CN103805245B - The method of hydrotreating of a kind of hydrocracking and hydrogenation dearomatization combination - Google Patents
The method of hydrotreating of a kind of hydrocracking and hydrogenation dearomatization combination Download PDFInfo
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Abstract
The invention discloses the method for hydrotreating of a kind of hydrocracking and hydrogenation dearomatization combination.Poor quality urges bavin and hydrogen to carry out hydrofining in gas-liquid counter current mode; The refining oil that generates carries out hydrogenation dearomatization reaction under noble metal catalyst exists; Wax oil and hydrogen carry out hydrocracking pretreatment reaction, after hydrocracking pretreated stream effluent mixes with hydrogenation dearomatization effluent, carry out hydrocracking reaction; Hydrocracking effluent, through being separated and fractionation, obtains different fractions product; Wherein cracking tail oil is circulated to hydrogenation dearomatization reactor.The present invention utilizes the feature that noble metal catalyst Hydrogenation is strong, not easily saturated monocycle with cracking and double ring arene hydrotreated lube base oil will be urged in bavin and cracked cycle oil, improve the cracking function of hydrocracking catalyst, not only can solve the limited problem of catalytic diesel oil treatment capacity, but also can light oil yield be increased substantially, and improve the quality of products.
Description
Technical field
The present invention relates to a kind of method of hydrocracking, particularly relate to the method for hydrotreating of a kind of hydrocracking and hydrogenation dearomatization combination.
Background technology
Along with crude oil heaviness, in poor quality increasingly, and market is to the minimizing of heavy oil demand, and to the increase of light oil demand, the deep conversion degree of heavy resid improves constantly.Wherein catalytic cracking is one of heavy oil means of heavy resid lighting.But the product characteristics that catalytic cracking obtains is generally poor, generally need just can obtain qualified product through further process again.In general the diesel oil distillate that catalytic cracking obtains has that aromaticity content is high, and cetane value is low, sulphur, nitrogen content high, is difficult to directly as product, and common processing means is also difficult to effectively improve its quality product.
The common method of current processing poor quality catalytic cracking diesel is hydrofining, and this technology investment is low, technology maturation, but has certain restriction to the improvement of diesel oil, generally diesel-fuel cetane number can only be improved 3-5 unit.And although the cetane value that the method for refining catalytic diesel oil significantly can improve catalytic diesel oil is mixed in hydrocracking, but the incorporation of its catalytic diesel oil is limited, if the incorporation of catalytic diesel oil is comparatively large, hydrocracking diesel product quality will significantly reduce, and improve more greatly cracking zone air speed, reduce hydrocracked product quality.
CN1156752A discloses a kind of diesel modifying technique, use hydrocracking catalyst, under the condition controlling certain nitrogen content, make the aromatic hydrocarbons in diesel oil carry out ring-opening reaction, can diesel-fuel cetane number be significantly improved, generally cetane value can be improved more than 10 units.But during due to poor quality catalytic cracking diesel that cetane value is extremely low, still can not obtain qualified product.
CN200610008420.X discloses a kind of method for hydrogen cracking producing industrial chemicals, after poor quality catalytic cracking diesel and heavy hydrogenated cracking stock being mixed in proportion, then carrying out hydrotreatment and hydrocracking, obtains the industrial chemicals of high-quality.Although more unmanageable catalytic cracking diesel oil can be converted into high-quality industrial chemicals by the method, have stricter control to the incorporation of catalytic diesel oil, the incorporation of catalytic diesel oil directly affects the quality product of hydrocracking compared with senior general.Catalytic diesel oil incorporation is generally no more than 20%, otherwise the temperature rise of refining reaction device is excessive, can not meet apparatus design requirement, and the boat coal smoke point produced can not arrive the requirement of producing 3# rocket engine fuel.
