CN101434864B - Coking light distillate hydrogenation modification method - Google Patents
Coking light distillate hydrogenation modification method Download PDFInfo
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Abstract
The invention relates to a method used for hydrogenation modification of coking light distillate oil; under hydrogenation refining condition, the raw material of the coking light distillate oil and hydrogen are contacted with W-Mo-Ni series of hydrogenation catalysts firstly; subsequently, naphtha distillate, coal oil distillate and diesel distillate are gained by stripping and distillation; wherein, the coal oil distillate and new hydrogen enter a low-pressure hydrogenation reactor and are contacted with Ni-series of hydrogenation catalysts; the product is separated by a gas-liquid separator; and the liquid product is used as high-quality jet fuel components and the hydrogen-rich gas is returned to the coking light distillate oil raw material and used for hydrogenation refining. The method can process the coking light distillate oil with bad quality into high-quality jet fuel, high-quality naphtha and clean diesel components by simple process, has the advantages of wide application of the raw material, flexible operation, stable running, and the like, and effectively improves the economical benefits of the enterprises.
Description
Technical field
The present invention relates to a kind of method of coking light distillate raw material hydro-upgrading, specifically coking light distillate raw material hydrogenation direct production high-quality 3
#Rocket(engine)fuel, the method for hydrotreated naphtha of production high-quality simultaneously and low-sulfur high hexadecane value diesel component is applicable to that the refinery of delayed coking unit adopts.
Background technology
The method that at present can direct production goes out qualified rocket(engine)fuel mainly contains two kinds: a kind of is that crude oil obtains kerosene(oil)fraction through air distillation, handles and obtains qualified rocket(engine)fuel product through facing hydrogen or non-hydro then; Another kind is to be raw material with the vacuum distillate, adopts the high-pressure hydrocracking technology also can direct production go out qualified rocket(engine)fuel product.First method plant investment and process cost are lower, but receive the restriction of raw material quantity, can not satisfy the fast-developing demand of air system; Though is raw material and adopt the high-pressure hydrocracking technology with the lower vacuum distillate of price, because device need be operated under HTHP, investment and tooling cost are all higher.
The delayed coking technology of residual oil is the important process process of heavy oil lighting in the refinery; Most at present refinings extensively all have delayed coking unit; Coking distillate can fractionate out coker gasoline, coker gas oil and wax tailings; But all have shortcoming of poor quality, that foreign matter content is high, must after refining, could use, generally can't produce high quality boat coal component.Coking gasoline and diesel adopts the course of processing of first fractionation back end hydrogenation or first hydrogenation aftercut basically in the prior art, and hydrogenated gasoline is as the raw material of cracking of ethylene raw material, catalytic reforming raw material or hydrogen manufacturing, and hydrogenated diesel oil is as the derv fuel oil blend component.Though above-mentioned two kinds of methods also can make coking gasoline and diesel be fully used, economic benefit needs further to improve, and the coker gasoline hydrogenation unit also through regular meeting because the too fast ordinary production that influences device of rising falls in pressure; The coker gas oil hydrogenated oil is as vehicle fuel, because country does not have profit basically to the regulation and control in market.
Along with the continuous development of civil aviaton's cause, the demand of rocket(engine)fuel constantly increases.For oil refining enterprise, rocket(engine)fuel is a high value added product, and is good in economic efficiency, and can also also can be used as the raw material of molecular sieve dewaxing unit winter as the high-grade low-freezing diesel oil blending component.Therefore, adopt coking light distillate to produce rocket(engine)fuel and can improve refinery's economic benefit.
US6294079 discloses a kind of from produce the unifining/hydrocracking combined process method of rocket(engine)fuel than heavier feedstocks.This method is passed through hydrofining reactor with raw material earlier; Get into then HP separator tell gently, in, weigh three parts; Gently, in and the part of last running get into second HP separator, residue last running gets into low severity hydrogen cracking section, product also gets into second HP separator.This method adopts two HP separators, can maximum produce rocket(engine)fuel, but technical process is complicated, invests higherly, and operating also has certain difficulty.
