CN101967391A - Complex sulfurization and denitrification method for distillate - Google Patents
Complex sulfurization and denitrification method for distillate Download PDFInfo
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Abstract
The invention discloses a complex sulfurization and denitrification method for distillate in petrochemical industry and petroleum refining technology. Through the method, sulfides and nitrides are removed from gasoline, diesel oil and other light oil distillate and the oil quality is improved. The technical scheme comprises the following steps of: filling a complexing agent anhydrous AlCl3 and the distillate in a reactor according to a mass ratio of sulfur and nitrogen elements in the distillate to AlCl3 of 0.012-0.120; adding water serving as a complexing aid, wherein the mass ratio of the water to the AlCl3 is 0.08-0.12; carrying out complex reaction at the temperature of between 50 and 80 DEG C for 50 to 70 minutes; after the reaction is finished, making the distillate stand to split phase, wherein the standing time is 10 to 20 minutes; and finally, taking an upper oil phase out, and adding 0.5 to 2.0 volume percent of water to clean residual complex in the oil so as to prepare the refined distillate. The method has the advantages of mild reaction condition, low operating cost, simple technical flow, low equipment investment, good sulfurization and denitrification effects, and use for removing sulfides and nitrides from the distillate in the petroleum refining technology.
Description
Technical field
The present invention relates to a kind of method that is used for the distillate complexing desulfurization removing nitric of petrochemical complex and petroleum refining process.
Background technology
Distillate mainly is meant light-end products such as straight-run spirit, catalytic gasoline, straight-run diesel oil and catalytic diesel oil.Sulfide in the distillate mainly contains mercaptan, thioether, disulphide, thiophene, alkylthrophene, thionaphthene, dibenzothiophene and 4,6-dimethyl Dibenzothiophene etc., wherein mercaptan, thioether, disulphide and thiophene-type sulfide mainly are present in the gasoline fraction, and thioether, thiophene and derivative thereof mainly are present in the diesel oil distillate.Sulfide harm mainly contains two aspects: the one, equipment is caused corrosion, and hydrogenation catalyst is poisoned, influence catalyzer work-ing life; The 2nd, the SOx after the sulphides burn forms acid rain, causes topsoil.Nitride in the distillate mainly contains basic nitrogen compound and non-basic nitrogen compound two big classes, and the harm of the more non-basic nitrogen compound of harm of basic nitrogen compound is bigger.Basic nitrogen compound can cause the activity of hydrogenation catalyst and selectivity to descend or inactivation, is hydrogenating desulfurization, the inhibitor that takes off aromatic hydrocarbons; Also can cause hydrocarbon polymer polymerization in the oil product, cause oil product to darken, viscosity increases, and stability reduces.
In industrial production, hydrofining is the main method of fractional oil desulfurizing denitrogenation.Hydrofining refers in the presence of hydrogen, and with the organic sulfide in the distillate with organic nitrogen compound is converted into hydrogen sulfide and ammonia removes, used catalyzer is generally Co-Mo, Ni-Mo, several catalyzer of Ni-W through catalyzer.The oil quality that this method is produced is good, yield height, but have following problem: reaction conditions is very harsh, and the general requirement working pressure is about 4.0MPa, and temperature is at 320～370 ℃, high-pressure process even require pressure to reach 10MPa; The hydrogenation unit investment is big, and the process cost height causes the oil product cost significantly to rise.
Because there is problem economically in fraction oil hydrodesulfurizing, for most of middle-size and small-size refineries, is difficult to bear high investment and process cost.Therefore, the non-hydrogenation desulfurization and denitrogenation technology of distillate is subjected to more attention gradually.At present, non-hydrogenating desulfurization technology mainly comprises the refining and oxide purification of refining with adsorbents, extracting and refining, complexing etc.; Non-hydrodenitrification technology comprises that mainly acid-alkali refining, solvent treatment, refining with adsorbents and complexometric extraction are refining etc.Non-hydrogenation method has simply, waits easily and fast characteristics, but because technical qualification are not overripened, and many methods also rest on the laboratory study stage, needs further to explore.Exist sorbent material little such as absorption method, problems such as adsorbent reactivation energy consumption height to the absorbed dose of sulfide or nitride; Solvent extration and oxidation style face the selectivity of sulfide or nitrogen compound relatively poor, the problem that the oil product yield is low.
