CN100594232C - Inferior fraction oil upgrading process - Google Patents
Inferior fraction oil upgrading process Download PDFInfo
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- CN100594232C CN100594232C CN200610046912A CN200610046912A CN100594232C CN 100594232 C CN100594232 C CN 100594232C CN 200610046912 A CN200610046912 A CN 200610046912A CN 200610046912 A CN200610046912 A CN 200610046912A CN 100594232 C CN100594232 C CN 100594232C
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Abstract
The inferior fraction oil upgrading process consists of a hydroupgrading process and a hydrorefining process. The mixture of inferior diesel oil with low cetane number and hydrogen is first made to pass through the hydroupgrading reaction region for eliminating sulfur, nitrogen and arene components to result in hydroupgraded matter; the hydroupgraded matter is then mixed with high cetane number diesel oil and/or coking gas diesel oil and the mixture is made to pass through the hydrorefining reaction region so as to obtain hydrorefined matters, which is gas-liquid separated into gas component returned to the reaction region and liquid phase product further fractionated in a fractionating tower into the diesel oil product. The process can treat different various fraction oils of different properties simultaneously, and has high diesel oil yield, capacity of raising cetane number and quality of fraction oil, low cost and low power consumption.
Description
Technical field
The present invention relates to a kind of method for modifying of inferior distillate oil, particularly improve the secondary processing distillate, especially the hydro-upgrading combined method of catalytic cracking diesel oil, coker gas oil, coking gasoline and diesel and straight-run diesel oil quality inferior, it can reduce the cetane value of its sulphur, nitrogen and aromaticity content and raising diesel oil distillate significantly, and improves the stability in storage of product.
Background technology
At present the trend that heaviness and poor qualityization accelerate has appearred in the world and domestic crude oil, the oil field scope that relates to also more and more widely, the increasingly stringent of the sustainable development of world economy and environmental regulation in addition, need to produce a large amount of light clean fuels, these all require existing oil Refining Technologies is improved, and produce satisfactory product with minimum cost.Because the poor qualityization of raw material, not only make the degradation of straight-run diesel oil, and the quality that comes from the secondary processing diesel oil cut of heavy oil lighting devices such as catalytic cracking and coking can be poorer, adopt existing technology to be difficult to the qualified diesel product that direct production conforms to quality requirements, this just requires to develop new working method.
The technology of existing secondary processing distillate is mainly finished by hydrogenation process, comprising: hydrofining technology, middle pressure hydrocracking technology and hydro-upgrading technology.
The hydrofining technology mainly contains two kinds: a kind of is with the single hop hydrofining under middle pressure or low pressure of secondary processing diesel oil cut, as FR2764902, RU2058371, US5068025, US5543036, US5817594, US5035793 etc., diesel oil fraction hydrogenating purified technology is all disclosed, this technology can be easy to make the sulphur content in the cut to reach low-down level, but the cetane value increase rate is very little, basically at 3～6 units, and the aromatic hydrocarbons degree of saturation is poor.
Another kind is to use two sections purification techniquess of noble metal catalyst, it can guarantee that sulphur, nitrogen in the diesel oil remove fully with aromatic hydrocarbons and removes in a large number in second section in first section, make sulphur in the product, nitrogen and aromaticity content reach requirement, as US5556824 and US5651878 etc., but the one-time investment of its catalyzer and device is very huge, divide two sections operations again, operation is very complicated, and the stability of catalyzer awaits further to verify, because volume space velocity is smaller, the processing power of device is limited in addition.
Adopt the middle pressure hydrocracking technology, as US5611912, US4985134, US4971680 and US4483760 etc., although the index of diesel oil distillate has all satisfied the requirement of specification, liquid yield is very low, especially the purpose product---it is more that diesel yield reduces, and the gasoline fraction octane value that cracking obtains is low, also needs the reformation technology further to process, and the hydrogen consumption is also very big.
Adopt the diesel oil fraction hydrogenating modification technology, as CN1156752A and CN1289832A etc., although can increase substantially diesel-fuel cetane number and reduce sulphur, foreign matter contents such as nitrogen, but it is low that this technology is only applicable to cetane value, the diesel raw material that aromaticity content is high, catalytic diesel oil (LCO) particularly, and be suitable for ability than the stock oil of higher coker gas oil etc. for coking gasoline and diesel mixing oil or cetane value, mainly be than higher because of the cetane value of coker gas oil own, can be low for the component concentration of hydro-upgrading raising cetane value, although through relatively harsher reaction conditions, the increase rate of the cetane value of hydro-upgrading product is also little, and the nitrogen content in the coker gas oil is than higher, need lower refining air speed and can satisfy the requirement of hydro-upgrading, influence the treatment capacity of device like this and shorten operational cycle of device than higher refining pressure.In addition, above-mentioned technology has been carried out the hydrogenation reaction of the degree of depth to raw materials such as catalytic diesel oils, nitride nearly all in the raw material is all removed, and be present in originally in the oil product some nitride---natural antioxidants also is removed in the lump, cause the storage stability of hydro-upgrading diesel product to descend.
