CN100478425C - Method for rectifying qualities of fractions of diesel oil - Google Patents
Method for rectifying qualities of fractions of diesel oil Download PDFInfo
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- CN100478425C CN100478425C CNB2004100711156A CN200410071115A CN100478425C CN 100478425 C CN100478425 C CN 100478425C CN B2004100711156 A CNB2004100711156 A CN B2004100711156A CN 200410071115 A CN200410071115 A CN 200410071115A CN 100478425 C CN100478425 C CN 100478425C
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Abstract
A process for modifying the diesel oil fraction includes such steps as chipping raw diesel oil to become heavy component and light component, hydrogenating heavy component, and hydrorefining the heavy component and light component to obtain high-quality diesel oil.
Description
Technical field
The present invention relates to a kind of method with the refining hydrocarbon ils of hydrogen, more particularly, the present invention is a kind of method of hydrofining diesel oil.
Background technology
Along with economy and developing of automobile industry, the consumption of vehicle fuel grows with each passing day, the quantity discharged of the pollutent in the vehicle exhaust (hydrocarbon polymer, carbon monoxide, carbonic acid gas, oxynitride, particulate matter etc.) is also increasing, the atmosphere polluting problem that causes is more and more serious, has caused the common concern of various countries.Expanding economy simultaneously also causes the environmental consciousness that people are more and more stronger, and more and more stricter environmental regulation.It should be noted that the material impact of vehicle fuel for the automobile product discharging, and corresponding requirement proposed, the discharging of hazardous and noxious substances will be strictly controlled in the vehicle exhaust, therefore the specification of petroleum products (fuel) also becomes more and more stricter, particularly to the control of sulphur content, to reduce the SO that engine exhaust emission goes out
xWith solid particulate matter to atmospheric pollution.The world fuel council has issued " world fuel standard " in June, 1999.The II that proposes in this standard, III class diesel oil standard require sulphur content respectively less than 300ppm, 30ppm.
Hydrotreatment is the main method of producing low-sulfur diesel-oil.Under certain temperature, pressure condition, hydrogen and raw material react on catalyzer, and sulfide and nitride are separately converted to hydrogen sulfide and ammonia.Select suitable process conditions according to raw material properties and required desulfurization degree.To existing diesel hydrotreating unit, in order to produce ultra-low-sulphur diesel, the most direct method is to increase the volume of catalyzer and improve temperature of reaction.For example depress at same reaction temperature and hydrogen branch that to handle sulphur content be the raw material of 1m%, the production sulphur content is that the volume of the required catalyzer of diesel oil of 50ppm and 15ppm is respectively that the production sulphur content is 2.0 times and 3.0 times of catalyst volume of the diesel oil of 500ppm.When air speed one timing, the temperature of reaction of producing 50ppm diesel oil is higher 30～40 ℃ than the temperature of reaction of producing 500ppm diesel oil, and reactions such as condensation, dehydrogenation have easily taken place under the high temperature, causes the reactor head coking, reactor pressure decrease increases sharply, and this will shorten the running period of catalyzer.
Another problem of diesel oil high temperature deep desulfurization process is the color deterioration of product.General diesel oil can be faint yellow because of containing heteroatomss such as nitrogen, and along with the generation of hydrodesulfurization reaction, these heteroatomss are removed, and it is colourless that diesel oil is become.But when deep desulfuration, high temperature can cause its oil product to present and have epipolic yellow-green colour, and product colour deepens, and this mainly is because at high temperature generated unstable, easy polymeric free radical, further forms the dark and difficult composition that removes of color.In order to solve color deterioration problem in the deep desulfurization process, two kinds of approach are arranged usually: (1) increases catalyst volume; (2) pressure of raising reactor.These two kinds of methods all mean a large amount of fund inputs, will increase the oil refining cost greatly.Therefore under the situation of relatively low pressure and less reactor volume, research and development reduce the diesel oil sulphur content to reduce the discharging of vehicle exhaust toxic substance, and the technology that reduces the formation of sweetening process chromoplastid simultaneously is that the refinery obtains the good both economical approach of low-sulfur diesel-oil of color.
