CN103242897A - Method for removing sulfur from fuel oil through electrolytic reduction - Google Patents
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- CN103242897A CN103242897A CN201310143888XA CN201310143888A CN103242897A CN 103242897 A CN103242897 A CN 103242897A CN 201310143888X A CN201310143888X A CN 201310143888XA CN 201310143888 A CN201310143888 A CN 201310143888A CN 103242897 A CN103242897 A CN 103242897A
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- desulfurization
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Abstract
The invention discloses a method for removing sulfur from fuel oil through electrolytic reduction. The method comprises the following steps of: adding a sodium metaborate and sodium hydroxide solution to a working electrode electrolytic tank, and then adding the fuel oil; adding a sodium hydroxide solution to a counter electrode electrolytic tank; applying voltage to the working electrode electrolytic tank and the counter electrode electrolytic tank, stirring the solution in the working electrode electrolytic tank, dropwise adding a catalyst and carrying out electrolytic reaction; and after the electrolytic reaction is ended, filtering a product, and separating a filtrate, wherein obtained upper oil is low-sulfur fuel oil. According to the method, the sodium metaborate is used as an electrolyte main body, a trace amount of sodium hydroxide is added for assisting the electrolyte, the sodium metaborate is converted to sodium borohydride under an alkaline condition, simultaneously, the sulphur in the fuel oil is reduced into H2S by using the reduction property of the sodium borohydride under the catalyst of metal chloride, and the H2S is absorbed. The method for removing the sulfur through the electrolytic reduction has the advantages that reaction conditions are mild, the circulation of boron is realized while the sulfur is removed from fuel oil, thus water liquid without sulphur can be recycled, resources and energy sources are saved, and the pollution to environments is reduced.
Description
Technical field
The invention belongs to fuel treatment and environmental chemistry field, relate in particular to the method for a kind of oil fuel electrolytic reduction desulfurization.
Background technology
Organic sulfide is a kind of objectionable impurities in the oil fuel (gasoline, diesel oil, kerosene etc.).The SO that its burning back generates
xBe one of main source of atmosphere acid rain, cause to the pollution of environment with to the infringement of human health.For vehicle fuel, SO
xTo HC, CO in the vehicle exhaust particularly the discharging of NOx and PM obvious facilitation is arranged, thereby cause the increase of pollutant emission.And, SO
xAlso can poison exhaust catalytic converter, the performance of infringement oxygen sensor and onboard diagnostic system etc.Huge in view of the harm of sulphur in the vehicle fuel, countries in the world have been promulgated stricter vehicle fuel standard in succession, and low-sulfur even the vehicle fuel that does not have sulphur have become development in future trend.
At present, low sulphur fuel oil is produced in industrial main application hydrogenating desulfurization, though this method can satisfy the low-sulfur requirement of oil fuel to a certain extent, but operational condition harshness, need under High Temperature High Pressure, to carry out, need special catalyzer and a large amount of highly purified hydrogen, investment and process cost height.And hydrodesulfurization process also can make alkene a large amount of in the oil fuel saturated, the paraffinic hydrocarbons cracking, thus cause the oil plant yield to descend and the reduction of octane value.Therefore, numerous investigator has invested sight the exploitation of non-hydrogenating desulfurization technology.
Sodium borohydride (NaBH
4) be a kind of reductive agent of excellent property, extensive application aspect organic chemistry and inorganic chemistry.At metal chloride (as NiCl
2, CoCl
2) its reducing power significantly improves when existing, and is obvious to the removal effect of sulphur in the organic sulfide.Existing a large amount of researchs are with NaBH
4Be applied to removing of coal and sulfur in gasoline as reductive agent, and obtained removal efficiency preferably.But, NaBH
4Expensive, a large amount of industrial application is uneconomic.And NaBH
4Hydrolysising by-product-sodium metaborate (NaBO
2) be very cheap, can be by NaBO by electrochemical reduction
2Preparation NaBH
4Therefore, if NaBH
4Electrochemical reduction preparation and NaBH
4Reduction and desulfurization is joined together, and forms a recycle system, can reduce the desulfurization expense greatly.Be applied to existing relevant bibliographical information (the Yafei Shen of reduction and desulfurization of coal about this combined process, et al.Innovative Desulfurization Process of Coal Water Slurry under Atmospheric Condition via Sodium Metaborate Electroreduction in the Isolated Slot.Energy Fuels, 2011,25,5007-5014.), but the desulfurization that is applied to oil fuel yet there are no relevant report.