CN200610008414.4 discloses a kind of method for hydrogen cracking, first poor quality catalytic cracking diesel is carried out hydrocracking, and the raw material such as crackate and VGO is mixed into the second hydrocracking reaction district, then isolates various light-end products and hydrogenation tail oil.Although the method can produce the heavy naphtha of Gao Fangqian and the tail oil of low BMCI value, adopt two high-pressure reactors, facility investment is higher, and improves the refining stage air speed of the second hydroconversion reaction zone, harsher to the Property requirements of VGO raw material.
CN200610008415.9 discloses a kind of method for hydrogen cracking, and by heavy distillate and catalytic diesel oil respectively after hydrofining, the logistics mixing of gained, enter hydrocracking reactor, the crackate fractionation of gained obtains different fractions product.Although the method can obtain high-quality hydrocracked product, facility investment is higher.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of method of hydrotreating producing light-end products, the method catalytic diesel oil inferior is first mixed together with the wax oil through weighted BMO spaces and enters hydrocracking reactor after hydrofining and aromatic saturation, hydrocracking reactor effluent enters the product that separation column obtains different fractions, and tail oil is circulated to the cyclical operation of aromatic saturation reactor hydrogenation dearomatization.The method significantly can improve light oil yield, the Chemicals of production high-quality, improves boat coal smoke point, the product properties such as diesel cetane-number.
The method of hydrotreating of a kind of hydrocracking of the present invention and hydrogenation dearomatization combination comprises following content:
(1) adopt fixed-bed reactor, the mode that catalytic diesel oil inferior contacts with gas-liquid counter current with hydrogen enters hydrofining reactor, carries out hydrogenation desulfurization and denitrogenation reaction, the Hydrobon catalyst that in reactor, filling is conventional;
(2) hydrofining reactor generates oil and enters hydrogenation dearomatization reactor, carries out aromatic saturation in the presence of hydrogen, filling noble metal hydrogenation dearomatization catalyst in reactor;
(3) adopt fixed-bed reactor, enter hydrocracking preatreating reactors after wax oil raw material mixes with hydrogen, the Hydrobon catalyst that in reactor, filling is conventional, carries out hydrogenation desulfurization and denitrogenation reaction;
(4) after hydrocracking preatreating reactors effluent mixes with hydrogenation dearomatization reactor effluent, enter hydrocracking reactor, carry out hydrocracking reaction, the hydrocracking catalyst that in hydrocracking reactor, filling is conventional;
(5) hydrocracking reactor effluent is through being separated and fractionation, and obtain the product of different fractions, wherein tail oil is circulated to hydrogenation dearomatization reactor.
In the inventive method; wherein hydrocracking pretreating raw material is generally vacuum gas oil (VGO), usually can also comprise straight-run gas oil (AGO), wax tailings (CGO), heavy catalytic cycle oil (HCO), deasphalted oil (DAO), coal synthetic oil or coal tar one or more.Vacuum gas oil is done general not higher than 550 DEG C, and density is not more than 0.933g/cm
3, nitrogen content is no more than 1500 μ g/g, C
7insolubles is not more than 100 μ g/g, and Fe, Ca, Ni, V content sum is no more than 1.0 μ g/g.Described catalytic diesel oil density inferior is generally 0.92g/cm
3~ 0.96g/cm
3, aromaticity content is 60% ~ 80%, and cetane value is 15 ~ 25, and the foreign matter content such as sulphur, nitrogen is high.In the inventive method, the mass ratio of described poor quality catalytic cracking diesel and wax oil raw material is generally 1:20 ~ 20:1, preferred 1:10 ~ 10:1.
In the inventive method, described weighted BMO spaces, hydrocracking and hydrogenation dearomatization operational condition comprise: reaction pressure 5.0 ~ 35.0MPa, preferably 6.0 ~ 19.0MPa; Average reaction temperature is 200 DEG C ~ 480 DEG C, preferably 270 DEG C ~ 450 DEG C; Volume space velocity is 0.1 ~ 15.0h
-1, preferably 0.2 ~ 3.0h
-1; Hydrogen to oil volume ratio is 100:1 ~ 2500:1, preferred 400:1 ~ 2000:1.