In order to obtain the good low-sulfur diesel-oil of color, the highly active hydrogenation catalyst of the continuous research and design of people, the technical process that exploitation is advanced.
US5403470 discloses a kind of back end hydrogenation decoloring method of diesel oil distillate, this method adopts two reactors, one is counter-current reactor instead, at the index request that reaches product than the sulphur that removes raw material under the exacting terms and nitrogen, the two anti-co-current reactors that adopt are relatively removing the chromoplastid compound under the demulcent condition.Two anti-temperature and hydrogen dividing potential drops are all anti-low than one, and air speed is anti-higher than one, and this method can obtain the good low-sulfur diesel-oil of color.
US4755280 discloses a kind of secondary hydrogenation treatment process, and this method can be improved its color and oxidation stability.But adopt iron catalyst at second section, because hydrogen sulfide easily makes iron catalyst poison, hydrogenation activity sharply reduces, and two sections sulfide and amount of nitrides need be reduced to below the 10ppm, and be uneconomical economically.
US3841995 discloses the method that reduces the diesel oil sulphur content and improve color, and this method adopts noble metal catalyst at second section, and as the Pt catalyzer, the sulfide of one section generation very easily makes poisoning of catalyst, and hydrogenation activity falls very soon, and the catalyzer life cycle is short.
EP0523679 discloses a kind of two sections diesel oil fraction hydrogenating treatment processs, and this method can production sulphur content be not more than 0.05%, and the Sai Shi colorimetric is greater than-10 diesel oil.First section temperature of reaction is 350～450 ℃, and reaction pressure is 45～100kg/cm
2, two sections temperature of reaction is 200～300 ℃, reaction pressure is 45～100kg/cm
2
US6103104 discloses a kind of method that solves diesel colour.Catalyzer divides two bed fillings, and the centre is provided with gas-liquid separation equipment.Gas stripping column is divided into two portions up and down, and also there is gas-liquid separation equipment the centre.Raw material injects from the reactor middle part, through flowing out behind the reactor lower bed layer catalyzer, successively by entering gas stripping column top behind interchanger, the separator, gas is carried back liquid returning reactor upper bed layer and is decoloured, behind the separating device of inside reactor, enter gas stripping column bottom gas again and carry, can obtain the good low-sulfur diesel-oil of color at the bottom of the gas stripping column.Desulphurization reaction mainly takes place in lower bed layer, and temperature is 360～450 ℃, and upper bed layer is mainly used in decolouring, and temperature of reaction is 260～350 ℃.The reactor and the gas stripping column internal structure complexity of this invention design, inconvenient operation.
Summary of the invention
The objective of the invention is to provide on the basis of existing technology a kind of method for modifying of diesel oil distillate.
Method provided by the invention comprises:
(1), diesel raw material is cut under 280～340 ℃ gently, heavy constituent;
(2), heavy constituent, hydrogen contact with hydrogenation catalyst, at hydrogen dividing potential drop 3.0～10MPa, 350～450 ℃ of temperature of reaction, liquid hourly space velocity 0.5～1.5h
-1, hydrogen-oil ratio 400～1000v/v condition under hydrodesulfurization reaction takes place;
(3), the light constituent with heavy constituent after step (2) hydrotreatment and step (1) mixes;
(4), the blending ingredients of step (3), hydrogen contact with hydrogenation catalyst, at hydrogen dividing potential drop 3.0～10MPa, 260～350 ℃ of temperature of reaction, liquid hourly space velocity 1.0～4.0h
-1, hydrogen-oil ratio 400～1000v/v condition under olefin saturation, hydrodesulfurization reaction and part aromatic hydrocarbons saturated reaction take place, the chromoplastid in the mixture flow transforms, thereby obtains the good low-sulfur diesel-oil of color.
This method is produced the fine-quality diesel oil that sulphur content satisfies II, III class oil index in " world's fuel oil standard ", and its ASlM color is less than 1.0 simultaneously.
Description of drawings
Accompanying drawing is the method for modifying synoptic diagram of diesel oil distillate provided by the invention.
