CN101899324B - Catalytic conversion method for producing light diesel oil with high hexadecane value and low olefin gasoline - Google Patents
Catalytic conversion method for producing light diesel oil with high hexadecane value and low olefin gasoline Download PDFInfo
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Abstract
The invention relates to a catalytic conversion method for producing light diesel oil with high hexadecane value and low olefin gasoline, which comprises the following steps: leading raw material oil to be in contact with a mild conversion catalyst in a mild conversion reactor for reaction, leading the reaction temperature, the oil gas residence time, and the weight ratio of the mild conversion catalyst to the raw material oil to be sufficient to obtain reaction products including 12-60% by weight of catalytic wax oil through the reaction, wherein the reaction products further comprises the diesel oil with the high hexadecane value and the gasoline; and leading the catalytic wax oil to carry out cracking reaction in a harsh conversion reactor, leading the generated oil gas to carry out hydrogen transfer reaction and isomerization reaction under a certain reaction environment, separating and finally obtaining the reaction product including the low olefin gasoline. The method can simultaneously directly produce the light diesel oil with the high hexadecane value and the low olefin gasoline through catalytic cracking.
Description
Technical field
The present invention relates to a kind of catalysis conversion method that improves catalytic cracking solar oil and quality of gasoline.More particularly, be to improve substantially by catalytic cracking the method that catalytic cracking solar oil cetane value reduces the catalytic gasoline olefin(e) centent simultaneously.
Background technology
Demand to high-quality diesel oil in worldwide increases day by day, to the day by day minimizing of demand of oil fuel.Although vapour, diesel oil increase in demand are different and different with the area, generally worldwide will be over to the gasoline demand rate of growth to the rate of growth of diesel oil demand.Therefore, more low-cetane catalysis solar oil just is being used to the blend component as diesel oil.And in order to satisfy the demand of high-quality diesel oil, need to carry out upgrading to the catalysis solar oil, perhaps directly produce a large amount of high-quality catalysis solar oils by catalytic cracking (FCC).
In prior art, the method for catalysis solar oil upgrading is mainly comprised hydrotreatment and alkylation, but these method costs are higher.
Another method is directly to improve the quality of catalysis solar oil in catalytic cracking process.CN101171063A has disclosed a kind of improvement and has been suitable as the FCC method that diesel oil fuel is used the distillate quality of mixed oil.The method combines the inter-stage molecular separation of segmentation FCC conversion process and polycyclic aromatic hydrocarbons species.Improve the output of diesel quality overhead product at the reaction zone that in the lifter of FCC reactor, harshness is lower and higher together with the selectivity molecular separation.But the method Special attention will be given to obtains the diesel oil distillate of the high hexadecane value of enriched saturated hydrocarbon by membrane sepn.
Summary of the invention
The objective of the invention is to provide on the basis of existing technology a kind of catalysis conversion method of producing high cetane number light diesel oil and low-alkene gasoline.
The catalysis conversion method of production high cetane number light diesel oil provided by the invention and low-alkene gasoline comprises:
Stock oil contacts with the mitigation conversion catalyst in relaxing conversion reactor and reacts, the weight ratio of temperature of reaction, the oil gas residence time, mitigation conversion catalyst and stock oil is enough to make reaction to obtain comprising the reaction product that accounts for stock oil 12~60 heavy % catalytic wax oil, and this reaction product also comprises high hexadecane value diesel oil and gasoline; Described catalytic wax oil is first carried out cracking reaction at harsh conversion reactor and harsh conversion catalyst, and the oil gas of generation carries out hydrogen transfer reactions and isomerization reaction under certain reaction environment, separates the reaction product that obtains comprising low-alkene gasoline.
Described stock oil is selected from or comprises petroleum hydrocarbon and/or other mineral oil, its Petroleum Hydrocarbon is selected from one or more the mixture in vacuum gas oil, atmospheric gas oil, coker gas oil, deasphalted oil, vacuum residuum, long residuum, and other mineral oil is one or more the mixture in liquefied coal coil, tar sand oil, shale oil.