In the inventive method, the catalyzer that weighted BMO spaces reaction zone adopts can be various commercial catalysts, also can be prepared by state of the art, the general first Kaolinite Preparation of Catalyst carrier of hydrotreating catalyst, then uses pickling process supported active metals component.Commodity hydrogenation pretreatment catalyst mainly contains, as Fushun Petrochemical Research Institute (FRIPP) develop 3926, 3936, CH-20, FF-14, FF-18, FF-24, FF-26, FF-36, FH-98, FH-UDS, the hydrogenation catalysts such as FZC-41, the HR-416 of Inst Francais Du Petrole, the hydrogenation catalysts such as HR-448, the ICR174 of CLG company, ICR178, the hydrogenation catalysts such as ICR179, Uop Inc. is newly developed HC-P, HC-KUF-210/220, the TK-525 of Topsoe company, TK-555, the hydrogenation catalysts such as TK-557, the KF-752 of AKZO company, KF-840, KF-848, KF-901, the hydrogenation catalysts such as KF-907, above-mentioned catalyzer may be used for present invention process method after carrying out vulcanization process.
Hydrocracking catalyst generally includes Cracking Component, hydrogenation component and tackiness agent.As can be comprise any applicable hydrocracking catalyst of prior art.Cracking Component generally includes amorphous aluminum silicide and/or molecular sieve, and conventional molecular sieve is as Y type or USY type molecular sieve.Tackiness agent is generally aluminum oxide or silicon oxide.Hydrogenation component is VI race, VII race or VIII race's metal, metal oxide or metallic sulfide, is more preferably one or more in iron, chromium, molybdenum, tungsten, cobalt, nickel or its sulfide or oxide compound.With the weight of catalyzer for benchmark, hydrogenation component content is generally 5 ~ 40wt%.Specifically existing hydrocracking catalyst can be selected, also specific hydrocracking catalyst can be prepared as required.Business hydrocracking catalyst mainly contains: HC-12, HC-14, HC-24, HC-39 etc. and the FRIPP of Uop Inc. develop 3905,3955, FC-12, FC-16, FC-24, FC-32,3971,3976, FC-26, FC-28 etc., and ICR126, ICR210 etc. that CHEVRON company develops.The FC-14 catalyzer that commodity catalyst for hydro-upgrading is developed as Fushun Petrochemical Research Institute (FRIPP), the SDD-800 catalyzer etc. of Shell company of U.S. research and development.
In the inventive method, the carrier of hydrogenation dearomatization catalyst is generally aluminum oxide, amorphous silicon aluminium, silicon oxide, titanium oxide etc., can contain other auxiliary agent in carrier, as one or more in P, Si, B, Ti and Zr, hydrogenation active component is generally precious metal simultaneously.Precious metal is generally selected from Pt and/or Pd, and with catalyst weight, the content of precious metal is 0.1% ~ 1.5%.Described noble metal hydrogenation catalyst can adopt commercial catalyst, also can by the existing method preparation in this area.Noble metal catalyst such as Fushun Petrochemical Research Institute (FRIPP) develops HDO-18 catalyzer, also can by described method preparations such as CN00123141.3.
In prior art, wax oil is mixed in the method for hydrogen cracking of refining catalytic diesel oil, if adopt the method for hydrogen cracking of one-stage serial, although the hydrocracked product of high-quality can be obtained, but the incorporation of catalytic diesel oil will have strict control, limited to the treatment capacity of catalytic diesel oil, and the smoke point mixing the cetane value of the diesel product after refining and density and boat coal is greatly affected, can not as the blend component of the diesel oil of high-quality and rocket engine fuel; If adopt the method for hydrogen cracking of catalytic diesel oil and wax oil sectional feeding, although can solve the limited problem of catalytic diesel oil treatment capacity, light constituent yield is subject to a definite limitation, and quality product cannot be guaranteed.The present invention is by hydrocracking and hydrogenation dearomatization combination, utilize the feature that noble metal catalyst Hydrogenation is strong, by the monocycle of not easily hydrotreated lube base oil and cracking in catalytic diesel oil and hydrocracking turning oil and double ring arene hydrotreated lube base oil, improve the cracking function of hydrocracking catalyst, not only can solve the limited problem of catalytic diesel oil treatment capacity, and significantly can improve light oil yield, improve the quality of products, as improved petroleum naphtha, boat coal, diesel yield, improve boat coal smoke point, improve diesel cetane-number and density etc.