Embodiment
In the technology of the present invention, raw material was handled through four steps:
The first step, with raw material under 280～340 ℃, be cut into gently, heavy constituent, the component that boiling point is lower than this cutting temperature is a light constituent, the unsaturated olefin component all is retained in the light constituent; The component that boiling point is higher than this cutting temperature is heavy constituent, and the sulfide of difficult reaction is present in the heavy constituent.
In second step, heavy constituent, hydrogen contact with hydrogenation catalyst, at hydrogen dividing potential drop 3.0～10MPa, 350～450 ℃ of temperature of reaction, liquid hourly space velocity 0.5～1.5h
-1, hydrogen-oil ratio 400～1000v/v condition under hydrodesulfurization reaction takes place, remove the sulfide of difficult reaction.
The 3rd step is with the light constituent mixing of the heavy constituent after the second step hydrotreatment and the first step.
In the 4th step, blending ingredients, the hydrogen in the 3rd step contact with hydrogenation catalyst, at hydrogen dividing potential drop 3.0～10MPa, 260～350 ℃ of temperature of reaction, liquid hourly space velocity 1.0～4.0h
-1, hydrogen-oil ratio 400～1000v/v condition under olefin saturation, hydrodesulfurization reaction and part aromatic hydrocarbons saturated reaction take place, the coloured intermediate in the mixture flow transforms, thereby obtains the good low-sulfur diesel-oil of color.The four-step reaction condition relaxed than second step, was fit to improve to greatest extent product colour.
Described diesel raw material is one or more the mixture that is selected from catalytic cracking diesel oil, straight-run diesel oil, coker gas oil or thermally splitting diesel oil.
Second step and used hydrogenation catalyst of the 4th step can be VIB and the VIII family non-precious metal catalysts that loads on the suitable carrier, VIB is Mo or W normally, VIII family is Ni or Co normally, be typically Ni-W, Co-Mo, Ni-Mo catalyzer, other catalyzer with hydrogenating function also can be used for this hydrogenation process.Support of the catalyst is generally unformed aluminum oxide, silica-alumina supports or absorbent charcoal carrier.Catalyst system therefor can be identical catalyzer in two reactors, and as Ni-W catalyzer or Co-Mo catalyzer, also different catalyzer is Co-Mo/Al as the catalyzer in first reactor
2O
3, second interior catalyzer of reactor is Ni-W/C or Ni-Mo/C.Catalyzer with high hydrogenation activity especially is fit to this reaction process.The catalyst in reactor filling also can be divided into a plurality of beds as required.
Below in conjunction with accompanying drawing method provided by the present invention is further detailed.
Accompanying drawing is the method for modifying synoptic diagram of diesel oil distillate provided by the invention.
The flow process of this method is described below: stock oil is cut into light constituent and heavy constituent, and wherein light constituent contains whole alkene, and the sulfide overwhelming majority of difficult reaction concentrates in the heavy constituent.Heavy constituent are boosted through pipeline 1 incoming stock pump 2, heavy constituent after boosting are passed through interchanger 4 (with the product heat exchange of reactor 13), pipeline 5, interchanger 6 (with the product heat exchange of reactor 10) successively through pipeline 3, mix after pipeline 7 enters process furnace 8 with hydrogen from pipeline 32, heating is after pipeline 9 enters reactor 10, by contacting, under hot conditions, remove the sulfide of difficult reaction with hydrogenation catalyst.
The product of reactor 10 mixes with the light constituent through pipeline 33, feedstock pump 34, pipeline 35, interchanger 36, pipeline 37 successively through pipeline 11, through pipeline 12 again with from circulating hydrogen, the fresh hydrogen of pipeline 28,29 are mixed after pipeline 31 enters reactor 13 respectively, under the catalyzer existence condition, remove the sulfide that contains in the light constituent, saturation of olefins etc.The effluent of reactor 13 enters high-pressure separator 17 successively behind pipeline 14, interchanger 4, pipeline 15, air-cooler 16, in separator, be divided into gas-liquid two-phase, wherein gas phase is a hydrogen rich stream, wherein is mainly hydrogen, comprises partial vulcanization hydrogen, ammonia and lighter hydrocarbons simultaneously.Hydrogen rich stream is separated into two parts after pipeline 25 enters recycle compressor 26 compressions, wherein a part through pipeline 27 with mix from the fresh hydrogen of pipeline 30 after enter reactor 10 at last and recycle, another part then through pipeline 28 with mix from the fresh hydrogen of pipeline 29 after enter reactor 13 at last and recycle.