For complexing abstraction, the domestic and foreign literature report is more at present.Document (Bauer L N.Seperation and concentration of sulfur-containing compounds based oncomplexation.Probl Khim Nefti, 1992) DMF solution-treated sour product with metal chloride has been proposed, electron pair interacts between organic sulfide and the metal chloride, generates water miscible complex compound and is removed.This metal chloride comprises CdCl
2, CoCl
2, NiCl
2Deng.
Document (Gerald Parkinson.Another new route to deep-desulfurization ofdiesel fule.Chemical Engineering, 107 (4), 2000) a kind of pre-treatment of having reported French CNRS research reduces the doctor treatment that the organosulfur back end hydrogenation is handled.In this method, mix with under the πDian Zi receptor compound (complexing agent) of a kind of Pi-acceptor of being called and the diesel oil normal temperature and pressure, alkylation dibenzothiophene complexing in complexing agent and the oil generates a kind of insoluble complex, removes by filter, then than hydrogenating desulfurization under the mild conditions.This method sweetening effectiveness is good, but can not remove the acidic components in the oil product.
Domestic, CN03129465.0 discloses a kind of faulty wax oil solvent extraction method, and it,, extracts faulty wax oil in the temperature range of 5: 0.01～1,30～110 ℃ of agent-oil ratios or/and water is extraction agent with organic acid, water-soluble polymer.The yield of raffinating oil can reach more than 95%, and basic nitrogen removal rate can reach more than 95%, and solvent recovering rate reaches more than 99%.
Document (hair is little for Yang Hongyun, Zhao Dezhi, etc. diesel caustic washing-complexometric extraction sulfur removal technology. Fusun PetroleumCollege's journal, 23 (1), 2003) adopt the mode of caustic prescrub that diesel oil is carried out the complexing desulfurization.At complex reagent V (L2)/V (L1)=0.2, agent oil volume ratio is 0.12, and the massfraction of complexing agent metallic compound B is 0.03% o'clock, and desulfurization degree is 67.2%, and the diesel oil rate of recovery reaches 96.0%.
Document (Liu Shuzhi, Fan Yinshuai, Wang Baohui, etc. complexometric extraction removes the basic nitrogen compound in the FCC diesel oil. chemical industry progress, 27 (1), 2008) and employing AlCl
3/ methyl alcohol is made complexing extractant, has investigated its removal effect to FCC diesel oil neutral and alkali nitride.At agent-oil ratio is 1.0, and formic acid and methyl alcohol volume ratio are 1: 4, AlCl
3When consumption was 1.0g/L, reaction 3min left standstill 15min, and the denitrification percent of diesel oil reaches 96.6%, and yield can reach 97.0%.
Document (Sun Zongli, Wang Enyang, kingdom's beam. the research of diesel oil complexing desulfuration purification. oil and gas chemical industry, 32 (2), 2005) employing DMF-FeCl
3As complexing extractant, utilize the homogeneous design experimental technique to carry out the complexing experiment, and return out relevant math equation, reach best complexing sweetening effectiveness.Experimental result also shows simultaneously, adopts complexometric extraction to be difficult to sulphur is taken off to 400 * 10
-6(w) below.
How separately though the desulfurization of distillate complexometric extraction, the denitrogenation method of existing bibliographical information are more, ubiquity complexing agent consumption is big, selectivity is not high and the problem of regeneration difficulty, and desulfurization, denitrification process research, has increased the complicacy of actually operating.
Summary of the invention
The objective of the invention is: in order to remove sulfide and the nitride in the light-end products distillates such as gasoline or diesel oil, improve oil quality, the special method that proposes a kind of distillate complexing desulfurization removing nitric.
