CN103789021B - A kind of high-nitrogen stock hydroprocessing process - Google Patents
A kind of high-nitrogen stock hydroprocessing process Download PDFInfo
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Abstract
The present invention relates to a kind of high-nitrogen stock hydroprocessing process, with high nitrogen heavy distillate for raw material, adopt two-stage process flow process, under Hydrofinishing conditions, heavy distillate raw material and hydrogen are mixed into first paragraph reaction zone, first paragraph reaction zone uses Hydrobon catalyst, the denitrification percent of first paragraph reaction zone controls to be 20% ~ 70%, gas phase after the effluent gas-liquid separation of first paragraph reaction zone continues to use after removing impurities matter, liquid phase after the effluent gas-liquid separation of first paragraph reaction zone enters second segment reaction zone and carries out hydrotreatment reaction, second segment reaction zone uses Hydrobon catalyst, second segment reaction zone reaction effluent enters separation system, obtain hydrotreatment reaction product.Compared with existing hydrotreating techniques, the inventive method can improve quality product and the working ability of device greatly, or at same quality product and working ability condition decline low operating pressure, reduces process cost.
Description
Technical field
The invention discloses a kind of hydroprocessing process, particularly a kind of two-stage hydrogenation treatment process of processing high-nitrogen stock.
Background technology
Along with the high speed development of Chinese national economy, refining of petroleum ability increases fast.Meanwhile, crude oil price remains high, and the proportion that crude oil procurement cost is accounted in oil refining total cost significantly rises, and the profit margin of oil refining enterprise reduces greatly.In addition, because crude quality is deteriorated year by year, the significantly increase of import high-sulfur height nitrogen crude runs, the requirement of environmental protection to oil refining process and petroleum product-quality is increasingly strict, and market is to the continuous increase of clear gusoline and industrial chemicals demand, makes the progress of market to hydrogen addition technology level have higher requirement.
In catalytic cracking process, the raw material of high sulfur content will cause the sulphur content of product petrol and diesel oil can not reach cleaning product requirement, but also can make the SO in catalytic cracking flue gas
xdischarge exceeds standard, and the high nitrogen-containing in catalytically cracked material will increase the consumption of catalyzer, increases process cost.Hydrotreating of FCC feedstock technology significantly can reduce sulphur nitrogen metal impurities content, improves product property, improves object product yield, therefore obtains and apply more and more widely.
Existing hydrotreating of FCC feedstock technique, as US4780193 discloses a kind of hydrorefining catalyst cracked charge method, produces the gasoline blending component that octane value is higher.CN101007964 discloses a kind of method of hydrotreating producing fine quality catalytic cracking raw material; but its working pressure is low; be not suitable for processing high-nitrogen stock; CN101987967 discloses a kind of hydroprocessing process of deep vacuum distillation wax oil; adopt two sections of flow processs; but its first paragraph uses active very weak hydrogenation protecting agent and demetalization protective material; second segment uses hydrogenating desulfurization and hydrodenitrogenation catalyst; cause unit capacity not high because monolith activity is lower during processing high nitrogen-containing raw material, or treating depth is not high.
Be deteriorated for current crude quality, foreign matter content increases, and the exploitation of crude oil decompression Shen Ba and other unconventional energy resource, make the raw material impurity content of hydrotreatment more and more higher, particularly the nitrogen content of some hydrotreated feed is higher, and during the hydrogenating materials of existing hydroprocessing process process high nitrogen-containing, need higher temperature of reaction, higher reaction pressure or lower operation air speed, the working ability of device declines, energy consumption increases simultaneously, and the operational cycle shortens.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide a kind of two-stage hydrogenation treatment process of improvement, processing high-nitrogen raw oil.Compare with existing hydrotreating techniques, greatly can improve quality product and the working ability of device, or at same quality product and working ability condition decline low operating pressure, reduce process cost.
High-nitrogen stock hydroprocessing process of the present invention comprises following content: with high nitrogen heavy distillate for raw material, adopt two-stage process flow process, under Hydrofinishing conditions, heavy distillate raw material and hydrogen are mixed into first paragraph reaction zone, first paragraph reaction zone uses Hydrobon catalyst, the denitrification percent of first paragraph reaction zone controls to be 20% ~ 70%, gas phase after the effluent gas-liquid separation of first paragraph reaction zone continues to use after removing impurities matter, liquid phase after the effluent gas-liquid separation of first paragraph reaction zone enters second segment reaction zone and carries out hydrotreatment reaction, second segment reaction zone uses Hydrobon catalyst, second segment reaction zone reaction effluent enters separation system, obtain hydrotreatment reaction product.
