CN100404646C - Method for modifying poor-quality diesel-oil by cut fraction - Google Patents
Method for modifying poor-quality diesel-oil by cut fraction Download PDFInfo
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- CN100404646C CN100404646C CNB2005100016852A CN200510001685A CN100404646C CN 100404646 C CN100404646 C CN 100404646C CN B2005100016852 A CNB2005100016852 A CN B2005100016852A CN 200510001685 A CN200510001685 A CN 200510001685A CN 100404646 C CN100404646 C CN 100404646C
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Abstract
The present invention relates to a method for modifying the cut fraction of poor-quality diesel oil. The raw material of the cut fraction of diesel oil and solvent are respectively filled in an extraction tower, the raw material of the cut fraction of the diesel oil is mixed with the solvent under the conditions that the pressure is normal, the extraction temperature is from 40 DEG C to 110 DEG C, and the weight ratio of the extraction solvent to the raw material is from 0.5 to 3 to 1, the tower top is provided with refined diesel oil with solvent, the tower bottom is provided with extracted oil with solvent, and sulfur and polycyclic aromatic hydrocarbon, the refined diesel oil and the extracted oil are respectively separated by a fractionation tower, and two streams of solvent separated by the fractionation tower is circularly used after the solvent is mixed. The method enables the cetane value of the cut fraction of the diesel oil to be improved more than 10 units, the desulfurization rate to reach 50%, and the polycyclic aromatic hydrocarbon to be reduced more than 60%.
Description
Technical field
The present invention relates to produce by solvent extraction process under a kind of condition of non-hydrogen the method for best buy diesel oil or diesel oil blending component, more particularly, belong to a kind of method poor-quality diesel-oil by cut fraction solvent extraction and then desulfurization and its cetane value of raising.
Background technology
Along with China's rapid economic development; particularly increasing to diesel oil distillate to the demand of best buy diesel oil; on the other hand; environmental protection department is to the increasingly stringent that requires of foreign matter content such as sulphur, nitrogen and cetane value in the diesel oil; as Europe after carrying out sulphur content in 1997 and being up to the low-sulfur new spec diesel oil index of 500ppm; European Parliament has passed through in 2000 again diesel oil sulphur content index dropped to and has been not more than 350ppm; the cetane value index is brought up to and is not less than 51; polycyclic aromatic hydrocarbons (more than two rings) is not higher than 11 heavy %, and 15 ℃ of density are not higher than 0.845 gram per centimeter
3And advise that the diesel cetane-number index is not less than 58 after 2005, and polycyclic aromatic hydrocarbons (more than two rings) is not higher than 1.0 heavy %, and 15 ℃ of density are not higher than 0.825 gram per centimeter
3California, USA resource management office (CARB) and U.S. environment management association (EMA) has also proposed the diesel oil index of high hexadecane value, low-sulfur, low aromatic hydrocarbons.At home, the new solar oil specification requirement cetane value of having implemented is not less than 45, and sulphur content is divided into and is not more than 0.20 heavy % and is not more than two kinds of specifications of 0.05 heavy %.Therefore, each oil refining enterprise all will face the problem of improving diesel quality.China is relatively loose to the requirement of diesel quality at present, and sulphur content does not also propose the requirement to aromaticity content for not being higher than 0.2 heavy %.But along with the reinforcement gradually of environmental protection consciousness, will inevitably increasingly stringent to the requirement of fuel oil quality.
The commercial Dissel oil of China mainly is made up of straight-run diesel oil, catalytic cracking diesel oil and multiple hydrogenation technique diesel oil.Along with the development trend and the import Middle East high-sulfur crude oil amount of crude oil in China heaviness, poor qualityization are increasing, the inferior quality of the diesel product of producing by crude distillation, oily use meeting serious environment pollution directly acts as a fuel.
Generally speaking, catalytic cracking diesel oil with low quality shows as that density is big, foreign matter content height, alkene, aromaticity content height such as sulphur and nitrogen, cetane value is low, gum level is high, storage stability is poor.Along with the development of heavy oil fluid catalytic cracking technology, in order to obtain better economic benefit, each oil refining enterprise improves the residual oil mixed refining amount of heavy oil catalytically cracking equipment one after another.The raising of catalytic cracking unit raw material slag-mixing amount causes the character of catalytic cracking diesel oil further to become bad.
Therefore, need the Technology of the effectively suitable China's national situation of research and development, to solve the diesel quality problem.In characterizing diesel oil character all multifactor, wherein cetane value is the compression ignite that is used for measuring fuel; The big young pathbreaker of cetane value influences what, the consumption of fuel of cold starting property, discharge.