Summary of the invention
The objective of the invention is to overcome traditional hydrodesulfurization and need High Temperature High Pressure, the condition harshness is invested and defectives such as process cost height and reduction oil fuel quality, has proposed the method for a kind of oil fuel electrolytic reduction desulfurization.This method utilizes electrochemical reaction to realize the conversion of sodium metaborate to sodium borohydride, utilizes the good reducing property of sodium borohydride simultaneously, under the catalysis of metal chloride, the sulphur in the oil fuel is reduced into H
2S, and absorbed, realize the gentle desulfurization to oil fuel, and reduce desulphurization cost.
The objective of the invention is to be achieved through the following technical solutions:
The present invention relates to the method for a kind of oil fuel electrolytic reduction desulfurization, comprise the steps:
A, in the working electrode electrolyzer, add sodium metaborate and sodium hydroxide solution as electrolytic solution, add oil fuel then;
B, in the counter electrode electrolyzer, add sodium hydroxide solution;
C, past working electrode, counter electrode electrolyzer feed voltage, stir solution in the work electrode electrolytic pool simultaneously, and drip catalyzer, carry out electrolytic reaction;
After d, electrolytic reaction finish, the product in the working electrode electrolyzer is filtered, separating filtrate, the gained upper oil phase is low sulphur fuel oil.
Preferably, the working electrode that adopts in the described working electrode electrolyzer is the boron-doped diamond film plate, and reference electrode is saturated calomel electrode; The counter electrode that adopts in the described counter electrode electrolyzer is graphite cake; The hydrogen sulfide that produces in the described electrolytic reaction imports in the electrolytic solution of counter electrode electrolyzer, absorbs and is used.
Preferably, the concentration 0.1～0.3mol/L of sodium metaborate described in the electrolytic solution of described working electrode electrolyzer, described concentration sodium hydroxide is 0.01～0.1mol/L, the volume ratio of described oil fuel and described electrolytic solution is 0.25～1.
Preferably, the sulphur content 〉=10ppm of described oil fuel.
Preferably, the described voltage that feeds toward the working electrode electrolyzer is pulsed voltage.
Preferably, in the described pulsed voltage, direct impulse voltage is-1.2～-1.8 volts, and the direct impulse voltage time length is 1～2 second, and reverse pulse voltage is 0.2～0.5 volt, and the reverse pulse voltage time length is 0.1～1 second.
Preferably, during solution, stirring velocity is 200rpm～600rpm in the described stirring work electrode electrolytic pool.
Preferably, behind the dropping catalyzer, catalyst consumption is 0.6～2mmol in every liter of interior total solution of working electrode electrolyzer; Described catalyzer is metal chloride.This metal chloride is preferably nickelous chloride or cobalt chloride.
Preferably, dropping time length 〉=10 of described catalyzer minute.
Preferably, described electrolytic reaction time 〉=20 minute.
Principle of work of the present invention is: for improving desulfuration efficiency, pulse voltage and boron-doped diamond film electrode are incorporated into this combined process, its former because: according to electrochemical reduction mechanism (negative electrode: BO
2 -+ 6H
2O+8e
-→ BH
4 -+ 8OH
-Anode: 4OH
--4e
-→ 2H
2O+O
2↑), BO
2 -Be to be reduced into BH at negative electrode
4 -, still, since the effect of repelling each other of the electric charge same sex, electronegative BO
2 -Be difficult near cathode surface, therefore, when carrying out electrochemical reduction with constant voltage, BO
2 -Be converted into BH
4 -Efficient lower.Yet, when applying pulsed voltage, namely on working electrode, alternately apply positive voltage and negative voltage, when applying positive voltage, electronegative BO
2 -Attracted to working electrode surface, when applying negative voltage, attracted to the BO of working electrode surface
2 -Be reduced into BH
4 -, so constantly circulation, BO
2 -Constantly attracted to working electrode surface and be reduced to BH
4 -Thereby, improved BO greatly
2 -Be converted into BH
4 -Efficient, corresponding desulfuration efficiency has also improved greatly.
On the other hand, when working electrode being applied positive voltage alternately and negative voltage, oxygen evolution reaction (4OH
--4e
-→ 2H
2O+O
2↑) and evolving hydrogen reaction (2H
2O+2e
-→ H
2↑+2OH
-) also may be simultaneous, this can reduce current efficiency greatly.Therefore, for fear of oxygen evolution reaction and evolving hydrogen reaction, need be with the electrode materials with broad potential window as working electrode, and the boron-doped diamond film electrode is the electrode materials that a quasi-representative has broad potential window.And the boron-doped diamond film electrode has strong corrosion resistance, can adapt to the alkaline environment of reaction system among the present invention; The low background current characteristic of boron-doped diamond film electrode can improve current efficiency.