Summary of the invention
At the deficiencies in the prior art, the object of the present invention is to provide the inferior distillate oil hydro-upgrading combination process that a kind of raw material sources are wide, cost is low, stability in storage is good, the diesel product cetane value height of gained, sulphur and nitrogen content are low, are the clean diesel products that meets environmental regulation and specification requirement.
The method for modifying of inferior distillate oil of the present invention comprises the steps:
A, under the operational condition of hydro-upgrading, raw material I obtains the hydro-upgrading distillate after handling through hydro-upgrading by the catalyst for hydro-upgrading bed;
The hydro-upgrading distillate of b, step a gained mixes with raw material II by after the hydrofining bed process hydrofining processing, obtains hydrotreatment mixed fraction oil;
The separating of oil gas circulation that obtains of the hydrotreatment mixed fraction of c, step b gained is used, and separates the liquid fractionation in separation column that obtains, and obtains diesel product.
The described raw material I of step a is low cetane value poor ignition quality fuel, its cetane value is less than 35, aromaticity content is greater than 45wt%, preferred cetane value is less than 30, aromaticity content is greater than 50wt%, the mixing oil of one or more in the diesel oil distillate that generally be selected from catalytic diesel oil, straight(-run) diesel distillate inferior, is obtained by the gelatin liquefaction process and the diesel oil distillate of coal tar.The described raw material II of step b is high hexadecane value diesel oil and/or coking gasoline and diesel, high hexadecane value diesel-fuel cetane number 〉=35 wherein, aromaticity content≤45wt%, preferred cetane value is greater than 40, aromaticity content is less than 35wt%, is generally in coker gas oil and the straight-run diesel oil one or both.Described coking gasoline and diesel is from the coker gasoline of coker and the mixing oil of coker gas oil, and its boiling range is generally 64 ℃～380 ℃.
The feed weight ratio of described raw material I of step a and the described raw material II of step b is 10: 90～90: 10, is preferably 20: 80～80: 20.
Compared with prior art, characteristics of the present invention are: it can increase a reactor on the basis of existing apparatus, perhaps newly-built one is with the device of at least two reactors, utilize the combination process of hydro-upgrading technology and hydrofining technology, can the different multiple distillate feedstock of working properties, make full use of hydro-upgrading and hydrofining technology advantage separately, when keeping diesel yield, produce the lightweight clean diesel product that meets environmental regulation and diesel oil specification requirement.This technology both can increase substantially the cetane value of diesel product as hydrogenation modifying process, reduced sulphur, nitrogen content, can reach the stability in storage that hydrofining technology reduces the sulphur content of diesel product and guarantees diesel oil again.In addition, hydro-upgrading technology and hydrofining technology combine, and the waste of energy when having avoided the raw material of different in kind to divide processing or hybrid process can reduce the facility investment and the process cost of device.
Description of drawings
Fig. 1 is a principle process synoptic diagram of the present invention.
Embodiment
The present invention is according to the difference of feedstock property and product requirement, and the described hydro-upgrading of step a can adopt method by single-stage hydrogenation technique, single hop series process hydrogenation technique and two-phase method hydrogenation technique.The method by single-stage hydrogenation technique is under the hydro-upgrading condition inferior distillate oil directly to be passed through the catalyst for hydro-upgrading bed; Single hop series process hydrogenation technique be under the hydro-upgrading condition with inferior distillate oil at first by the hydrofining bed, again by the catalyst for hydro-upgrading bed; The two-phase method hydrogenation technique be under the hydrofining condition with inferior distillate oil at first by the hydrofining section, product liquid under the hydro-upgrading condition again by the catalyst for hydro-upgrading bed.The described hydrofining of step b is conventional hydrofining technology.
In the inventive method in single hop series process and the two-phase method hydro-upgrading part among used Hydrobon catalyst and the step b used Hydrobon catalyst be the diesel oil hydrofining catalyst of routine, these two kinds of catalyzer can be with a kind of catalyzer, also can be different catalyzer.Generally they are active ingredient with group vib and/or group VIII metal, are carrier with aluminum oxide or siliceous aluminum oxide, and the group vib metal is generally Mo and/or W, and the group VIII metal is generally Co and/or Ni.In the weight of catalyzer, the group vib metal content is counted 10wt%～35wt% with oxide compound, and the group VIII metal content is counted 3wt%～15wt% with oxide compound, and its character is as follows: specific surface is 100～650m
2/ g, pore volume are 0.15～0.6ml/g.Main catalyzer has FH-5, FH-98,3936 that Fushun Petrochemical Research Institute develops, Hydrobon catalysts such as 3996, the function class that also can be external catalyst Co. exploitation is like catalyzer, HC-K, HC-P as Uop Inc., KF-847, the KF-848 etc. of the TK-555 of Topsor company, TK-565 catalyzer and AKZO company.Operational condition can adopt conventional operational condition, is generally stagnation pressure 3.0MPa～18.0MPa, and temperature of reaction is 300 ℃～440 ℃, volume space velocity 0.3h during liquid
-1～6.0h
-1, hydrogen to oil volume ratio is 100: 1～2000: 1.