Described mitigation conversion catalyst comprises zeolite, inorganic oxide, clay.In butt, each component accounts for respectively total catalyst weight: zeolite 5 is heavy~and 40 heavy %, the preferred 10 heavy % in heavy~30; Inorganic oxide 0.5 is heavy~50 heavy %; Clay 0 is heavy~70 heavy %.Its mesolite is lived as activity and is divided, and is selected from large pore zeolite.Described large pore zeolite refers to one or more the mixture in this group zeolite that the super steady Y that is obtained by Rare Earth Y, rare earth hydrogen Y, different methods, high silicon Y consist of.
Inorganic oxide is selected from silicon-dioxide (SiO as matrix
2) and/or aluminium sesquioxide (Al
2O
3).In butt, in inorganic oxide, silicon-dioxide accounts for the 50 heavy % in heavy~90, and aluminium sesquioxide accounts for the 10 heavy % in heavy~50.
Clay is selected from one or more in kaolin, halloysite, polynite, diatomite, halloysite, saponite, rectorite, sepiolite, attapulgite, hydrotalcite, wilkinite as caking agent.
The active ingredient of described harsh conversion catalyst can be selected from molecular sieve or its mixture or the pure aluminium silicate of the y-type zeolite of Y or the HY type zeolite that contains or do not contain rare earth, the ultrastable Y-type zeolite that contains or do not contain rare earth, process chemistry and/or stabilization treatment, also can add the appropriate shape component of selecting, the carrier of catalyzer is inorganic oxide and the natural clay (as kaolin) of synthetic again.
Described reactor be selected from riser tube, etc. one or more the combination in the fluidized-bed, isodiametric fluidized-bed, upstriker transfer limes, downstriker transfer limes of linear speed, or the two or more combinations of same reactor, described combination comprises series connection or/and in parallel, and wherein riser tube is the isodiametric riser tube of routine or the riser tube of various forms reducing.
Relaxing conversion reactor can be identical with harsh conversion reactor, also can difference, the riser tube of the preferred reducing of harsh conversion reactor, about the more detailed description of this reactor referring to CN1237477A.
The reaction conditions that relaxes conversion reactor is as follows: temperature of reaction is 420~550 ℃ preferred 430~500 ℃ more preferably 430~480 ℃; The oil gas residence time is 0.1~5 second preferred 0.5~4 second more preferably 0.8~3 second; Relax conversion catalyst and stock oil weight ratio and be 1~10 preferred 1~8 more preferably 1~6; Reaction pressure is 130~450 kPas preferred 250~400 kPas.
Harsh conversion reactor can be divided into two reaction zones, and the reaction conditions of each reaction zone is as follows:
The first reaction zone mainly carries out cracking reaction, and temperature of reaction is 480 ℃~600 ℃ preferred 485~580 ℃, and the reaction times is 0.1~3 second preferred 0.5~2 second, and the weight ratio of harsh conversion catalyst and catalytic wax oil is 0.5~25: 1 preferred 1~15: 1; The weight ratio of pre-lift medium and catalytic wax oil is 0.01~2: 1 preferred 0.05~1: 1; Reaction pressure is 130~450 kPas preferred 250~400 kPas.
Second reaction zone mainly carries out hydrogen transfer reactions and isomerization reaction, and temperature of reaction is 450 ℃~550 ℃ preferred 460~530 ℃; Keep close operation mutually in second reaction zone, the beds dense phase density is 100~700 kg/ms
3Preferred 120~500 kg/ms
3The weight hourly space velocity of second reaction zone is 1~50 hour
-1Preferred 1~40 hour
-1Reaction pressure is 130~450 kPas preferred 250~400 kPas.
In a more preferred embodiment, a position, described stock oil is introduced in reactor, or in the position of identical or different height more than, described stock oil is introduced in reactor.
In a more preferred embodiment, described method also comprises separates mitigation conversion reaction product with the mitigation conversion catalyst, relax conversion catalyst and return to the mitigation conversion reactor after stripping, coke burning regeneration, product after separation comprises high hexadecane value diesel oil and catalytic wax oil, gasoline etc., and described gasoline can enter the second reaction zone reaction of harsh conversion reactor.
In a more preferred embodiment, described method also comprises separates harsh conversion reaction product with harsh conversion catalyst, and harsh conversion catalyst returns to harsh conversion reactor after stripping, coke burning regeneration, and the product after separation comprises low-alkene gasoline etc.
In a more preferred embodiment, described catalytic wax oil is that initial boiling point is not less than the cut of 350 ℃.