Accompanying drawing explanation
Fig. 1 is a kind of principle process schematic diagram of present invention process method.
Embodiment
Below in conjunction with the drawings and specific embodiments, method of the present invention is described in more detail.
As shown in Figure 1, method of the present invention is specific as follows: poor quality catalytic cracking diesel 1 and hydrogen 2 adverse current are by hydrofining reactor 3, hydrofining reactor generates oil 4 and enters hydrogenation dearomatization reactor 5, wax oil raw material 6 enters weighted BMO spaces reactor 7, effluent 8 and hydrogenation dearomatization reactor effluent 9 are mixed into hydrocracking reactor 10, hydrocracking reactor effluent 11 enters high-pressure separator 12 and is separated the gas phase 13 obtained and recycles, liquid phase 14 enters separation column 15, separation obtains gas 16, light naphthar 17, heavy naphtha stone 18, boat coal 19, diesel oil 20, tail oil 21, tail oil 21 is circulated to hydrogenation dearomatization reactor 5 cyclical operation.
Particular case of the present invention is further illustrated below by embodiment.Hydrobon catalyst is the FF-46 hydrogenation catalyst that Fushun Petrochemical Research Institute develops, and hydrocracking catalyst is FC-32, and hydrogenation dearomatization catalyst is FHDA-1.The volume ratio of Iran VGO and MIP diesel oil is 20:1.
Table 1 stock oil main character.
| Stock oil | Iran VGO | MIP diesel oil |
| Density (20 DEG C)/gcm -3 | 0.9168 | 0.9440 |
| Boiling range/DEG C | ||
| IBP/10% | 336/379 | 136/227 |
| 30%/50% | 409/433 | 252/275 |
| 70%/90% | 463/506 | 303/343 |
| 95%/EBP | 525/542 | 357/371 |
| Condensation point/DEG C | 36 | -24 |
| Carbon residue, % | 0.39 | 0.23 |
| S，% | 1.59 | 0.81 |
| N/μg·g -1 | 1281 | 914 |
| C，% | 85.99 | 89.70 |
| H，% | 12.25 | 9.40 |
| BMCI value | 47.7 | 80.1 |
| Cetane value (actual measurement) | — | ～15 |
| Mass spectrum forms, % | ||
| Paraffinic hydrocarbons | 20.3 | 13.4 |
| Total cycloalkanes | 31.9 | 8.3 |
| Total aromatic hydrocarbons | 45.3 | 78.3 |
| Colloid | 2.5 | 0.0 |
Table 2 technological condition.
| Reactor | Refining stage | Cracking zone |
| Catalyzer | FF-46 | FC-32/FF-46 |
| Reactor inlet hydrogen dividing potential drop, MPa | 15.5 | 15.5 |
| Reactor inlet hydrogen to oil volume ratio | 750:1 | 750:1 |
| Volume space velocity, h -1 | 1.0 | 1.5/15 |
| Average reaction temperature, DEG C | 385 | 394 |
| > 370 per pass conversion, v% | — | ～69 |
Table 3 technological condition.
| Reactor | Refining stage | Hydrogenation dearomatization section |
| Catalyzer | FZC/FF-46 | FHDA-1 |
| Reactor inlet hydrogen dividing potential drop, MPa | 15.5 | 15.5 |
| Reactor inlet hydrogen-oil ratio, v/v | 500:1 | 500:1 |
| Volume space velocity, h -1 | 1.5 | 2.0 |
| Average reaction temperature, DEG C | 345 | 350 |
Table 4. hydrocracked product distributes, %.