Aromaticity content in the diesel oil will influence NO in flame temperature and the combustion processes
xDischarge, polycyclic aromatic hydrocarbons influence particulate and form, and enter in the emissions of diesel engines thing.
Sulphur in the diesel oil mainly exists with thionaphthene or dibenzothiophene form, account for more than 85% of total cure thing basically, and the character of other organic sulfide is more approaching.Sulphur atom all links to each other with two carbon atoms in all these thiophene-type sulfides.Sulphur can cause engine system corrosion and wearing and tearing, and exhaust-gas treatment system efficient is reduced, and increases particulate emissions.
The technology of upgrading commercial Dissel oil or upgrading commercial Dissel oil blend component mainly comprises the catalytic reforming of hydrofining and upgrading, non-hydrogen and adds relevant improving agent at present.
CN1289832A discloses a kind of method for modifying of catalytic cracking diesel oil, is that 3.0～10.0 MPas, temperature are that 320～440 ℃, hydrogen to oil volume ratio are 400～1000, liquid hourly space velocity is 0.2～3.0 hour in the hydrogen dividing potential drop
-1Condition under, make raw material pass through the placed in-line Hydrobon catalyst of single hop and hydrocracking catalyst and without intermediate section from.This method makes the product diesel-fuel cetane number improve 10 more than the unit than raw material, and the sulphur nitrogen content significantly reduces.
CN1340598A discloses a kind of method of poor ignition quality fuel non-hydrogen catalytic reforming, mainly be with diesel oil distillate injecting lift pipe or fluidized-bed reactor after the preheating, be lower than 600 ℃ catalyzer contact reacts with coke content≤0.3%, temperature, temperature of reaction is 250～550 ℃, and weight hourly space velocity is 1～120h
-1, the weight ratio of catalyzer and diesel oil distillate is 2～20, and the weight ratio of water vapour and diesel oil distillate is 0.01～0.15, and reaction pressure is 0.13～0.45MPa.Reaction product isolated and spent agent, spent agent Returning reactor after stripping, regeneration recycles.This method can obviously improve diesel-fuel cetane number, and to reducing foreign matter contents such as its sulphur, nitrogen certain effect is arranged.
More than diesel oil distillate is carried out in the prior art of upgrading, by under hydro condition, diesel oil distillate is carried out hydrotreatment, reach desulfurization, denitrogenation, alkene is saturated, aromatic hydrocarbons is saturated purpose, to improve diesel quality.The upgrading of this method is effective, but cost is than higher, and some at present domestic oil refining enterprises lack the means of hydrofinings or hydrocracking, even possess the means of hydrotreatment, also exists the working ability deficiency, lacks problem such as hydrogen source.Adopt the modification technology technology more complicated of catalytic cracking freshening diesel oil distillate, certain by product is arranged, and raw material is had requirement.
Summary of the invention
The objective of the invention is to provide on the basis of existing technology a kind of method of modifying poor-quality diesel-oil by cut fraction, to reduce its cetane value of its sulphur, polycyclic aromatic hydrocarbon content and raising.
Method provided by the invention comprises: diesel oil distillate raw material and solvent carry out extraction tower, in normal pressure, extraction tower tower top temperature is that 70-75 ℃, extraction solvent are 0.5-3 with the weight ratio of raw material: mix under 1 the condition, cat head is solvent-laden refined diesel oil, it at the bottom of the tower solvent-extracted oil that contains that is rich in sulphur and polycyclic aromatic hydrocarbons, isolate refined diesel oil respectively and extract oil out through separation column, recycle after the isolated two bursts of solvent of separation column.
The inventive method is raw material with the diesel oil distillate, and desulfurization degree reaches 50% more than the unit can to make the cetane value of diesel oil distillate improve 10 through solvent extraction process, and polycyclic aromatic hydrocarbons descends more than 60%.The method of physical sepn is adopted in this invention, can utilize existing full scale plant, and process cost is lower, and technology is flexible, can satisfy existing and in the future market and environmental regulation to the quality requirement of commercial Dissel oil.
Description of drawings
Accompanying drawing is the method synoptic diagram of modifying poor-quality diesel-oil by cut fraction provided by the invention.
Embodiment
Method provided by the invention is so concrete enforcement: diesel oil distillate raw material and solvent inject extraction tower respectively, in normal pressure, extraction tower tower top temperature is that 70-75 ℃, extraction solvent are 0.5-3 with the weight ratio of raw material: mix under 1 the condition, cat head is solvent-laden refined diesel oil, it at the bottom of the tower solvent-extracted oil that contains that is rich in sulphur and polycyclic aromatic hydrocarbons, isolate refined diesel oil respectively and extract oil out through separation column, recycle after the isolated two bursts of solvent of separation column.