In a more preferred embodiment, described catalytic wax oil hydrogen richness is not less than 11.0 heavy %, preferably is not less than 11.5 heavy %.
Compared with prior art, beneficial effect major embodiment of the present invention is in the following areas:
Adopt and relax conversion reactor by the optimal control of processing parameter and catalyst property, farthest with the alkane in raw material, alkylaromatic hydrocarbon side chain etc. optionally cracking enter in product solar oil cut, being mainly alkane in the composition of guaranteeing the solar oil cut, thereby can realize producing high cetane number light diesel oil by catalyzed conversion; Adopt the double-reaction area structure of harsh conversion reactor uniqueness, by the catalyzed conversion of catalytic wax oil, realize producing low olefin catalytic gasoline.Finally realize simultaneously producing high cetane number light diesel oil and low olefin catalytic gasoline by this assembly catalyze cracking technique.
Description of drawings
Accompanying drawing is the basic procedure schematic diagram of the catalysis conversion method of production high cetane number light diesel oil provided by the invention and low-alkene gasoline.
Embodiment
Further illustrate method provided by the present invention below in conjunction with accompanying drawing, but the present invention is not therefore subject to any restriction.
Accompanying drawing is the basic procedure schematic diagram of the catalysis conversion method of production high cetane number light diesel oil provided by the invention and low-alkene gasoline.
The present invention's mitigation conversion reactor used is conventional riser reactor, and harsh conversion reactor is to carry out in a kind of reducing riser reactor, about the more detailed description of this reactor referring to CN1237477A.
as shown in Figure 1, the mitigation conversion catalyst of regeneration is through regenerator sloped tube 12, controlled by guiding valve 11 and enter the pre lift zone that relaxes conversion reactor 2, the pre-lift medium also enters pre lift zone through pipeline 1, under the effect of pre-lift medium, the mitigation conversion catalyst of regeneration enters through pre lift zone and relaxes conversion reactor 2, stock oil also enters through pipeline 3 and relaxes conversion reactor 2, contact with the mitigation conversion catalyst, reaction, up, reacted finish mixture enters settling vessel 4 from leg outlet, carry out gas solid separation by cyclonic separator 5, oil gas after separation advances settling vessel collection chamber 6.Be advanced into stripping stage 7 under band charcoal reclaimable catalyst after reaction oil gas separates, adopt superheated vapour to carry out stripping at stripping stage 7, band Pd/carbon catalyst after stripping through inclined tube 8 to be generated, controlled by guiding valve 9 to enter revivifier 10 regeneration, the catalyzer after regeneration through regenerator sloped tube 12, controlled by guiding valve 11 to return to the pre lift zone that relaxes conversion reactor 2 to recycle.
Reaction product oil gas in collection chamber 6 enters follow-up separation system 14 through main oil gas piping 13, separates the dry gas that obtains and draws through pipeline 15; Separating the liquefied gas that obtains draws through pipeline 16; Separating the gasoline that obtains draws through pipeline 17; Separating the diesel oil that obtains draws through pipeline 18; Separating the catalytic wax oil that obtains draws through pipeline 19.
The first reaction zone that the catalytic wax oil of drawing from pipeline 19 enters harsh conversion reactor 20 reacts; The second reaction zone that the gasoline that separates from pipeline 17 can enter harsh conversion reactor 20 reacts.Second reaction zone can also be introduced the regenerated catalyst of reclaimable catalyst, cooling etc.Need further to separate from harsh conversion reactor 20 reaction oil gas out, reclaimable catalyst needs reprocessing cycle to use, and does not draw in figure.
The following examples will be further described the present invention, but not thereby limiting the invention.The raw material oil properties of using in embodiment and Comparative Examples is listed in respectively table 1.Embodiment relax in conversion reactor and harsh conversion reactor the catalyst A of using and catalyst B be respectively self-control and commercially available, wherein catalyst B is conventional catalytic cracking catalyst, produced by catalyzer branch office of Sinopec Group Shandong catalyst plant, trade names are MLC-500, and the character of catalyst B is listed in table 2.