| Project | Numerical value |
| Dry gas | 1.02 |
| Liquefied gas | 1.10 |
| Light naphthar | 9.66 |
| Heavy naphtha | 37.05 |
| Boat coal | 27.80 |
| Diesel oil | 23.35 |
| C 5 ＋Liquid is received | 97.86 |
Table 5 product property.
| Cut, DEG C | <65 | 65~132 | 132~230 | 230~370 |
| Density (20 DEG C), g/cm 3 | 0.6568 | 0.7236 | 0.7787 | 0.8291 |
| Boiling range, DEG C | ||||
| IBP/10% | 26/29 | 82/91 | 135/151 | 237/263 |
| 30%/50% | 31/35 | 96/101 | 165/181 | 275/290 |
| 70%/90% | 41/54 | 108/117 | 196/210 | 312/346 |
| 95%/EBP | 58/63 | 125/130 | 218/226 | 360/368 |
| Sulphur, μ g/g | <0.5 | <0.5 | <5 | <5 |
| Nitrogen, μ g/g | <0.5 | <0.5 | ||
| Aromatic hydrocarbons, v% | 2.1 | |||
| Freezing point, DEG C | <-60 | |||
| Smoke point, mm | 30 | |||
| Condensation point, DEG C | <-50 | |||
| Cetane index (ASTM D 4737-96a) | 73.5 |
Comparative example 1
Adopt the mixing oil of conventional hydrocracking tail oil recycle to extinction flow processing Iran VGO and MIP diesel oil, volume ratio is 20:1.
Table 6 technological condition.
| Reactor | Refining stage | Cracking zone |
| Catalyzer | FF-46 | FC-32/FF-46 |
| Reactor inlet hydrogen dividing potential drop, MPa | 15.5 | 15.5 |
| Reactor inlet hydrogen to oil volume ratio | 750:1 | 750:1 |
| Volume space velocity, h -1 | 1.0 | 1.5/15 |
| Average reaction temperature, DEG C | 385 | 394 |
| > 370 per pass conversion, v% | — | ～69 |
Table 7. hydrocracked product distributes, %.
| Project | Numerical value |
| Dry gas | 1.04 |
| Liquefied gas | 1.12 |
| Light naphthar | 8.66 |
| Heavy naphtha | 27.05 |
| Boat coal | 25.80 |
| Diesel oil | 24.35 |
| C 5 ＋Liquid is received | 97.85 |
Table 8 product property.
| Cut, DEG C | <65 | 65~132 | 132~230 | 230~370 |
| Density (20 DEG C), g/cm 3 | 0.6574 | 0.7240 | 0.7787 | 0.8291 |
| Boiling range, DEG C: | ||||
| IBP/10% | 26/30 | 82/92 | 135/151 | 237/263 |
| 30%/50% | 32/37 | 98/102 | 165/183 | 276/293 |
| 70%/90% | 42/55 | 109/118 | 198/212 | 315/347 |
| 95%/EBP | 59/64 | 127/131 | 219/227 | 362/369 |
| Sulphur, μ g/g | <0.5 | <0.5 | <5 | <5 |
| Nitrogen, μ g/g | <0.5 | <0.5 | ||
| Aromatic hydrocarbons, v% | 2.3 | |||
| Freezing point, DEG C | <-60 | |||
| Smoke point, mm | 24 | |||
| Condensation point, DEG C | <-50 | |||
| Cetane index (ASTM D 4737-96a) | 65.5 |
As can be seen from embodiment, wax oil and catalytic diesel oil can produce the gasoline blending component of high-quality, industrial chemicals, boat coal and diesel oil by method of hydrotreating of the present invention.