Described diesel oil distillate raw material is selected from one or more in straight(-run) diesel distillate, the secondary processing diesel oil cut, and wherein the secondary processing diesel oil cut is selected from one or more in catalytic cracking diesel oil, catalytic pyrolysis diesel oil, coker gas oil, thermally splitting diesel oil, the viscosity breaking diesel oil.Described diesel oil distillate can be the full cut of above-mentioned cut, also can be the narrow fraction of above-mentioned cut, and the boiling spread of described diesel oil distillate is 180-360 ℃.
The solvent extraction process device is the normal pressure liquid liquid extracting knockout tower of continuously feeding, solvent is selected from one or more in furfural, the N-alkyl pyrrolidone, preferred solvent is a furfural, solvent is from the charging of extraction tower top, diesel oil distillate is from underfeed, 70-75 ℃ of tower top temperature scope in the extraction tower, the agent-oil ratio of solvent extraction (being the weight ratio of extraction solvent and raw material) is 0.5-3: 1 preferred 0.8-2: 1; In the reverse duration of contact of extraction tower internal solvent and diesel oil distillate, the inlet amount decision by diesel oil distillate and solvent was generally 0.5-3 hour.The extracting cat head is isolated solvent-laden refined diesel oil, obtains solvent-laden extraction oil at the bottom of the tower; Two strands of products adopt CO down at 140-170 ℃ at the bottom of cat head and the tower
2Or/and N
2Carry out stripping, the gained solvent cycle is used, and the refined diesel oil behind the recovery solvent can directly be made commercial Dissel oil or diesel oil blending component, and the extraction oil behind the recovery solvent can be made hydrotreatment or catalytically cracked material.
Below in conjunction with accompanying drawing method provided by the present invention is further detailed, but does not therefore limit the present invention.
Accompanying drawing is the method synoptic diagram of modifying poor-quality diesel-oil by cut fraction provided by the invention.
Diesel oil distillate after the preheating enters extraction tower 2 through pipeline 1, furfural solvent after the preheating simultaneously enters extraction tower 2 through pipeline 3, diesel oil distillate carries out the aromatic hydrocarbons extracting with furfural solvent reverse contact in extraction tower 2, wherein solvent-laden treated oil enters separation column 5 through pipeline 4, introduce separation column 5 from the stripping gas of pipeline 10 simultaneously, solvent is deviate from through separation column 5 tops of tower, be circulated to extraction tower 2 through pipeline 6,3 successively after the condensation, the tower bottoms of separation column 5 is a refined diesel oil, through pipeline 12 caterpillars, this cut can directly be made commercial Dissel oil or diesel oil blending component.
Solvent-laden extraction oil enters separation column 8 through pipeline 7, introduce separation column 8 from the stripping gas of pipeline 11 simultaneously, the de-oiling solvent is deviate from through separation column 8 tops of tower, be circulated to extraction tower 2 through pipeline 9,3 successively after the condensation, the tower bottoms of separation column 8 is the extraction oil that is rich in polycyclic aromatic hydrocarbons and thiophene-based material, through pipeline 13 caterpillars, this cut can be made hydrotreatment or catalytically cracked material.
The inventive method is raw material with the diesel oil distillate, adopt traditional solvent extraction process method, the treatment capacity of service temperature, raw material and solvent by changing extraction tower and finish are than (the reverse duration of contact in extraction tower), can obtain the refined diesel oil of different properties requirement more neatly, can make the cetane value of diesel oil distillate improve 10 more than the unit, desulfurization degree reaches 50%, and polycyclic aromatic hydrocarbons descends more than 60%, satisfies the requirement of environmental regulation and burning and exhausting.
The following examples will give further instruction to present method, but therefore not limit the present invention.
With the inlet amount of 6500 gram straight distillation light diesel oil raw materials,, enter from the solvent tower bottom through being preheated to 45 ℃ with 650 Grams Per Hours; Simultaneously 5500 gram furfural solvents (production of Hebei Gaobeidian furfural mill) with the inlet amount of 550 Grams Per Hours, are heated to 70 ℃, enter from solvent tower top.Reverse contact is after 2 hours in extraction tower, and cat head obtains solvent-laden refined diesel oil continuously, obtains solvent-laden extraction oil at the bottom of the tower continuously.With solvent-laden refined diesel oil and solvent-laden extraction oil, under 160 ℃ of conditions, adopt CO respectively
2Carry out stripping, finally obtain refined diesel oil and extract oil out; Two strands of solvents recycle after reclaiming.Straight distillation light diesel oil solvent extraction operating procedure condition and extracting the results are shown in Table 1, and the character correlation data before and after the defeated straight distillation light diesel oil solvent extraction of pipe is refining sees Table 2.