Compared with prior art, the present invention has following beneficial effect:
1, method reaction conditions gentleness of the present invention, process cost is low, and having overcome traditional hydrodesulfurization needs High Temperature High Pressure, condition harshness, the defective of investment and process cost height and reduction oil fuel quality;
2, the present invention unites NaBH
4Electrochemical reduction preparation and NaBH
4The reduction and desulfurization process is applied to the desulfurization of oil fuel, by using pulsed voltage and boron-doped diamond film electrode, obtained higher desulfuration efficiency, and realized the circulation of boron in desulfurization, desulfurization waste liquor is able to recycle, economize on resources and the energy, and reduced pollution to environment.
Description of drawings
By reading the detailed description of non-limiting example being done with reference to the following drawings, it is more obvious that other features, objects and advantages of the present invention will become:
Fig. 1 is oil fuel electrolytic reduction desulfurizer of the present invention and schematic diagram;
Wherein, 1, constant temperature blender with magnetic force, 2, the counter electrode electrolyzer, 3, the working electrode electrolyzer, 4, working electrode, 5, counter electrode, 6, reference electrode, 7, electrochemical workstation.
Embodiment
The present invention is described in detail below in conjunction with drawings and Examples.Following examples will help those skilled in the art further to understand the present invention, but not limit the present invention in any form.Should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, can also make certain adjustments and improvements.These all belong to protection scope of the present invention.
Device of the present invention and principle are ionogen with the sodium metaborate as shown in Figure 1, pass through cathodic reduction reaction, sodium metaborate is converted into sodium borohydride, utilize the good reducing property of sodium borohydride simultaneously, under the catalysis of metal chloride, the sulphur in the oil fuel is reduced into H
2S, and absorbed.The boron-doped diamond film plate is working electrode in the electrolyzer, and graphite cake is counter electrode, and saturated calomel electrode is reference electrode.Below the metal chloride catalyst that adopts among each embodiment be prepare by the following method and:
A, take by weighing a certain amount of metal chloride, be dissolved in 50mlH
2Among the O, low-grade fever is fully dissolved;
B, solution is settled to 1000ml, obtaining concentration is the metal chloride catalyst solution of 0.01mol/L.
The oil fuel electrolytic reduction desulfurizer that present embodiment adopts and principle are as shown in Figure 1, be ionogen with the sodium metaborate, pass through cathodic reduction reaction, sodium metaborate is converted into sodium borohydride, utilize the good reducing property of sodium borohydride simultaneously, under the catalysis of metal chloride, the sulphur in the oil fuel is reduced into H
2S separates namely obtaining the low-sulfur fuel oil production again by filtration, separating funnel.The boron-doped diamond film plate is working electrode 4 in the working electrode electrolyzer 3, and saturated calomel electrode is reference electrode 6, and graphite cake is counter electrode 5 in the counter electrode electrolyzer 2, and the hydrogen sulfide of generation passes through airway, finally imports in the counter electrode electrolyzer to be absorbed by electrolytic solution.In working electrode electrolyzer 3, add sodium metaborate and sodium hydroxide solution as electrolytic solution, adding oil fuel then stirs, add sodium hydroxide solution in the counter electrode electrolyzer 2, feed pulsed voltage toward working electrode, counter electrode electrolyzer 3,2 then, adopt constant temperature blender with magnetic force 1 to stir mixing solutions in the work electrode electrolytic pool 3 simultaneously, carry out electrolytic reaction; Electrolytic reaction is closed electrochemical workstation 7 after finishing, and the product in the working electrode electrolyzer 3 is filtered, and filtrate is separated with separating funnel, and the gained upper oil phase is the low-sulfur fuel oil production.
In the present embodiment, be to handle object with gasoline, sodium metaborate concentration is 0.1mol/L in the working electrode electrolyzer, naoh concentration is 0.01mol/L, gasoline (sulphur content is 406ppm) is 0.25 with electrolytic solution volume ratio, feed pulsed voltage toward the working electrode electrolyzer, direct impulse voltage is-1.2V, reverse pulse voltage is 0.2V, and the direct impulse voltage time length is 1s, and the reverse pulse voltage time length is 0.1s, simultaneously with solution in the stirring velocity stirring work electrode electrolytic pool of 400rpm, and slowly drip nickel chloride catalyst agent 0.8mmol/L, and the dropping time is 30 minutes, the electrolytic reaction time is 1 hour.Final oil fuel product is measured sulphur content by the sulphur blood urea/nitrogen analyzer, records the gasoline products desulfurization degree and reaches 81%.