CN1478867A discloses a kind of method of producing rocket(engine)fuel from coking distillate.This method adopts an acidic catalyst that contains zeolite to coker gas oil or coking gasoline and diesel raw material, under appropriate processing condition, coking raw oil is carried out hydrotreatment, and product can obtain the rocket(engine)fuel product after fractionation.This method is owing to adopt an acidic catalyst, and the nitrogen content of raw oil is had certain requirement, thus be not that all coking gasoline and diesel raw materials all are suitable for, and handle naphthenic base coking distillate inferior and also acquire a certain degree of difficulty.
CN1458233A discloses a kind of method of coking full fraction oil hydrogenation refining.This method adopts the coking full fraction oil hydrogenation refining flow process, is used for production high-quality derv fuel oil fuel.This method can not obtain high-quality 3
#Rocket(engine)fuel.
Summary of the invention
To the deficiency of prior art, the invention provides a kind of coking light distillate hydrogenation modification method, to reach the raising added value of product, increase the purpose of refinery's economic benefit.
The method of coking light distillate hydrogenation modification provided by the invention comprises following content: the coking light distillate raw material at first contacts with the W-Mo-Ni series hydrocatalyst under the unifining condition with hydrogen; Pass through stripping and fractionation then; Fractionation obtains naphtha fraction, kerosene(oil)fraction and diesel oil distillate; Wherein kerosene(oil)fraction gets into a low-voltage hydrogenation reactor drum with new hydrogen, contacts with the Ni series hydrocatalyst, and product is through gas-liquid separator; Liquid product is as high-quality rocket(engine)fuel component, and hydrogen-rich gas returns the unifining of coking light distillate raw material and uses.
Coking light distillate raw material hydrofining reaction condition is: hydrogen dividing potential drop 3.4MPa～10.0MPa is preferably 4.8MPa～8.0MPa; Temperature of reaction is 260 ℃～360 ℃, is preferably 300 ℃～350 ℃; Volume space velocity is 0.5h
-1～3.0h
-1, be preferably 1.0h
-1～2.0h
-1Hydrogen to oil volume ratio is 300～800, is preferably 300～600.Kerosene(oil)fraction low-voltage hydrogenation reaction conditions is: hydrogen dividing potential drop 0.5MPa～3.0MPa is preferably 0.5MPa～2.2MPa; Temperature of reaction is 100 ℃～300 ℃, is preferably 160 ℃～240 ℃; Volume space velocity is 0.5h
-1～3.0h
-1, be preferably 0.8h
-1～2.0h
-1Hydrogen to oil volume ratio is 100～500, is preferably 200～350.
Hydrogenation process adopts two reactor drums; The coking light distillate raw material at first gets into first reactor drum; Reaction mass contacts with the catalyzer of high hydrogenation activity under comparatively high temps and pressure condition; Remove impurity and saturated a part of aromatic hydrocarbons such as most sulphur nitrogen, product gets into HP separator, in HP separator, carries out gas-liquid separation.The isolated hydrogen-rich gas of coking light distillate raw material hydrofining reaction elute recycles; Isolated liquid product gets into gas and puies forward fractionating system; The kerosene(oil)fraction that fractionates out is getting into second reactor drum; Under than the demulcent processing condition, carry out the aromatic hydrogenation saturated reaction, the aromaticity content of product and smoke point just can satisfy 3 fully like this
#The specification of quality of rocket(engine)fuel.
It is high-activity hydrofining catalyst that described Hydrobon catalyst is selected W-Mo-Ni.Its composition comprises: Tungsten oxide 99.999 35wt%～42wt%, nickel oxide 13wt%～20wt%, molybdenum oxide 12wt%～18wt%; Total metal contents in soil is at 60wt%～80wt%; Catalyzer contains refractory oxide solid support materials such as aluminum oxide, siliceous aluminum oxide, silicon oxide simultaneously; Can also contain auxiliary agents such as titanium, zirconium, phosphorus, boron, method for preparing catalyst can adopt the coprecipitation method preparation.Described low pressure hydrocatalyst for saturating arylhydrocarbon is the Ni series catalysts; Its nickel oxide content is 40wt%～60wt%; Catalyzer contains refractory oxide solid support materials such as aluminum oxide, siliceous aluminum oxide, silicon oxide simultaneously; Can contain little auxiliary, auxiliary agent such as titanium, zirconium, boron, molybdenum etc., method for preparing catalyst can adopt kneading method, pickling process or coprecipitation method etc.