The liquid phase stream that comes out in separator 17 bottoms enters light pressure separator 19 through pipeline 18 further to be separated, gas phase is drawn through pipeline 24, liquid phase enters stripping tower 21 again through pipeline 20, the raw gasline of cat head is drawn through pipeline 23, bottom product is the good low-sulfur diesel-oil of color, and this product is lowered the temperature after pipeline 22 is drawn through interchanger 36 (with the light constituent heat exchange).
Through after the art breading of the present invention, can produce the fine-quality diesel oil that sulphur content satisfies II, III class oil index in " world's fuel oil standard ", its ASlM color is less than 1.0 simultaneously.
The following examples will give further instruction to present method, but therefore not limit present method.
The catalyzer trade mark used in embodiment and the Comparative Examples is RN-10, is produced by the Chang Ling catalyst plant.
With a kind of catalytic diesel oil is stock oil, and its density is 0.9003kg/cm
3, sulphur content is 7500ppm, and nitrogen content is 670ppm, and initial boiling point is 203 ℃, and 50% to distillate be 292 ℃ a little, and doing is 365 ℃, and the ASlM color value is 6.5.Earlier raw material is cut under 310 ℃ gently, heavy constituent, then hydrotreatment is carried out in heavy constituent, at last hydrofining is carried out in heavy constituent after the hydrotreatment and light constituent again, processing condition and test-results are as shown in table 1.As can be seen from Table 1, utilize the technology of the present invention can obtain the diesel oil more much lower than ordinary method sulphur content, the color of diesel oil improves simultaneously.
Comparative Examples 1
Comparing with embodiment 1, is that stock oil carries out the single hop operation with the full cut of identical catalytic diesel oil.Processing condition and test-results are as shown in table 1.As can be seen from Table 1, the sulphur content of this Comparative Examples is up to 438ppm, and colourity is also higher.
Mixing oil with a kind of catalytic diesel oil and straight-run diesel oil is a stock oil, and its density is 0.8739kg/cm
3, sulphur content is 1.0m%, and nitrogen content is 109ppm, and initial boiling point is 208 ℃, and 50% to distillate be 281 ℃ a little, and doing is 383 ℃, and the ASlM color value is 6.5.Earlier raw material is cut under 300 ℃ gently, heavy constituent, then hydrotreatment is carried out in heavy constituent, at last hydrofining is carried out in heavy constituent after the hydrotreatment and light constituent again, processing condition and test-results are as shown in table 2.As can be seen from Table 2, utilize the technology of the present invention can obtain low-sulfur diesel-oil, the color of diesel oil improves simultaneously.
Comparative Examples 2
Comparing with embodiment 2, is that stock oil carries out the single hop operation with the full cut of identical catalytic diesel oil.Processing condition and test-results are as shown in table 2.As can be seen from Table 2, the sulphur content of this Comparative Examples is up to 495ppm, and colourity is also higher.
Mixing oil with a kind of coker gas oil and catalytic diesel oil is a stock oil, and its density is 0.8903kg/cm
3, sulphur content is 1.25m%, and nitrogen content is 398ppm, and initial boiling point is 201 ℃, and 50% to distillate be 282 ℃ a little, and doing is 357 ℃, and the ASlM color value is 8.0.Earlier raw material is cut under 300 ℃ gently, heavy constituent, then hydrotreatment is carried out in heavy constituent, at last hydrofining is carried out in heavy constituent after the hydrotreatment and light constituent again, processing condition and test-results are as shown in table 3.As can be seen from Table 3, utilize the technology of the present invention can obtain low-sulfur diesel-oil, the color of diesel oil improves simultaneously.