In the inventive method, the nitrogen content of high nitrogen heavy distillate raw material is generally 2500 more than μ g/g, is preferably 3500 more than μ g/g, is generally 3000 ~ 15000 μ g/g.The initial boiling point of high nitrogen heavy distillate raw material is generally 220 ~ 450 DEG C, and be preferably 300 ~ 420 DEG C, final boiling point is generally 500 ~ 700 DEG C, is preferably 550 ~ 650 DEG C.Be generally the raw material of catalytic cracking unit.
In the inventive method, the denitrification percent of first paragraph reaction zone preferably controls to be 30% ~ 60%.The temperature of reaction of first paragraph reaction zone is 300 ~ 480 DEG C, and reaction pressure is 5.0 ~ 20.0MPa, and hydrogen to oil volume ratio is 100:1 ~ 4000:1, and during liquid, volume space velocity is 0.2 ~ 4.0h
-1.Preferred operational condition is: temperature of reaction is 330 ~ 450 DEG C, and reaction pressure is 8.0 ~ 17.0MPa, and hydrogen to oil volume ratio is 400:1 ~ 2000:1, and during liquid, volume space velocity is 0.5 ~ 3.0h
-1.
In the inventive method, in second segment reaction zone, temperature of reaction is 250 ~ 500 DEG C, and reaction pressure is 5.0 ~ 20.0MPa, and hydrogen to oil volume ratio is 100:1 ~ 4000:1, and during liquid, volume space velocity is 1.0 ~ 10.0h
-1.Be preferably: temperature of reaction is 300 ~ 440 DEG C, and reaction pressure is 8.0 ~ 17.0MPa, and hydrogen to oil volume ratio is 400:1 ~ 2000:1, and during liquid, volume space velocity is 1.0 ~ 4.0h
-1.
In the inventive method, first paragraph reaction zone reaction effluent carries out gas-liquid separation, and gas phase removal hydrogen sulfide and ammonia Posterior circle continue to use, and can be circulated to first paragraph reaction zone, also can be delivered to second segment reaction zone.Liquid phase enters second segment reaction zone and carries out hydrotreatment reaction further.First second segment reaction zone reaction effluent carries out gas-liquid separation, gas phase removal hydrogen sulfide and ammonia Posterior circle use, also first paragraph reaction zone can be direct cycled to, liquid phase enters fractionating system, isolate petroleum naphtha, diesel oil and tail oil as required, tail oil as catalytically cracked material, or without separation, directly as catalytically cracked material.
In the inventive method, according to unit scale, first paragraph reaction zone can arrange one or several reactors, and second segment reaction zone also can arrange one or several reactors.First paragraph reaction zone and second segment reaction zone can use a set of recycle hydrogen system, also can arrange recycle hydrogen system respectively.When adopting a set of recycle hydrogen system, need to be optimized hydrogen flow path, namely the gas phase of first paragraph reaction zone reaction effluent gas-liquid separation carries out depriving hydrogen sulphide and deamination, then for second segment reaction zone, gas phase after the reaction effluent gas-liquid separation of second segment reaction zone is cycled to used in first paragraph reaction zone, and the new hydrogen that reaction process is supplemented enters second segment reaction zone.
In the inventive method, Hydrobon catalyst can be the arbitrary commerical prod in this area, also can prepare according to state of the art, add refining controlling catalyst generally with one or more in W, Mo, Ni and Co for active ingredient, 20% ~ 90% is generally with the active ingredient of oxide basis weight content in the catalyst, be generally 25% ~ 65%, Hydrobon catalyst is under response behaviour, and hydrogenation active component is sulphided state.
In the inventive method, mainly there is the reaction such as desulfurization, denitrogenation, deoxidation, aromatic saturation of raw material in first paragraph reaction zone; Second segment reaction zone proceeds the reactions such as deep hydrodesulfurizationof, denitrogenation, deoxidation, aromatic saturation occur.