The method of present embodiment is with embodiment 1, difference is: sodium metaborate concentration is 0.15mol/L in the working electrode electrolyzer, naoh concentration is 0.1mol/L, gasoline (sulphur content is 406ppm) is 1/3 with electrolytic solution volume ratio, feed pulsed voltage toward the working electrode electrolyzer, direct impulse voltage is-1.5V, reverse pulse voltage is 0.3V, the direct impulse voltage time length is 1.5s, the reverse pulse voltage time length is 0.5s, simultaneously with solution in the stirring velocity stirring work electrode electrolytic pool of 400rpm, and slowly drips nickel chloride catalyst agent 0.6mmol/L, the dropping time is 30 minutes, and the electrolytic reaction time is 1 hour.After reaction finishes, the product in the working electrode electrolyzer is filtered, filtrate is separated with separating funnel, and gained gasoline products desulfurization degree reaches 97%.
Embodiment 3
The method of present embodiment is with embodiment 1, difference is: sodium metaborate concentration is 0.15mol/L in the working electrode electrolyzer, naoh concentration is 0.01mol/L, gasoline (sulphur content is 406ppm) is 1/3 with electrolytic solution volume ratio, feed pulsed voltage toward the working electrode electrolyzer, direct impulse voltage is-1.5V, reverse pulse voltage is 0.5V, the direct impulse voltage time length is 1.5s, the reverse pulse voltage time length is 0.5s, simultaneously with solution in the stirring velocity stirring work electrode electrolytic pool of 200rpm, and slowly drips cobalt-chloride catalyst 0.6mmol/L, the dropping time is 30 minutes, and the electrolytic reaction time is 1 hour.After reaction finishes, the product in the working electrode electrolyzer is filtered, filtrate is separated with separating funnel, and gained gasoline products desulfurization degree reaches 90%.
Embodiment 4
The method of present embodiment is with embodiment 1, difference is: be to handle object with diesel oil, sodium metaborate concentration is 0.3mol/L in the working electrode electrolyzer, naoh concentration is 0.02mol/L, diesel oil (sulphur content is 406ppm) is 1 with electrolytic solution volume ratio, feed pulsed voltage toward the working electrode electrolyzer, direct impulse voltage is-1.8V, reverse pulse voltage is 0.3V, and the direct impulse voltage time length is 2s, and the reverse pulse voltage time length is 1s, simultaneously with solution in the stirring velocity stirring work electrode electrolytic pool of 600rpm, and slowly drip cobalt-chloride catalyst 2mmol/L, and the dropping time is 30 minutes, the electrolytic reaction time is 1.5 hours.After reaction finishes, the product in the working electrode electrolyzer is filtered, filtrate is separated with separating funnel, and gained diesel product desulfurization degree reaches 78%.
The method of present embodiment is with embodiment 1, difference is: be to handle object with diesel oil, sodium metaborate concentration is 0.2mol/L in the working electrode electrolyzer, naoh concentration is 0.02mol/L, diesel oil (sulphur content is 406ppm) is 1/3 with electrolytic solution volume ratio, feed pulsed voltage toward the working electrode electrolyzer, direct impulse voltage is-1.5V, reverse pulse voltage is 0.3V, the direct impulse voltage time length is 1.5s, the reverse pulse voltage time length is 0.5s, simultaneously with solution in the stirring velocity stirring work electrode electrolytic pool of 400rpm, and slowly drip nickel chloride catalyst agent 1.2mmol/L, and the dropping time is 30 minutes, the electrolytic reaction time is 1.5 hours.After reaction finishes, the product in the working electrode electrolyzer is filtered, filtrate is separated with separating funnel, and gained diesel product desulfurization degree reaches 86%.
In conjunction with above embodiment, as can be known: because the sodium metaborate that the present invention adopts is the hydrolysate of sodium borohydride, chemical property is stable, low price; The electrochemical method that adopts is a kind of chemical technology of green, can realize sodium metaborate by the process of charging and discharge to the conversion of sodium borohydride, and technology is simple, reaction temperature and, the chemical reagent recycle do not bring secondary pollution etc.; The present invention has overcome traditional hydrodesulfurization needs High Temperature High Pressure, condition harshness, the defective of investment and process cost height and reduction oil fuel quality; And the inventive method has realized the circulation of boron in desulfurization, and desulfurization waste liquor is able to recycle, economizes on resources and the energy, and has reduced pollution to environment.In addition, by embodiment 1,2,3 and embodiment 4,5 more as can be known: use this method and handle the sweetening effectiveness of gasoline and be better than diesel oil generally.
More than specific embodiments of the invention are described.It will be appreciated that the present invention is not limited to above-mentioned specific implementations, those skilled in the art can make various distortion or modification within the scope of the claims, and this does not influence flesh and blood of the present invention.