Through the coking light distillate raw material that the inventive method is handled, the kerosene product that obtains can directly satisfy mercaptan sulfur less than 20 μ g/g, smoke point greater than 3 of 25mm
#The requirement of rocket(engine)fuel specification.The hydrotreated naphtha of by-product can reach S＜0.5 μ g/g, N＜0.5 μ g/g, and alkene can be used as the raw material of catalytic reforming raw material or preparing ethylene by steam cracking less than 1v%; Hydrogenated diesel oil can be used as low-sulfur high hexadecane value diesel oil blending component.
The over point of described coking light distillate raw material is generally 30～70 ℃, and final boiling point is generally 320～380 ℃.Contents such as concrete processing condition can be confirmed by those skilled in the art according to material elementses such as raw material properties, quality product requirements.
The invention has the advantages that: through optimize technical process and operational condition (raw material at first warp than the unifining under the severe condition; Kerosene(oil)fraction after the unifining carries out the low-voltage hydrogenation reaction; The new hydrogen of reactive system is adopted in the reaction of kerosene low-voltage hydrogenation; Isolating hydrogen-rich gas is as the hydrogen make-up of raw material hydrofining reaction behind the kerosene low-voltage hydrogenation); And the catalyzer matching scheme of optimizing (raw material unifining and kerosene(oil)fraction low-voltage hydrogenation adopt the catalyzer matching scheme of optimizing), can be converted into the higher rocket(engine)fuel component of value, by-product high-quality hydrotreated naphtha and low-sulfur high hexadecane value diesel oil blending component simultaneously with being worth lower coking light distillate.Technical process is simple relatively, reduced the operating severity of system, is prone to coking, short problem of operational cycle when having overcome the independent hydrogenation of coker gasoline.Raw oil flexibility of the present invention is strong, can process various coking light distillates of different nature, and quality product can meet the demands fully.The device flexibility of operation is big, according to the variant prodn purpose, only needs the adjusting process condition can satisfy production high-quality 3
#The requirement of rocket(engine)fuel, dewaxing by molecular sieve raw material or high-grade low-freezing diesel oil blending component.
Description of drawings
Fig. 1 is the inventive method process flow diagram.
Wherein 1 is the coking light distillate raw material, and 2 is recycle hydrogen, and 3 is coking light distillate raw material hydrofining reactor; 4 is coking light distillate raw material hydrofining reactor reaction product gas-liquid separator, and 5 is coking light distillate raw material hydrofining reactor liquid product separation column, and 6 is kerosene(oil)fraction hydrogenation saturating reactor; 7 is kerosene(oil)fraction hydrogenation saturated reaction product gas-liquid separator, and 8 are boat product of coal component, and 9 is new hydrogen; 10 is hydrotreated naphtha, and 11 is hydrogenated diesel oil.
Embodiment
Following embodiment will be described further the present invention.
Coking light distillate raw material Hydrobon catalyst is the Hydrobon catalyst FH-FS catalyzer of Fushun Petrochemical Research Institute's development and production, and kerosene(oil)fraction low-voltage hydrogenation catalyzer is the hydrocatalyst for saturating arylhydrocarbon FHJ of Fushun Petrochemical Research Institute's development and production.Its physico-chemical property is seen table 1,3
#The rocket(engine)fuel specification is seen table 2.
Get into first reactor drum after coking light distillate raw material 1 and the contacted with hydrogen, at reaction conditions be: hydrogen pressure component 4.8MPa, volume space velocity 2.5h
-1, 320 ℃ of temperature of reaction, hydrogen to oil volume ratio 500: 1.Second reactor drum at reaction conditions is: hydrogen pressure component 1.8MPa, volume space velocity 2.0h
-1, 300: 1 raw oil character of 170 ℃ of temperature of reaction, hydrogen to oil volume ratio and test-results list in table 3.