Comparative Examples 3
Comparing with embodiment 3, is that stock oil carries out the single hop operation with the full cut of identical catalytic diesel oil.Processing condition and test-results are as shown in table 3.As can be seen from Table 3, the sulphur content of this Comparative Examples is up to 462ppm, and colourity is also higher.
Table 1
Table 2
Table 3
Claims (4)
1, a kind of method for modifying of diesel oil distillate, its feature exists
This method comprises:
(1), diesel raw material is cut under 280～340 ℃ gently, heavy constituent;
(2), heavy constituent, hydrogen contact with hydrogenation catalyst, at hydrogen dividing potential drop 3.0～10MPa, 350～450 ℃ of temperature of reaction, liquid hourly space velocity 0.5～1.5h
-1, hydrogen-oil ratio 400～1000v/v condition under hydrodesulfurization reaction takes place;
(3), the light constituent with heavy constituent after step (2) hydrotreatment and step (1) mixes;
(4), the blending ingredients of step (3), hydrogen contact with hydrogenation catalyst, at hydrogen dividing potential drop 3.0～10MPa, 260～350 ℃ of temperature of reaction, liquid hourly space velocity 1.0～4.0h
-1, hydrogen-oil ratio 400～1000v/v condition under olefin saturation, hydrodesulfurization reaction and part aromatic hydrocarbons saturated reaction take place, the chromoplastid in the mixture flow transforms, thereby obtains the good low-sulfur diesel-oil of color.
2,, it is characterized in that described diesel raw material is one or more the mixture that is selected from catalytic cracking diesel oil, straight-run diesel oil, coker gas oil or thermally splitting diesel oil according to the method for claim 1.
3, according to the method for claim 1, it is characterized in that step (2) and the used hydrogenation catalyst of step (4) they are VIB and the VIII family non-precious metal catalysts that loads on the suitable carrier,
4, according to the method for claim 3, it is characterized in that described group vib base metal is Mo or W, VIII family base metal is Ni or Co, suitable carrier is unformed aluminum oxide, silica-alumina supports or absorbent charcoal carrier.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR101245470B1 (en) * | 2005-02-25 | 2013-03-25 | 에스케이에너지 주식회사 | Method for Preparation of Ultra Low Sulfur Diesel Fuel Having Improved Color Properties |
| CN100590179C (en) * | 2006-06-16 | 2010-02-17 | 中国石油化工股份有限公司 | Diesel oil fraction hydroupgrading process |
| CN100590180C (en) * | 2006-06-16 | 2010-02-17 | 中国石油化工股份有限公司 | Diesel oil fraction upgrading and pour point reducing process |
| CN102465015B (en) * | 2010-11-05 | 2015-01-14 | 中国石油化工股份有限公司 | Shale oil processing method |
| CN109988599B (en) * | 2017-12-29 | 2021-07-09 | 中国石油化工股份有限公司 | Flexible hydrogenation modification process for inferior diesel oil |
| CN109988600B (en) * | 2017-12-29 | 2021-07-09 | 中国石油化工股份有限公司 | Flexible hydrogenation modification process for poor diesel oil |
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| EP0523679A2 (en) * | 1991-07-19 | 1993-01-20 | Nippon Oil Co., Ltd. | A process for the production of low-sulfur diesel gas oil |
| US5403470A (en) * | 1993-01-28 | 1995-04-04 | Union Oil Company Of California | Color removal with post-hydrotreating |
| US5409599A (en) * | 1992-11-09 | 1995-04-25 | Mobil Oil Corporation | Production of low sulfur distillate fuel |
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2004
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0523679A2 (en) * | 1991-07-19 | 1993-01-20 | Nippon Oil Co., Ltd. | A process for the production of low-sulfur diesel gas oil |
| US5409599A (en) * | 1992-11-09 | 1995-04-25 | Mobil Oil Corporation | Production of low sulfur distillate fuel |
| US5403470A (en) * | 1993-01-28 | 1995-04-04 | Union Oil Company Of California | Color removal with post-hydrotreating |
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