Claims (10)
1. a method of hydrotreating for hydrocracking and hydrogenation dearomatization combination, comprises following content:
(1) adopt fixed-bed reactor, the mode that catalytic diesel oil inferior contacts with gas-liquid counter current with hydrogen enters hydrofining reactor, carries out hydrogenation desulfurization and denitrogenation reaction;
(2) hydrofining reactor generates oil and enters hydrogenation dearomatization reactor, carries out aromatic saturation in the presence of hydrogen, filling noble metal hydrogenation dearomatization catalyst in reactor;
(3) adopt fixed-bed reactor, enter hydrocracking preatreating reactors after wax oil raw material mixes with hydrogen, in reactor, filling conventional hydro catalyst for refining, carries out hydrogenation desulfurization and denitrogenation reaction;
(4) after hydrocracking preatreating reactors effluent mixes with hydrogenation dearomatization reactor effluent, enter hydrocracking reactor, carry out hydrocracking reaction, the hydrocracking catalyst that in hydrocracking reactor, filling is conventional;
(5) hydrocracking reactor effluent is through being separated and fractionation, and obtain the product of different fractions, wherein tail oil is circulated to hydrogenation dearomatization reactor.
2. in accordance with the method for claim 1, it is characterized in that, described wax oil raw material is vacuum gas oil.
3. in accordance with the method for claim 2, it is characterized in that, in described wax oil raw material, also comprise one or more in straight-run gas oil, wax tailings, heavy catalytic cycle oil, deasphalted oil, coal synthetic oil or coal tar.
4. in accordance with the method for claim 1, it is characterized in that, doing of described wax oil raw material is no more than 550 DEG C, and density is not more than 0.933g/cm
3, nitrogen content is no more than 1500 μ g/g, C
7insolubles is not more than 100 μ g/g, and Fe, Ca, Ni, V content sum is no more than 1.0 μ g/g.
5. in accordance with the method for claim 1, it is characterized in that, the density of described catalytic diesel oil inferior is 0.92g/cm
3~ 0.96g/cm
3, aromaticity content is 60% ~ 80%, and cetane value is 15 ~ 25.
6. in accordance with the method for claim 1, it is characterized in that, described catalytic diesel oil inferior and the mass ratio of wax oil raw material are 1:20 ~ 20:1.
7. in accordance with the method for claim 1, it is characterized in that, the operational condition of described hydrocracking pre-treatment, hydrocracking and hydrogenation dearomatization is: reaction pressure 5.0 ~ 35.0MPa, average reaction temperature is 200 DEG C ~ 480 DEG C, and volume space velocity is 0.1 ~ 15.0h
-1, hydrogen to oil volume ratio is 100:1 ~ 2500:1.
8. in accordance with the method for claim 1, it is characterized in that, described hydrocracking catalyst comprises Cracking Component, hydrogenation component and tackiness agent, Cracking Component comprises amorphous aluminum silicide and/or molecular sieve, tackiness agent is aluminum oxide or silicon oxide, hydrogenation component is VI race, VII race or VIII race's metal, metal oxide or metallic sulfide, and with the weight of catalyzer for benchmark, hydrogenation component content is 5 ~ 40wt%.
9. in accordance with the method for claim 1, it is characterized in that, described hydrogenation dearomatization catalyst with one or more in aluminum oxide, amorphous silicon aluminium, silicon oxide, titanium oxide for carrier, hydrogenation active component is selected from Pt and/or Pd, with the weighing scale of catalyzer, the content of hydrogenation active component is 0.1% ~ 1.5%.
10. in accordance with the method for claim 9, it is characterized in that, in described carrier, one or more containing in P, Si, B, Ti and Zr are auxiliary agent simultaneously.
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| US11084992B2 (en) * | 2016-06-02 | 2021-08-10 | Saudi Arabian Oil Company | Systems and methods for upgrading heavy oils |
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| CN100497547C (en) * | 2005-10-24 | 2009-06-10 | 中国石油化工股份有限公司 | Hydrocracking method |
| CN102344826B (en) * | 2010-08-05 | 2014-05-28 | 中国石油化工股份有限公司 | Combined hydrogenation method for producing catalytic raw material and high-quality diesel oil |
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