For achieving the above object, the present invention solves this technical problem by the following technical solutions: a kind of method of distillate complexing desulfurization removing nitric is characterized in that: present method blends into one fractional oil desulfurizing, denitrification process, with anhydrous AlCl
3Be complexing agent, help the network agent with water; Need predict sulphur content, the nitrogen content of distillate earlier, then with complexing agent AlCl
3, help network agent water and the distillate reactor of packing into to mix; AlCl
3Consumption press element sulphur and nitrogen element/AlCl
3Mass ratio be 0.012～0.120, quality is unit with g; Add again and help network agent water, water and AlCl
3Mass ratio be 0.08～0.12; After having fed in raw material, closed reactor stirs and heats up, and the complex reaction temperature is 50～80 ℃, reaction times 50～70min; Reaction is left standstill phase-splitting with distillate after finishing, and time of repose is 10～20min; Take out upper oil phase at last, by volume, volume is with the unit of being upgraded to, and remaining complex compound during the washing of adding 0.5～2.0% is fuel-displaced promptly gets and makes with extra care distillate.
The present invention compares with existing fractional oil desulfurizing denitrogenation method, has following beneficial effect: the reaction conditions gentleness, and temperature＜100 ℃, atmospheric operation, process cost is low; Need not hydrogen source, pressure-resistant equipment and Claus desulfurizer, technical process is simple, and facility investment is low; Can remove sulfide and nitride simultaneously, avoid loaded down with trivial details independent desulfurization, denitrogenation operation; Complexing agent takes off the gelationus effect in addition, and oil stability is improved.
Specific implementation method
The invention will be further described below by example, and the analytical procedure that experiment is adopted is as follows:
Total sulfur content adopts total sulfur content assay method (SH/T0235-92) mensuration in the oils, desulfurization degree=(sulphur content of 1-treated oil)/stock oil sulphur content; Basic nitrogen compound content adopts petroleum products neutral and alkali nitrogen analysis method (SH/T0162-92) to measure denitrification percent=(basic n content of 1-treated oil)/stock oil basic n content.
Example 1
Get sulphur content 1197 μ g/g, the straight-run spirit of basic n content 29 μ g/g is stock oil, presses element sulphur and nitrogen element/AlCl
3Mass ratio be 0.048, H
2O/AlCl
3Mass ratio be 0.10, with 0.766gAlCl
3, 0.076g water adds in the 30.0g straight-run spirit, encloses container stirs and is warming up to 60 ℃, reaction 50min.Reaction is left standstill 20min after finishing, and gets the water washing that upper oil phase adds 1.0% volume, obtains refining straight-run spirit.The treated oil sulphur content is 32 μ g/g, desulfurization degree 97.3%; Basic n content is 0, denitrification percent 100.0%.
Example 2
Get sulphur content 562 μ g/g, the straight-run spirit of basic nitrogen compound 19 μ g/g is stock oil, presses element sulphur and nitrogen element/AlCl
3Mass ratio be 0.060, H
2O/AlCl
3Mass ratio be 0.09, with 0.291g AlCl
3, 0.026g water adds in the 30.0g straight-run spirit, encloses container stirs and is warming up to 50 ℃, reaction 60min.Reaction is left standstill 15min after finishing, and gets the water washing that upper oil phase adds 0.5% volume, obtains refining straight-run spirit.The treated oil sulphur content is 13 μ g/g, desulfurization degree 97.7%; Basic n content is 0, denitrification percent 100.0%.
Example 3
Get sulphur content 619 μ g/g, the FCC gasoline of basic n content 56 μ g/g is stock oil, presses element sulphur and nitrogen element/AlCl
3Mass ratio be 0.020, H
2O/AlCl
3Mass ratio be 0.12, with 1.012gAlCl
3, 0.121g water adds in the 30.0gFCC gasoline, encloses container stirs and is warmed up to 60 ℃, reaction 60min.Reaction is left standstill 10min after finishing, and gets the water washing that upper oil phase adds 0.5% volume, obtains refining FCC gasoline.The treated oil sulphur content is 72 μ g/g, desulfurization degree 88.4%; Basic n content is 0, denitrification percent 100.0%.
