has the characteristics of simple and clean process, high desulfurization rate, no significant loss of the octane number or the cetane number, and easiness in industrial application.

Description

technical field [0001] The invention belongs to the technical fields of catalysis, petroleum processing and petrochemical industry, and relates to a process for removing sulfur-containing compounds in fuel oil. More specifically, the continuous removal of sulfur-containing compounds in fuel oil is realized through oxidation, separation and adsorption steps. Background technique [0002] The reality of environmental pollution has put forward more and more stringent standards on the quality of fuel oil. The current industrial method for producing low-sulfur clean fuels is hydrodesulfurization (HDS) technology. The hydrodesulfurization method requires very harsh reaction conditions and high hydrogen consumption, resulting in a significant increase in energy consumption and operating costs. Removal of residual fused-ring sulfur-containing compounds by oxidation is more efficient than hydrodesulfurization. In addition, oxidative desulfurization technology also has the advantage...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10G53/14
CPCC10G53/14C10G2300/202
Inventor 王安杰刘颖雅孙志超只海涛李翔王立陈永英
Owner DALIAN UNIV OF TECH
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