Visible by table 3, hydrogenation kerosene can satisfy 3 fully
#The rocket(engine)fuel specification standards; Hydrotreated naphtha can be used as the requirement of reformer feed, also can be used as the cracking of ethylene raw material; Hydrogenated diesel oil is a fine derv fuel oil blend component.
Get into first reactor drum after coking light distillate raw material 2 and the contacted with hydrogen, at reaction conditions be: hydrogen pressure component 5.6MPa, volume space velocity 1.8h
-1, 320 ℃ of temperature of reaction, hydrogen to oil volume ratio 500: 1.Second reactor drum at reaction conditions is: hydrogen pressure component 1.7MPa, volume space velocity 1.5h
-1, 190 ℃ of temperature of reaction, hydrogen to oil volume ratio 350: 1.Raw oil character and test-results are listed in table 4.
Visible by table 4, hydrogenation kerosene can satisfy 3 fully
#The rocket(engine)fuel specification standards; Hydrotreated naphtha can be used as the requirement of reformer feed, also can be used as the cracking of ethylene raw material; Hydrogenated diesel oil is a fine derv fuel oil blend component.
Get into first reactor drum after coking light distillate raw material 3 and the contacted with hydrogen, at reaction conditions be: hydrogen pressure component 5.6MPa, volume space velocity 1.5h
-1, 330 ℃ of temperature of reaction, hydrogen to oil volume ratio 550: 1.Second reactor drum at reaction conditions is: hydrogen pressure component 1.8MPa, volume space velocity 1.2h
-1, 300: 1 raw oil character of 185 ℃ of temperature of reaction, hydrogen to oil volume ratio and test-results list in table 5.
Visible by table 5, hydrogenation kerosene can satisfy 3 fully
#The rocket(engine)fuel specification standards; Hydrotreated naphtha can be used as the requirement of reformer feed, also can be used as the cracking of ethylene raw material; Hydrogenated diesel oil is a fine derv fuel oil blend component.
Comparative Examples 1
Adopt conventional non-noble metal hydrogenation catalyst for refining (two reactor drums all use the Hydrobon catalyst FH-98 of Fushun Petrochemical Research Institute's development and production) to use same technical process and processing condition (by embodiment 3 processing condition) that result and present method comparing result that the coking light distillate raw material carries out hydrotreatment are seen table 6.Visible by table 6 result, adopt conventional non-noble metal hydrogenation catalyst for refining gained rocket(engine)fuel product smoke point can not satisfy 3
#Rocket(engine)fuel is not less than the requirement of 25mm, the quality product that other index also obtains far below the inventive method.
The character index request of table 1 catalyzer
| The catalyzer numbering | FH-FS | FHJ |
| Reactive metal | MoO 3-WO 3-NiO | NiO |
| Carrier | γ-Al 2O 3 | γ-Al 2O 3 |
| Active metallic content, wt% | 60.0～80.0 | 40.0～60.0 |
| Physical properties | ||
| Pore volume, ml/g | 0.18～0.25 | ≮0.30 |
| Specific surface area, m 2/g | ≮130 | 80～170 |
| Tap density, g/ml | 1.20～1.40 | 0.90～1.20 |
Table 23
#The rocket(engine)fuel specification
| Project | Specification |
| Density (20 ℃), g/ml | 0.775～0.830 |
| Boiling range, |
|
| 10% recovered temperature, ℃ | Be not higher than 205 |
| Final boiling point, ℃ | Be not higher than 300 |
| Sulphur, μ g/g | Be not more than 2000 |
| Mercaptan sulfur, μ g/g | Be not more than 20 |