Example 4
Get sulphur content 1023 μ g/g, the FCC gasoline of basic n content 86 μ g/g is stock oil, presses element sulphur and nitrogen element/AlCl
3Mass ratio be 0.017, H
2O/AlCl
3Mass ratio be 0.10, with 1.957gAlCl
3, 0.196g water adds in the 30.0gFCC gasoline, encloses container stirs and is warmed up to 65 ℃, reaction 60min.Reaction is left standstill 20min after finishing, and gets the water washing that upper oil phase adds 2.0% volume, obtains refining FCC gasoline.The treated oil sulphur content is 107 μ g/g, desulfurization degree 89.5%; Basic n content is 0, denitrification percent 100.0%.
Example 5
Get sulphur content 711 μ g/g, the straight-run diesel oil of basic n content 37 μ g/g is stock oil, presses element sulphur and nitrogen element/AlCl
3Mass ratio be 0.040, H
2O/AlCl
3Mass ratio be 0.11, with 0.561gAlCl
3, 0.062g water adds in the 30.0g straight-run diesel oil, encloses container stirs and is warmed up to 70 ℃, reaction 60min.Reaction is left standstill 15min after finishing, and gets the water washing that upper oil phase adds 1.5% volume, obtains refined straight-run diesel.The treated oil sulphur content is 34 μ g/g, desulfurization degree 95.2%; Basic n content is 0, denitrification percent 100.0%.
Example 6
Get sulphur content 1733 μ g/g, the straight-run diesel oil of basic n content 97 μ g/g is stock oil, presses element sulphur and nitrogen element/AlCl
3Mass ratio be 0.030, H
2O/AlCl
3Mass ratio be 0.10, with 1.830gAlCl
3, 0.183g water adds in the 30.0g straight-run diesel oil, encloses container stirs and is warmed up to 70 ℃, reaction 60min.Reaction is left standstill 15min after finishing, and gets the water washing that upper oil phase adds 1.5% volume, obtains refined straight-run diesel.The treated oil sulphur content is 67 μ g/g, desulfurization degree 96.1%; Basic n content is 0, denitrification percent 100.0%.
Example 7
Get sulphur content 1311 μ g/g, the FCC diesel oil of basic n content 172 μ g/g is stock oil, presses element sulphur and nitrogen element/AlCl
3Mass ratio be 0.024, H
2O/AlCl
3Mass ratio be 0.11, with 1.854gAlCl
3, 0.204g water adds in the 30.0gFCC diesel oil, encloses container stirs and is warmed up to 65 ℃, reaction 70min.Reaction is left standstill 20min after finishing, and gets the water washing that upper oil phase adds 2.0% volume, obtains refining FCC diesel oil.The treated oil sulphur content is 320 μ g/g, desulfurization degree 75.6%; Basic n content is 0, denitrification percent 100.0%.
Example 8
Get sulphur content 896 μ g/g, the FCC diesel oil of basic n content 261 μ g/g is stock oil, presses element sulphur and nitrogen element/AlCl
3Mass ratio be 0.012, H
2O/AlCl
3Mass ratio be 0.11, with 2.892gAlCl
3, 0.318g water adds in the 30.0gFCC diesel oil, encloses container stirs and is warmed up to 80 ℃, reaction 60min.Reaction is left standstill 20min after finishing, and gets the water washing that upper oil phase adds 2.0% volume, obtains refining FCC diesel oil.The treated oil sulphur content is 156 μ g/g, desulfurization degree 82.6%; Basic n content is 8 μ g/g, denitrification percent 96.9%.
Example 9
Get sulphur content 4213 μ g/g, the winterization gasoline of basic n content 5 μ g/g is a stock oil, presses element sulphur and nitrogen element/AlCl
3Mass ratio be 0.120, H
2O/AlCl
3Mass ratio be 0.09, with 1.054gAlCl
3, 0.095g water adds in the 30.0g condensate oil, encloses container stirs and is warmed up to 50 ℃, reaction 60min.Reaction is left standstill 20min after finishing, and gets upper oil phase and adds 0.5 (volume) % water washing, obtains refining winterization gasoline.The treated oil sulphur content is 142 μ g/g, desulfurization degree 96.6%; Basic n content is 0, denitrification percent 100.0%.