Those skilled in the art it is generally acknowledged, Hydrobon catalyst has resistance to nitrogen, and the ammonia in reaction system does not have restraining effect to catalyst performance, the impact of reaction are just fallen to the factor of hydrogen partial pressure.But by learning the in-depth analysis of existing hydroprocessing technique, when processing high-nitrogen stock, reaction generates a large amount of ammonia, has a significant effect to the nitrogen removal performance of Hydrobon catalyst, when adopting this area ordinary method, need the denitrification effect needed for could obtaining under higher temperature of reaction.The present invention is by optimizing two-stage hydrocracking technical process, Hydrobon catalyst is assigned in differential responses district by suitable proportion, achieves while the identical hydrogenation removing impurities matter degree of depth, reduce temperature of reaction, improve hydrofining effluent quality, and extend running period.Meanwhile, lower temperature also can promote that aromatic saturation reacts, and denitrification reaction is generally ring-opening reaction, thus temperature of reaction is reduced further.That is, when processing same high-nitrogen stock under identical air speed, because two-stage reaction has higher reactivity worth and aromatic saturation reaction faster, its nitrogen content is directly removed to certain depth by a reactor needs higher average reaction temperature by than two reactors.The degree that this impact is estimated considerably beyond this area.Because hydrofining reaction temperature reduces greatly, thus the running period of device can be improved, or improve the working ability of device under same running period, and catalytic cracking feeds quality can be improved.Requiring catalytically cracked material quality one timing, just can improve treatment capacity or reduce working pressure, greatly will improve the economic benefit of enterprise.When particularly adopting suitable hydrogen flow path, while guarantee reactivity worth, greatly can reduce facility investment and the running expense of device, increase the economic benefit of enterprise further.
Accompanying drawing explanation
Fig. 1 is a kind of principle process flow sheet of the present invention.
Embodiment
Two-stage hydrogenation treatment process process of the present invention, a kind of idiographic flow comprises:
(1) first paragraph hydrotreating reactor filling Hydrobon catalyst; (2) stock oil and hydrogen are mixed into the reactions such as first paragraph hydrotreating reactor generation hydrogenating desulfurization, denitrogenation, deoxidation, aromatic saturation; (3) first paragraph hydrotreatment generates oil and enters high-pressure separator, and continue after the gas removal ammonia separated, hydrogen sulfide to use, the liquid separated enters second segment hydrotreating reactor; (4) first paragraph hydrotreatment generates oil and enters second segment hydrotreating reactor with hydrogen is mixed, proceeds the reactions such as hydrogenating desulfurization, denitrogenation, deoxidation, aromatic saturation occur; (5) second segment hydrotreatment generates oil and enters high-pressure separator, and the gas circulation separated uses, and the liquid separated enters fractionating system; (6) one or more in petroleum naphtha, diesel oil and tail oil can be isolated as required, tail oil as catalytic cracking unit charging, or without separation directly as catalytic cracking unit charging.
The present invention's high-nitrogen raw oil used can be one or more in the wax tailings of crude oil, deasphalted oil, shale oil and coal synthetic oil, crude oil deep vacuum distillation cut wet goods cut.
The Hydrobon catalyst used in first paragraph and second segment hydrotreatment can be conventional hydrorefining catalyst for heavy oil, generally be made up of carrier and the hydrogenation metal component be loaded on carrier, comprise group VIB active metal component in the periodic table of elements, as tungsten and/or molybdenum; And the VIIIth race's active metal component, as nickel and/or cobalt.The carrier that Hydrobon catalyst uses is inorganic refractory oxide, as aluminum oxide, amorphous silicon aluminium, silicon oxide, titanium oxide etc.The business Hydrobon catalyst that can select mainly contains: Uop Inc. develop HC-K, HC-T, HC-P and Fushun Petrochemical Research Institute develop 3936,3996, FF-16, FF-26, FF-36, FF-46 etc.
The present invention is explained further below in conjunction with drawings and Examples.
Stock oil 1 enters first paragraph hydrofining reactor 3 after mixing with recycle hydrogen 2, after removing partial impurities, reaction effluent enters separator 5 along pipeline 4 and is separated, isolated gas 6 goes out device, first paragraph reaction zone generates oil 7 and mixes with second segment hydrogen 8, enter second segment hydrofining reactor 9 and remove the impurity such as S, N, O further, second segment reaction zone effluent enters separation system 11 along pipeline 10 and is separated, and is separated into gas 12, petroleum naphtha 13, diesel oil 14 and tail oil 15.
Below by embodiment, the present invention program and effect are described.Used catalyst is the commercial catalyst of Fushun Petrochemical Research Institute's development and production.