| Aromatic hydrocarbons, m% (quality) | Be not more than 20 |
| Alkene, m% (quality) | Be not more than 5.0 |
| Smoke point, mm | Be not less than 25 |
Table 3 embodiment 1 raw oil character and test-results
| Oil property | |
Hydrotreated naphtha | Hydrogenation kerosene | Hydrogenated diesel oil |
| Density, g/cm 3 | 0.7710 | ?0.7116 | ?0.7953 | ?0.8649 |
| Boiling range (IBP～EBP), ℃ | 60～331 | ?58～140 | ?137～247 | ?243～330 |
| S，μg/g | 759 | ?＜0.5 | ?＜1.0 | ?5.6 |
| N，μg/g | 584 | ?＜0.5 | ?＜1.0 | ?2.8 |
| Mercaptan sulfur, μ g/g | ?＜1.0 | |||
| Composition/v% | ||||
| Alkene | ?38.2 | ?＜1.0 | ?＜0.1 | |
| Aromatic hydrocarbons | ?1.6 | |||
| Smoke point, mm | ?37.0 | |||
| Cetane value | ?64 |
Table 4 embodiment 2 raw oil character and test-results
| Oil property | |
Hydrotreated naphtha | Hydrogenation kerosene | Hydrogenated diesel oil |
| Density, g/cm 3 | 0.7435 | ?0.7048 | ?0.7812 | ?0.8604 |
| Boiling range (IBP～EBP), ℃ | 34～346 | ?36～142 | ?137～241 | ?243～343 |
| S，μg/g | 9300 | ?＜0.5 | ?＜1.0 | ?5.6 |
| N，μg/g | 188 | ?＜0.5 | ?＜1.0 | ?2.8 |
| Mercaptan sulfur, μ g/g | ?＜1.0 | |||
| Composition/v% | ||||
| Alkene | ?27.3 | ?＜1.0 | ?＜0.1 | |
| Aromatic hydrocarbons | ?2.7 | |||
| Smoke point, mm | ?34.0 | |||
| Cetane value | ?58 |
Table 5 embodiment 3 raw oil character and test-results
| Oil property | |
Hydrotreated naphtha | Hydrogenation kerosene | Hydrogenated diesel oil |
| Density, g/cm 3 | 0.7511 | ?0.7028 | ?0.7809 | ?0.8569 |
| Boiling range (IBP～EBP), ℃ | 54～336 | ?58～160 | ?157～239 | ?243～338 |
| S，μg/g | 9300 | ?＜0.5 | ?＜1.0 | ?5.6 |
| N，μg/g | 188 | ?＜0.5 | ?＜1.0 | ?2.8 |
| Mercaptan sulfur, μ g/g | ?＜1.0 | |||
| Composition/v% | ||||
| Alkene | ?33.8 | ?＜1.0 | ?＜0.1 | |
| Aromatic hydrocarbons | ?3.8 | |||
| Smoke point, mm | ?31.5 | |||
| Cetane value | ?55 |
Table 6 comparative example 1 and the inventive method comparative test result
| Oil property | |
Conventional hydrogenation kerosene | Present method hydrogenation kerosene |
| Density, g/cm 3 | 0.7421 | 0.7816 | 0.7809 |
| Boiling range (IBP～EBP), ℃ | 54～336 | 153～243 | 157～239 |
| S，μg/g | 9300 | 76 | ＜1.0 |
| N，μg/g | 188 | 9.7 | ＜1.0 |
| Mercaptan sulfur, μ g/g | ＜1.0 | ＜1.0 | |
| Composition/v% | |||
| Aromatic hydrocarbons | 24.8 | 3.8 | |
| Smoke point, mm | 22.6 | 31.5 |
Claims (7)
1. coking light distillate hydrogenation modification method; Comprise following content: the coking light distillate raw material at first contacts with the W-Mo-Ni series hydrocatalyst under the unifining condition with hydrogen; Pass through stripping and fractionation then, fractionation obtains naphtha fraction, kerosene(oil)fraction and diesel oil distillate, and wherein kerosene(oil)fraction gets into a low-voltage hydrogenation reactor drum with new hydrogen; Contact with the Ni series hydrocatalyst; Product is through gas-liquid separator, and liquid product is as high-quality rocket(engine)fuel component, and hydrogen-rich gas returns the unifining of coking light distillate raw material and uses;
Wherein W-Mo-Ni series hydrocatalyst reactive metal composition comprises: Tungsten oxide 99.999 35wt%～42wt%, nickel oxide 13wt%～20wt%, molybdenum oxide 12wt%～18wt% are 60wt%～80wt% in oxide compound reactive metal total content; The Ni series catalysts is 40wt%～60wt% in nickel oxide content;
Wherein the over point of coking light distillate raw material is 30～70 ℃, and final boiling point is 320～380 ℃.