Catalyst A preparation method is summarized as follows:
Water glass solution and 1 liter of free acid that to configure 2 liters of silica concentrations be 155g/L are 148g/L, Al
2O
3Content is the acidified aluminum sulfate solution of 20g/L, and above-mentioned two kinds of solution enter the flash mixer reaction simultaneously, obtain silicon sol.
Add 465g kaolin (Kaolin of Suzhou company, solid content 80 % by weight) in the silicon sol of above-mentioned preparation, pulling an oar obtained kaolin-silicon sol in 1 hour.
Contain Al
2O
3The pseudo-boehmite of 124g (Shandong Aluminum Plant, Al
2O
3Content is 33 % by weight) and the 450g deionized water mix making beating 30 minutes, then adding 25 ml concns is the hydrochloric acid (acid/Al of 31 % by weight
2O
3Mol ratio is 0.2) peptization, continue making beating 2 hours, then adding the 656g molecular sieve content is that the ground DASY0.0 molecular sieve of 32 % by weight (is a kind of overstable gamma zeolite, produced by the Shandong catalyst plant, lattice constant is 2.445nm) slurries, pulled an oar 30 minutes, and obtained the mixed serum of pseudo-boehmite and molecular sieve.
The kaolin of above-mentioned preparation-silicon sol slurries are mixed making beating 10 minutes with the pseudo-boehmite of above-mentioned preparation and the mixed serum of molecular sieve, obtain catalyst slurry, it is that 20~120 microns, silica content are that 29.9 % by weight, kaolin content are that 35.9 % by weight, alumina content are that 13.9 % by weight, molecular sieve content are the particle of 20.3 % by weight that the slurries that obtain are spray dried to diameter, and drying temperature is 180 ℃.With deionized water wash to without sodium ion for detecting, 150 ℃ of oven dry obtain the present invention's catalyst A used.
Embodiment
The present embodiment explanation is adopted method provided by the invention to carry out the selective cracking reaction and is produced high cetane number light diesel oil and low olefin catalytic gasoline situation.
The kitty cracker schema as shown in drawings, stock oil A is through pipeline 3 injecting lift pipe reactors 2, contact, react in the bottom of riser reactor with the catalyst A that is promoted by water vapor, weight ratio (abbreviation agent-oil ratio) at riser reactor inner catalyst A and stock oil A is 3: 1, the residence time of stock oil A in riser reactor is 1.6 seconds, and temperature of reaction is 450 ℃.Collection chamber pressure is 0.2 MPa, the separation system 14 of oil gas from entering the rear portion after riser tube out separates by cyclonic separator.And enter stripping stage with the reclaimable catalyst of charcoal, and the reclaimable catalyst after stripping goes revivifier regeneration, and the catalyzer after regeneration returns to riser reactor and recycles.Separation system 14 catalytic wax oil out enters the first reaction zone of reducing riser reactor 20 through pipeline 19, separation system 14 raw gasline out enters the second reaction zone of reducing riser reactor 20 through pipeline 17.
Test conditions, test-results are listed in table 3, and wherein water-oil ratio is the weight ratio abbreviation of pre-lift water vapor and corresponding stock oil, and gasoline property is listed in table 4, and diesel oil character is listed in table 5.
As can be seen from Table 3, the diesel yield of embodiment is up to 35.72 heavy %; As can be seen from Table 4, in the gasoline of embodiment 1, olefin(e) centent is only 22 volume %; The diesel oil alkane content of embodiment is up to 52.2, and diesel cetane-number is up to 48.