Embodiment 1 and 2 is one section and processes the embodiment of high-nitrogen stock with two sections of wax oil hydrogenation treatment process, so that the advance of two-stage hydrogenation treatment process processing high-nitrogen stock to be described.Condition and the results are shown in following table 1.
High-nitrogen stock simultaneous test processed by table 1.
| Embodiment | Embodiment 1 | Embodiment 2 | Reference example 1 |
| Stock oil character | |||
| Density/kgm -3 | 950.1 | 950.1 | 950.1 |
| Boiling range/DEG C | 236~544 | 236~544 | 236~544 |
| Sulphur content/quality % | 2.03 | 2.03 | 2.03 |
| Nitrogen content/μ gg -1 | 6127 | 6127 | 6127 |
| Processing condition | |||
| First paragraph catalyzer | FF-36 | FF-36 | FF-36 |
| Second segment catalyzer | FF-36 | FF-36 | / |
| First paragraph denitrification percent, % | 45 | 55 | / |
| Pressure/MPa | 15.7 | 13.7 | 15.7 |
| Temperature/DEG C (often kind of catalyzer) | 375/385 | 385/393 | 400 |
| Volume space velocity/h -1(often kind of catalyzer) | 1.0/1.0 | 1.0/1.0 | 0.5 |
| Hydrogen to oil volume ratio (often kind of catalyzer) | 900/900 | 900/900 | 900 |
| Tail oil: S content/μ gg -1 | 50 | 47 | 52 |
| N content/μ gg -1 | 302 | 298 | 328 |
Table 1 data show, when obtaining order product property and being close, the inventive method can reduce temperature of reaction greatly, if embodiment 1 is compared with comparative example 1; Or can greatly reduce reaction pressure and temperature of reaction, if embodiment 2 is compared with comparative example 1.
Embodiment 3,4 and 5 is processing deep drawing wax oil embodiment, to further illustrate the advance of two-stage hydrogenation treatment process of the present invention.Actual conditions and the results are shown in following table 2.
Deep drawing wax oil simultaneous test processed by table 2.
| Embodiment | Embodiment 3 | Embodiment 4 | Embodiment 5 | Reference example 2 |
| Stock oil character | ||||
| Density/kgm -3 | 0.9392 | 0.9392 | 0.9392 | 0.9392 |
| Boiling range/DEG C | 241~602 | 241~602 | 241~602 | 241~602 |
| Sulphur content/quality % | 2.97 | 2.97 | 2.97 | 2.97 |
| Nitrogen content/μ gg -1 | 3153 | 3153 | 3153 | 3153 |
| Processing condition | ||||
| First paragraph catalyzer | FF-46 | FF-46 | FF-46 | FF-46 |
| Second segment catalyzer | FF-46 | FF-46 | FF-46 | / |
| First paragraph denitrification percent, % | 45 | 45 | 50 | / |
| Pressure/MPa | 15.7 | 13.7 | 12.0 | 15.7 |
| Temperature/DEG C (often kind of catalyzer) | 373/385 | 377/391 | 385/398 | 392 |
| Volume space velocity/h -1(often kind of catalyzer) | 1.2/1.2 | 1.2/1.2 | 1.2/1.2 | 0.6 |
| Hydrogen to oil volume ratio (often kind of catalyzer) | 900/900 | 900/900 | 900/900 | 900 |
| Tail oil: S content/μ gg -1 | 51 | 53 | 66 | 46 |
| N content/μ gg -1 | 308 | 294 | 374 | 288 |
Above embodiment shows, adopt two-stage hydrogenation treatment process, Hydrobon catalyst is divided into two sections of fillings, when processing high nitrogen or height does raw material, effectively can play the activity of Hydrobon catalyst, and can provide high-quality charging for downstream catalytic cracking unit.
Because hydrofining reaction temperature reduces greatly, thus the running period of device can be improved, or improve the working ability of device under same running period, or reduce working pressure when keeping same denitrification percent.