2. according to the described method of claim 1, it is characterized in that coking light distillate raw material hydrofining reaction condition is: hydrogen dividing potential drop 3.4MPa～10.0MPa, temperature of reaction is 260 ℃～360 ℃, volume space velocity is 0.5h
-1～3.0h
-1, hydrogen to oil volume ratio is 300～800.
3. according to the described method of claim 1, it is characterized in that kerosene(oil)fraction low-voltage hydrogenation reaction conditions is: hydrogen dividing potential drop 0.5MPa～3.0MPa, temperature of reaction is 100 ℃～300 ℃, volume space velocity is 0.5h
-1～3.0h
-1, hydrogen to oil volume ratio is 100～500.
4. according to the described method of claim 1, it is characterized in that coking light distillate raw material hydrofining reaction condition is: the hydrogen dividing potential drop is 4.8MPa～8.0MPa, and temperature of reaction is 300 ℃～350 ℃, and volume space velocity is 1.0h
-1～2.0h
-1, hydrogen to oil volume ratio is 300～600.
5. according to the described method of claim 1, it is characterized in that kerosene(oil)fraction low-voltage hydrogenation reaction conditions is: the hydrogen dividing potential drop is 0.5MPa～2.2MPa, and temperature of reaction is 160 ℃～240 ℃, and volume space velocity is 0.8h
-1～2.0h
-1, hydrogen to oil volume ratio is 200～350.
6. according to the described method of claim 1, it is characterized in that W-Mo-Ni series hydrocatalyst and Ni series catalysts contain the refractory oxide solid support material.
7. according to the described method of claim 1, it is characterized in that the isolated hydrogen-rich gas of coking light distillate raw material hydrofining reaction elute recycles.
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| CN101942335B (en) * | 2009-07-09 | 2013-04-10 | 中国石油化工股份有限公司 | Gasoline and diesel oil combined hydrogenation process |
| CN101942334B (en) * | 2009-07-09 | 2013-10-09 | 中国石油化工股份有限公司 | Production method of molecular sieve dewaxing raw material |
| CN102268292B (en) * | 2010-06-07 | 2014-02-26 | 中国石油化工集团公司 | Combined hydrogenation method |
| CN102268293B (en) * | 2010-06-07 | 2014-01-15 | 中国石油化工集团公司 | Hydrogenation combined process |
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| US3540999A (en) * | 1969-01-15 | 1970-11-17 | Universal Oil Prod Co | Jet fuel kerosene and gasoline production from gas oils |
| CN1458233A (en) * | 2002-05-15 | 2003-11-26 | 中国石油化工股份有限公司 | Process for coking full fraction oil hydrogenation refining |
| CN1478867A (en) * | 2002-08-29 | 2004-03-03 | 中国石油化工股份有限公司 | Method of producing jet fuel from coking distillate |
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- 2007-11-15 CN CN2007101583695A patent/CN101434864B/en active Active
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| US3172843A (en) * | 1960-05-03 | 1965-03-09 | Dssulfubization process | |
| US3540999A (en) * | 1969-01-15 | 1970-11-17 | Universal Oil Prod Co | Jet fuel kerosene and gasoline production from gas oils |
| CN1458233A (en) * | 2002-05-15 | 2003-11-26 | 中国石油化工股份有限公司 | Process for coking full fraction oil hydrogenation refining |
| CN1478867A (en) * | 2002-08-29 | 2004-03-03 | 中国石油化工股份有限公司 | Method of producing jet fuel from coking distillate |
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