From table 1, table 2 as can be seen, straight distillation light diesel oil is behind the solvent extraction process upgrading, and the yield of refined diesel oil is 91.6 heavy %, and compares before the solvent extraction, and density reduces, and zero pour slightly increases; Diesel-fuel cetane number can improve 10 more than the unit, and sulphur content has reduced about 50%, and two rings and the above aromaticity content of two rings reduce more than 50%.
Adopt solvent extraction device and the testing sequence identical, adopts different solvent extraction process conditions, the catalytic diesel oil raw material is carried out solvent extraction, obtain refined diesel oil and extraction is oily with embodiment 1.Catalytic diesel oil solvent extraction operating procedure condition sees Table 3, and the character correlation data before and after the catalytic diesel oil solvent extraction is refining sees Table 4.
From table 3, table 4 as can be seen, because the character characteristics of catalytic diesel oil self adopt the solvent extraction process condition also relatively harsher, the ratio of extraction temperature increase, solvent and raw material strengthens.Behind the solvent extraction process upgrading, the yield of refined diesel oil is 84.1 heavy %, and density and actual gum content all reduce; The cetane value of refined diesel oil also improves 10 more than the unit, and sulphur content has reduced about 50%, and two rings and the above aromaticity content of two rings reduce more than 50%.
Table 1
| The solar oil raw material | |
| The solvent title | Furfural |
| Tower top temperature, ℃ | 70 |
| Temperature in the tower, ℃ | 62 |
| Column bottom temperature, ℃ | 45 |
| The diesel feed temperature, ℃ | 45 |
| The solvent feed temperature, ℃ | 70 |
| Agent-oil ratio (weight) | 0.85∶1 |
| Stripping gas | CO 2 |
| The stripping temperature, ℃ | 160 |
| The refined diesel oil yield, heavy % | 91.6 |
| Extract oily yield out, heavy % | 7.6 |
| Total recovery, heavy % | 99.2 |
Table 2
| |
||
| Title | Straight distillation light diesel oil | Refined diesel oil |
| Density, g/cm 3(20℃) | 0.8295 | 0.8238 |
| Zero pour, ℃ | -30 | -24 |
| Cetane value | 54.7 | 67.5 |
| Refractive index (ND 20) | 1.4638 | 1.4568 |
| Hydrogen richness, heavy % | 13.60 | 14.02 |
| Sulphur content, ppm | 1400 | 710 |
| Nitrogen content, ppm | 17 | 18 |
| Paraffinic hydrocarbons, heavy % | 49.0 | 52.9 |
| Total naphthenic hydrocarbon, heavy % | 34.1 | 35.8 |
| One ring/two rings | 21.5/10.1 | 22.9/11.9 |
| More than three rings | 2.5 | 1.0 |
| Total aromatic hydrocarbons, heavy % | 16.9 | 11.3 |
| Monocycle/two rings | 9.7/6.6 | 8.8/2.5 |
| More than three rings | 0.6 | 0.0 |
Table 3
| The catalytic diesel oil raw material | |
| The solvent title | Furfural |
| Tower top temperature, ℃ | 75 |
| Temperature in the tower, ℃ | 65 |
| Column bottom temperature, ℃ | 50 |
| The diesel feed temperature, ℃ | 50 |
| The solvent feed temperature, ℃ | 75 |
| Agent-oil ratio (weight) | 1∶1 |
| Stripping gas | CO 2 |
| The stripping temperature, ℃ | 160 |
| The refined diesel oil yield, heavy % | 84.1 |
| Extract oily yield out, heavy % | 14.6 |
| Total recovery, heavy % | 98.7 |
Table 4
| Comparative Examples 2 | |
|
| Title | Catalytic diesel oil | Refined diesel oil |
| Density, g/cm 3(20℃) | 0.8856 | 0.8624 |
| Existent gum, mg/100mL | 176 | 104 |
| Cetane value | 29.9 | 40.1 |
| Sulphur content, ppm | 2010 | 990 |
| Paraffinic hydrocarbons, heavy % | 26.5 | 35.4 |
| Total naphthenic hydrocarbon, heavy % | 19.1 | 23.9 |
| Total aromatic hydrocarbons, heavy % | 54.1 | 40.5 |
| Monocycle/two rings | 22.1/27.1 | 25.6/13.0 |
| More than three rings | 4.9 | 1.9 |
Claims (7)
1. the method for a modifying poor-quality diesel-oil by cut fraction, it is characterized in that this method comprises: diesel oil distillate raw material and solvent inject extraction tower respectively, at normal pressure, the extraction tower tower top temperature is 70-75 ℃, extraction solvent is 0.5-3 with the weight ratio of raw material: mix under 1 the condition, cat head is solvent-laden refined diesel oil, it at the bottom of the tower solvent-extracted oil that contains that is rich in sulphur and polycyclic aromatic hydrocarbons, isolate refined diesel oil respectively and extract oil out through separation column, recycle after the isolated two bursts of solvent of separation column, described solvent is selected from furfural, in the N-alkyl pyrrolidone one or more, be 0.5-3 hour the duration of contact of raw material and solvent in extraction tower.