Claims (10)
1. the method for oil fuel electrolytic reduction desulfurization is characterized in that, comprises the steps:
A, in the working electrode electrolyzer, add sodium metaborate and sodium hydroxide solution as electrolytic solution, add oil fuel then;
B, in the counter electrode electrolyzer, add sodium hydroxide solution;
C, past working electrode, counter electrode electrolyzer feed voltage, stir solution in the work electrode electrolytic pool simultaneously, and drip catalyzer, carry out electrolytic reaction;
After d, electrolytic reaction finish, the product in the working electrode electrolyzer is filtered, separating filtrate, the gained upper oil phase is low sulphur fuel oil.
2. the method for oil fuel electrolytic reduction according to claim 1 desulfurization is characterized in that, the working electrode that adopts in the described working electrode electrolyzer is the boron-doped diamond film plate, and reference electrode is saturated calomel electrode; The counter electrode that adopts in the described counter electrode electrolyzer is graphite cake; The hydrogen sulfide that produces in the described electrolytic reaction imports in the electrolytic solution of counter electrode electrolyzer.
3. the method for oil fuel electrolytic reduction according to claim 1 desulfurization, it is characterized in that, the concentration of sodium metaborate described in the electrolytic solution of described working electrode electrolyzer is 0.1～0.3mol/L, described concentration sodium hydroxide is 0.01～0.1mol/L, and the volume ratio of described oil fuel and described electrolytic solution is 0.25～1.
4. the method for oil fuel electrolytic reduction according to claim 1 desulfurization is characterized in that, the sulphur content 〉=10ppm of described oil fuel.
5. the method for oil fuel electrolytic reduction according to claim 1 desulfurization is characterized in that, the described voltage that feeds toward the working electrode electrolyzer is pulsed voltage.
6. the method for oil fuel electrolytic reduction according to claim 5 desulfurization, it is characterized in that, described pulsed voltage, direct impulse voltage is-1.2～-1.8 volts, the direct impulse voltage time length is 1～2 second, reverse pulse voltage is 0.2～0.5 volt, and the reverse pulse voltage time length is 0.1～1 second.
7. the method for oil fuel electrolytic reduction according to claim 1 desulfurization is characterized in that, during solution, stirring velocity is 200rpm～600rpm in the described stirring work electrode electrolytic pool.
8. the method for oil fuel electrolytic reduction according to claim 1 desulfurization is characterized in that, behind the dropping catalyzer, catalyst consumption is 0.6～2mmol in every liter of interior total solution of working electrode electrolyzer; Described catalyzer is metal chloride.
9. the method for oil fuel electrolytic reduction according to claim 1 desulfurization is characterized in that, dropping time length 〉=10 of described catalyzer minute.
10. the method for oil fuel electrolytic reduction according to claim 1 desulfurization is characterized in that, described electrolytic reaction time 〉=20 minute.
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Cited By (3)
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| CN103602348A (en) * | 2013-10-17 | 2014-02-26 | 上海交通大学 | Gasoline extraction-reduction desulphurization method |
| US20180051217A1 (en) * | 2016-04-15 | 2018-02-22 | Baker Hughes, A Ge Company, Llc | Chemical process for sulfur reduction of hydrocarbons |
| CN110157461A (en) * | 2019-05-15 | 2019-08-23 | 上饶师范学院 | One kind being based on NaBH4Fuel oil extraction-deoxidized desulfurization method of electrochemical regeneration |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103602348A (en) * | 2013-10-17 | 2014-02-26 | 上海交通大学 | Gasoline extraction-reduction desulphurization method |
| US20180051217A1 (en) * | 2016-04-15 | 2018-02-22 | Baker Hughes, A Ge Company, Llc | Chemical process for sulfur reduction of hydrocarbons |
| US10570344B2 (en) * | 2016-04-15 | 2020-02-25 | Baker Hughes, A Ge Company, Llc | Chemical process for sulfur reduction of hydrocarbons |
| US11053447B2 (en) | 2016-04-15 | 2021-07-06 | Baker Hughes Holdings Llc | Chemical process for sulfur reduction of hydrocarbons |
| CN110157461A (en) * | 2019-05-15 | 2019-08-23 | 上饶师范学院 | One kind being based on NaBH4Fuel oil extraction-deoxidized desulfurization method of electrochemical regeneration |
| CN110157461B (en) * | 2019-05-15 | 2021-07-02 | 上饶师范学院 | Based on NaBH4Electrochemical regeneration fuel oil extraction-reduction desulfurization method |
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