Claims (10)
1. a high-nitrogen stock hydroprocessing process, with high nitrogen heavy distillate for raw material, adopt two-stage process flow process, under Hydrofinishing conditions, heavy distillate raw material and hydrogen are mixed into first paragraph reaction zone, first paragraph reaction zone uses Hydrobon catalyst, the denitrification percent of first paragraph reaction zone controls to be 20% ~ 70%, gas phase after the effluent gas-liquid separation of first paragraph reaction zone continues to use after removing impurities matter, liquid phase after the effluent gas-liquid separation of first paragraph reaction zone enters second segment reaction zone and carries out hydrotreatment reaction, second segment reaction zone uses Hydrobon catalyst, second segment reaction zone reaction effluent enters separation system, obtain hydrotreatment reaction product,
First paragraph reaction zone and second segment reaction zone use a set of recycle hydrogen system, the gas phase of first paragraph reaction zone reaction effluent gas-liquid separation carries out depriving hydrogen sulphide and deamination, then for second segment reaction zone, the gas phase of second segment reaction zone reaction effluent gas-liquid separation is cycled to used in first paragraph reaction zone, and the new hydrogen that reaction process is supplemented enters second segment reaction zone.
2. method according to claim 1, is characterized in that: the nitrogen content of high nitrogen heavy distillate raw material is 2500 more than μ g/g.
3. method according to claim 2, is characterized in that: the nitrogen content of high nitrogen heavy distillate raw material is 3500 more than μ g/g.
4. method according to claim 1, is characterized in that: the nitrogen content of high nitrogen heavy distillate raw material is 3000 ~ 15000 μ g/g.
5. method according to claim 1 and 2, is characterized in that: the initial boiling point of high nitrogen heavy distillate raw material is 220 ~ 450 DEG C, and final boiling point is 500 ~ 700 DEG C.
6. method according to claim 5, is characterized in that: the initial boiling point of high nitrogen heavy distillate raw material is 300 ~ 420 DEG C, and final boiling point is 550 ~ 650 DEG C.
7. method according to claim 1, is characterized in that: the denitrification percent of first paragraph reaction zone controls to be 30% ~ 60%.
8. the method according to claim 1 or 7, is characterized in that: the temperature of reaction of first paragraph reaction zone is 300 ~ 480 DEG C, and reaction pressure is 5.0 ~ 20.0 MPa, and hydrogen to oil volume ratio is 100:1 ~ 4000:1, and during liquid, volume space velocity is 0.2 ~ 4.0 h
-1; In second segment reaction zone, temperature of reaction is 250 ~ 500 DEG C, and reaction pressure is 5.0 ~ 20.0 MPa, and hydrogen to oil volume ratio is 100:1 ~ 4000:1, and during liquid, volume space velocity is 1.0 ~ 10.0 h
-1.
9. the method according to claim 1 or 7, it is characterized in that: the operation condition of first paragraph reaction zone is: temperature of reaction is 330 ~ 450 DEG C, reaction pressure is 8.0 ~ 17.0 MPa, and hydrogen to oil volume ratio is 400:1 ~ 2000:1, and during liquid, volume space velocity is 0.5 ~ 3.0 h
-1; The operation condition of second segment reaction zone is: temperature of reaction is 300 ~ 440 DEG C, and reaction pressure is 8.0 ~ 17.0 MPa, and hydrogen to oil volume ratio is 400:1 ~ 2000:1, and during liquid, volume space velocity is 1.0 ~ 4.0 h
-1.
10. method according to claim 1, it is characterized in that: Hydrobon catalyst with one or more in W, Mo, Ni and Co for active ingredient, with the active ingredient of oxide basis weight content in the catalyst for 20% ~ 90%, Hydrobon catalyst is under response behaviour, and hydrogenation active component is sulphided state.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1940030A (en) * | 2005-09-28 | 2007-04-04 | 中国石油化工股份有限公司 | Hydrogenation cracking method of high-output diesel oil from high-nitrogen content heavy raw material |
| CN101831317A (en) * | 2010-05-08 | 2010-09-15 | 何巨堂 | Hydrogenation method of hydrocarbon with high contents of aryl and nitrogen |
| CN102041073A (en) * | 2009-10-16 | 2011-05-04 | 中国石油化工股份有限公司 | Hydrocracking method for anthracene oil |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1940030A (en) * | 2005-09-28 | 2007-04-04 | 中国石油化工股份有限公司 | Hydrogenation cracking method of high-output diesel oil from high-nitrogen content heavy raw material |
| CN102041073A (en) * | 2009-10-16 | 2011-05-04 | 中国石油化工股份有限公司 | Hydrocracking method for anthracene oil |
| CN101831317A (en) * | 2010-05-08 | 2010-09-15 | 何巨堂 | Hydrogenation method of hydrocarbon with high contents of aryl and nitrogen |
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