Example 10
Get sulphur content 2650 μ g/g, the winterization gasoline of basic n content 10 μ g/g is a stock oil, presses element sulphur and nitrogen element/AlCl
3Mass ratio be 0.120, H
2O/AlCl
3Mass ratio be 0.08, with 0.665gAlCl
3, 0.053g water adds in the 30.0g condensate oil, encloses container stirs and is warmed up to 50 ℃, reaction 60min.Reaction is left standstill 15min after finishing, and gets upper oil phase and adds 0.5 (volume) % water washing, obtains refining winterization gasoline.The treated oil sulphur content is 108 μ g/g, desulfurization degree 95.9%; Basic n content is 0, denitrification percent 100.0%.
Claims (1)
1. the method for a distillate complexing desulfurization removing nitric is characterized in that: the fractional oil desulfurizing denitrification process is blent into one, with anhydrous AlCl
3Be complexing agent, help the network agent with water; Need predict sulphur content, the nitrogen content of distillate earlier, then with complexing agent, help network agent and the distillate reactor of packing into to mix; AlCl
3Consumption press element sulphur and nitrogen element/AlCl
3Mass ratio be 0.012～0.120; Add again and help network agent water, water and AlCl
3Mass ratio be 0.08～0.12; After having fed in raw material, closed reactor stirs and heats up, and the complex reaction temperature is 50～80 ℃, reaction times 50～70min; Reaction is left standstill phase-splitting with distillate after finishing, and time of repose is 10～20min; Take out upper oil phase at last, by volume, remaining complex compound during the washing of adding 0.5～2.0% is fuel-displaced promptly gets and makes with extra care distillate.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102492463A (en) * | 2011-12-09 | 2012-06-13 | 宁夏宝塔石化集团应用技术研究院（有限公司） | Hydrocarbon washing refining method |
| CN103289728A (en) * | 2012-03-03 | 2013-09-11 | 辽宁石油化工大学 | Straight-run diesel oil desulfurating method |
| CN104194824A (en) * | 2014-08-27 | 2014-12-10 | 天津开发区信达化工技术发展有限公司 | Decolorizing, deodorizing and refining method of lubricating oil |
| CN105112094A (en) * | 2015-09-17 | 2015-12-02 | 淄博爱森石化工程有限公司 | Acid-free refining method for base oil |
| CN113881455A (en) * | 2021-10-26 | 2022-01-04 | 武汉工程大学 | Method for performing complex extraction denitrification and deslagging on waste oil distillation product oil |
| CN114874806A (en) * | 2022-04-19 | 2022-08-09 | 武汉工程大学 | Desulfurization combined reagent and method for removing thiophene sulfides in oil product by using same |
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| CN1386823A (en) * | 2001-05-23 | 2002-12-25 | 西南石油学院 | Process for removing sulfur and arene from solvent oil |
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2010
- 2010-09-30 CN CN2010105018713A patent/CN101967391A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1386823A (en) * | 2001-05-23 | 2002-12-25 | 西南石油学院 | Process for removing sulfur and arene from solvent oil |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102492463A (en) * | 2011-12-09 | 2012-06-13 | 宁夏宝塔石化集团应用技术研究院（有限公司） | Hydrocarbon washing refining method |
| CN103289728A (en) * | 2012-03-03 | 2013-09-11 | 辽宁石油化工大学 | Straight-run diesel oil desulfurating method |
| CN104194824A (en) * | 2014-08-27 | 2014-12-10 | 天津开发区信达化工技术发展有限公司 | Decolorizing, deodorizing and refining method of lubricating oil |
| CN105112094A (en) * | 2015-09-17 | 2015-12-02 | 淄博爱森石化工程有限公司 | Acid-free refining method for base oil |
| CN113881455A (en) * | 2021-10-26 | 2022-01-04 | 武汉工程大学 | Method for performing complex extraction denitrification and deslagging on waste oil distillation product oil |
| CN114874806A (en) * | 2022-04-19 | 2022-08-09 | 武汉工程大学 | Desulfurization combined reagent and method for removing thiophene sulfides in oil product by using same |
| CN114874806B (en) * | 2022-04-19 | 2024-02-13 | 武汉工程大学 | Desulfurization combined reagent and method for removing thiophene sulfides in oil products by using same |
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Application publication date: 20110209 |