Table 1
Type of feed | A |
Density (20 ℃), kg/m 3 | 858.6 |
Kinematic viscosity (100 ℃), millimeter 2/ second | 4.9 |
Carbon residue, heavy % | 0.03 |
Total nitrogen, heavy % | 0.05 |
Sulphur, heavy % | 0.06 |
Carbon, heavy % | 86.3 |
Hydrogen, heavy % | 13.64 |
Heavy metal content, ppm | |
Nickel | <0.1 |
Vanadium | <0.1 |
Boiling range, ℃ | |
Initial boiling point | 290 |
10% | 372 |
30% | 415 |
50% | 440 |
70% | 470 |
90% | 502 |
Final boiling point | / |
Table 2
Catalyzer | B |
Chemical constitution, heavy % | |
Aluminum oxide | 46.4 |
Sodium oxide | 0.05 |
Apparent density, kg/m 3 | 860 |
Pore volume, ml/g | 0.12 |
Specific surface area, rice 2/ gram | 120 |
Abrasion index, heavy % hour -1 | 1.2 |
Size composition, heavy % | |
0~40 micron | 15.8 |
40~80 microns | 65.9 |
>80 microns | 18.3 |
Table 3
Embodiment | |
Relax reactor | |
Temperature of reaction, ℃ | 450 |
Reaction times, second | 1.6 |
Agent- |
3 |
Water-oil ratio | 0.05 |
Harsh reactor | |
Reaction zone I temperature, ℃ | 495 |
The reaction zone I residence time, second | 1.2 |
Reaction zone II temperature, ℃ | 485 |
Reaction zone II air speed, h -1 | 30 |
Agent- |
6 |
Water-oil ratio | 0.05 |
Products distribution, heavy % | |
Dry gas | 1.28 |
Liquefied gas | 18.64 |
Gasoline | 37.25 |
Solar oil | 35.72 |
Slurry oil | 4.33 |
Coke | 2.68 |
Loss | 0.1 |
Table 4
Gasoline property | Embodiment |
Density (20 ℃), g/cm 3 | 0.72 |
Boiling range | |
Initial boiling point | 38 |
10% | 58 |
30% | 75 |
50% | 100 |
70% | 136 |
90% | 175 |
Do, ℃ | 197 |
Alkene, v% | 22.0 |
Aromatic hydrocarbons, v% | 24.0 |
Sulphur, μ g/g | 25 |
RON | 90 |
MON | 80 |
Inductive phase, min | >500 |
Table 5
Diesel oil character | Embodiment |
Density, g.cm -3 | 0.8460 |
Refractive power | 1.4716 |
Zero pour, ℃ | -2 |
Boiling range, ℃ | |
Initial boiling point | 198 |
5% | 220 |
10% | 230 |
30% | 253 |
50% | 270 |
70% | 294 |
90% | 323 |
Final boiling point | 356 |
Form heavy % | |
Paraffinic hydrocarbons | 52.2 |
Naphthenic hydrocarbon | 24.4 |
Aromatic hydrocarbons | 23.4 |
Cetane value | 48 |
Claims (19)
1. catalysis conversion method of producing high cetane number light diesel oil and low-alkene gasoline, it is characterized in that stock oil in relaxing conversion reactor with relax conversion catalyst and contact and react, the weight ratio of temperature of reaction, the oil gas residence time, mitigation conversion catalyst and stock oil is enough to make reaction to obtain comprising the reaction product that accounts for stock oil 12~60 heavy % catalytic wax oil, and this reaction product also comprises high hexadecane value diesel oil and gasoline; Described catalytic wax oil is carried out cracking reaction in harsh conversion reactor, the oil gas of generation carries out hydrogen transfer reactions and isomerization reaction under certain reaction environment, separates the reaction product that obtains comprising low-alkene gasoline.
2. according to the method for claim 1, it is characterized in that described stock oil is selected from or comprises petroleum hydrocarbon and/or other mineral oil, its Petroleum Hydrocarbon is selected from one or more the mixture in vacuum gas oil, atmospheric gas oil, coker gas oil, deasphalted oil, vacuum residuum, long residuum, and other mineral oil is one or more the mixture in liquefied coal coil, tar sand oil, shale oil.
3. according to the method for claim 1, it is characterized in that described mitigation conversion catalyst comprises zeolite, inorganic oxide, clay, in butt, each component accounts for respectively total catalyst weight: zeolite 5 is heavy~and 40 heavy %; Inorganic oxide 0.5 is heavy~50 heavy %; Clay 0 is heavy~70 heavy %.
4. according to the method for claim 3, it is characterized in that described zeolite is selected from large pore zeolite, described large pore zeolite refers to one or more the mixture in this group zeolite that the super steady Y that is obtained by Rare Earth Y, rare earth hydrogen Y, different methods, high silicon Y consist of.
5. according to the method for claim 3, it is characterized in that described inorganic oxide is selected from silicon-dioxide and/or aluminium sesquioxide, in butt, in inorganic oxide, silicon-dioxide accounts for the 50 heavy % in heavy~90, and aluminium sesquioxide accounts for the 10 heavy % in heavy~50.