2. according to the method for claim 1, it is characterized in that described diesel oil distillate raw material is selected from one or more in straight(-run) diesel distillate, the secondary processing diesel oil cut.
3. according to the described method of claim 2, it is characterized in that the secondary processing diesel oil cut is selected from one or more in catalytic cracking diesel oil, catalytic pyrolysis diesel oil, coker gas oil, thermally splitting diesel oil, the viscosity breaking diesel oil.
4. according to the method for claim 1, it is characterized in that described solvent is a furfural.
5. according to the method for claim 1, the weight ratio that it is characterized in that extraction solvent and diesel oil distillate charging is 0.8-2: 1.
6. according to the method for claim 1, the operational condition that it is characterized in that separation column is to adopt gaseous matter to carry out the solvent stripping under the 140-170 ℃ of condition, and recycles.
7. according to the method for claim 6, it is characterized in that gaseous matter is CO
2Or/and N
2
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2022170257A1 (en) * | 2021-02-08 | 2022-08-11 | HollyFrontier LSP Brand Strategies LLC | Methods of preparing naphthenic process oil via extraction and separation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102021025B (en) * | 2009-09-18 | 2014-04-09 | 北京金伟晖工程技术有限公司 | System and method for preparing high-quality diesel oil at low cost |
| CN102021022B (en) * | 2009-09-18 | 2014-03-26 | 北京金伟晖工程技术有限公司 | System for preparing high-quality diesel with dual-hydrogenation unit and method thereof |
| WO2011032352A2 (en) * | 2009-09-18 | 2011-03-24 | 北京金伟晖工程技术有限公司 | System for hydrogenating a raffinate to produce high quality diesel and method thereof |
| CN102382678B (en) * | 2010-08-25 | 2014-02-26 | 中国石油化工股份有限公司 | Method for producing aromatic hydrocarbon from coked gasoline |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0236021A2 (en) * | 1986-02-24 | 1987-09-09 | ENSR Corporation (a Delaware Corporation) | Process for upgrading diesel oils |
| US4761222A (en) * | 1985-12-20 | 1988-08-02 | Phillips Petroleum Company | Method for separating normally liquid organic compounds |
| CN1197834A (en) * | 1997-04-25 | 1998-11-04 | 清华大学 | Process for refining of diesel oil by solvent extraction of catalytic diesel oil to denitrify |
| CN1386823A (en) * | 2001-05-23 | 2002-12-25 | 西南石油学院 | Process for removing sulfur and arene from solvent oil |
| CN1405275A (en) * | 2001-08-04 | 2003-03-26 | 赵玉翠 | Combined process of refining catalytic diesel |
-
2005
- 2005-02-05 CN CNB2005100016852A patent/CN100404646C/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4761222A (en) * | 1985-12-20 | 1988-08-02 | Phillips Petroleum Company | Method for separating normally liquid organic compounds |
| EP0236021A2 (en) * | 1986-02-24 | 1987-09-09 | ENSR Corporation (a Delaware Corporation) | Process for upgrading diesel oils |
| CN1197834A (en) * | 1997-04-25 | 1998-11-04 | 清华大学 | Process for refining of diesel oil by solvent extraction of catalytic diesel oil to denitrify |
| CN1386823A (en) * | 2001-05-23 | 2002-12-25 | 西南石油学院 | Process for removing sulfur and arene from solvent oil |
| CN1405275A (en) * | 2001-08-04 | 2003-03-26 | 赵玉翠 | Combined process of refining catalytic diesel |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022170257A1 (en) * | 2021-02-08 | 2022-08-11 | HollyFrontier LSP Brand Strategies LLC | Methods of preparing naphthenic process oil via extraction and separation |
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