6. according to the method for claim 3, it is characterized in that described clay is selected from one or more in kaolin, polynite, diatomite, halloysite, saponite, rectorite, sepiolite, attapulgite, hydrotalcite, wilkinite.
7. according to the method for claim 1, it is characterized in that the reaction conditions that relaxes conversion is: 420~550 ℃ of temperature of reaction, 0.1~5 second oil gas residence time, the weight ratio 1~10 of mitigation conversion catalyst and stock oil.
8. according to the method for claim 7, it is characterized in that the reaction conditions that relaxes conversion is: 430~500 ℃ of temperature of reaction, 0.5~4 second oil gas residence time, the weight ratio 1~8 of mitigation conversion catalyst and stock oil.
9. according to the method for claim 8, it is characterized in that the reaction conditions that relaxes conversion is: 430~480 ℃ of temperature of reaction, 0.8~3 second oil gas residence time, the weight ratio 1~6 of mitigation conversion catalyst and stock oil.
10. according to the method for claim 1, it is characterized in that the reaction conditions of cracking reaction in harsh the conversion is: temperature of reaction is 480 ℃~600 ℃, and the reaction times is 0.1~3 second, and the weight ratio of harsh conversion catalyst and catalytic wax oil is 0.5~25: 1; The weight ratio of pre-lift medium and catalytic wax oil is 0.01~2: 1.
11. according to the method for claim 10, it is characterized in that the reaction conditions of cracking reaction in harsh the conversion is: temperature of reaction is 485~580 ℃, and the reaction times is 0.5~2 second, and the weight ratio of harsh conversion catalyst and catalytic wax oil is 1~15: 1; The weight ratio of pre-lift medium and catalytic wax oil is 0.05~1: 1.
12. according to the method for claim 1, it is characterized in that in harsh the conversion, the reaction conditions of hydrogen transfer reactions and isomerization reaction is: temperature of reaction is 450 ℃~550 ℃; Weight hourly space velocity is 1~50 hour-1.
13. according to the method for claim 12, it is characterized in that in harsh the conversion, the reaction conditions of hydrogen transfer reactions and isomerization reaction is: temperature of reaction is 460~530 ℃; Weight hourly space velocity is 1~40 hour-1.
14. the method according to claim 1, it is characterized in that described method also comprise with mitigation conversion reaction product with relax conversion catalyst and separate, relax conversion catalyst and return to the mitigation conversion reactor after stripping, coke burning regeneration, product after separation comprises high hexadecane value diesel oil and catalytic wax oil, gasoline, and described gasoline enters harsh conversion reactor and carries out hydrogen transfer reactions and isomerization reaction.
15. according to the method for claim 1, it is characterized in that described method also comprises separates harsh conversion reaction product with harsh conversion catalyst, harsh conversion catalyst returns to harsh conversion reactor after stripping, coke burning regeneration.
16. the method according to claim 1, it is characterized in that described reactor be selected from riser tube, etc. one or more the combination in the fluidized-bed, isodiametric fluidized-bed, upstriker transfer limes, downstriker transfer limes of linear speed, or the two or more combinations of same reactor, described combination comprises series connection or/and in parallel, and wherein riser tube is the isodiametric riser tube of routine or the riser tube of various forms reducing.
17. according to the method for claim 1, it is characterized in that described catalytic wax oil is that initial boiling point is not less than the cut of 350 ℃.
18. according to the method for claim 1 or 17, it is characterized in that described catalytic wax oil hydrogen richness is not less than 11.0 heavy %.
19. according to the method for claim 18, it is characterized in that described catalytic wax oil hydrogen richness is not less than 11.5 heavy %.
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US5846402A (en) * | 1997-05-14 | 1998-12-08 | Indian Oil Corporation, Ltd. | Process for catalytic cracking of petroleum based feed stocks |
CN101054533A (en) * | 2007-05-28 | 2007-10-17 | 中国石油大学(华东) | Quality modifying technique for sulfur-containing fuel oil |
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US5846402A (en) * | 1997-05-14 | 1998-12-08 | Indian Oil Corporation, Ltd. | Process for catalytic cracking of petroleum based feed stocks |
CN101054533A (en) * | 2007-05-28 | 2007-10-17 | 中国石油大学(华东) | Quality modifying technique for sulfur-containing fuel oil |
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