Hydro-upgrading catalyst system therefor in the inventive method is conventional diesel oil hydrogenation modification catalyzer, is active ingredient with group vib and/or group VIII metal generally, and the group vib metal is generally Mo and/or W, and the group VIII metal is generally Co and/or Ni.The carrier of this catalyzer be in aluminum oxide, siliceous aluminum oxide and the molecular sieve one or more, preferably contain molecular sieve, described molecular sieve can be Y, β or ZSM type molecular sieve.Weight in catalyzer, the group vib metal content is counted 10wt%～35wt% with oxide compound, and the group VIII metal content is counted 3wt%～15wt% with oxide compound, and molecular sieve content is 5wt%-40wt%, alumina content is 10wt%～80wt%, and its specific surface is 100m
2/ g～650m
2/ g, pore volume are 0.15ml/g～0.50ml/g.Main catalyzer have that Fushun Petrochemical Research Institute develops 3963, FC-18 catalyzer etc.For catalyst for hydro-upgrading, require to have certain hydrogenation activity and certain lytic activity, should guarantee that the hydrogenation of alkene and aromatic hydrocarbons is saturated in the diesel oil distillate, also require the aromatic hydrocarbons generation ring-opening reaction after saturated.The operational condition of hydro-upgrading can adopt conventional operational condition, and be generally: stagnation pressure 3.0MPa～18.0MPa, temperature of reaction is 300 ℃～440 ℃, volume space velocity 0.3h during liquid
-1～4.0h
-1, hydrogen to oil volume ratio is 100: 1～2000: 1.
Figure 1 shows that a principle flow chart of the present invention, at first raw material 1 is mixed into hydro-upgrading reactor 3 with hydrogen 2, obtains the low hydro-upgrading of impurity such as sulfur-bearing, nitrogen and generates oil 4.Hydro-upgrading generate oil 4 and raw material 5, and hydrogen 6 be mixed into hydrofining reactor 7, through series reaction, obtain hydrofining and generate oil 8, hydrofining generates oil 8 and enters high-pressure separator 9, being separated into high pressure hydrogen-rich gas 10 mixes after compressor 12 loops back hydro-upgrading reactor 3 and hydrofining reactor 7 with new hydrogen 11, the liquid product of separating 13 enters separation column 14, and further fractionation obtains gas 15, gasoline 16 and diesel oil 17.Below in conjunction with specific embodiment 1～7 explanation the solution of the present invention and effect.
The trade mark of the Hydrobon catalyst that embodiment is used is FH-98, is produced by Wenzhou catalyst plant, and the trade mark of used catalyst for hydro-upgrading is 3963 and FC-18, is produced by Fushun petrochemical corporation (complex) catalyst plant.Stock oil-1, stock oil-2 and stock oil-3 are diesel raw material, and stock oil-4 is the coking gasoline and diesel raw material.
Table 1 stock oil character
| The stock oil title | Stock oil-1 | Stock oil-2 | Stock oil-3 | Stock oil-4 |
| Density (20 ℃)/gcm -3 | 0.9173 | 0.8710 | 0.9322 | 0.8302 |
| The boiling range scope, ℃ | 174～381 | 178～365 | 167～363 | 64～356 |
| Sulphur content, wt% | 0.65 | 1.65 | 0.35 | 0.95 |
| Nitrogen content, wt% | 0.08 | 0.06 | 0.13 | 0.07 |
| Cetane value | 29.1 | 56.0 | 24.0 | - |
| Aromaticity content, wt% | 57.2 | 23.1 | 65.4 | 18.9 |
Table 2 embodiment processing condition
| Numbering | |
The | Embodiment | 2 | |
|
| Stock oil | Stock oil-1 | - | Stock oil-1 | Stock oil-3 | Stock oil-3 | |
| Hydro-upgrading segment process condition | - | |||||
| Hydro-upgrading section catalyzer | FH-98 /3963 | - | FH-98 /3963 | FH-98 /3963 | FH-98 /3963 | |
| Catalyst ratio (v/v) | 60/40 | - | 60/40 | 50/50 | 50/50 | |
| Reaction pressure/MPa | 8.0 | - | 6.0 | 8.0 | 13.0 | |
| Temperature of reaction/℃ | 360 | - | 365 | 365 | 365 | |
| LHSV/h -1 | 1.0 | - | 1.2 | 1.0 | 1.2 | |
| Hydrogen to oil volume ratio (v/v) | 700∶1 | - | 700∶1 | 700∶1 | 700∶1 | |
| The hydrofining technology condition | ||||||
| Feed oil | Hydro-upgrading generates oil/stock oil-2 | Stock oil-1/ stock oil-2 | Hydro-upgrading generates oil/stock oil-2 | Hydro-upgrading generates oil/stock oil-2 | Hydro-upgrading generates oil/stock oil-2 | |
| Feed oil ratio (Wt/Wt) | 30/70 | 30/70 | 40/60 | 20/80 | 50/50 | |
| Hydrofining section catalyzer | FH-98 | FH-98 | FH-98 | FH-98 | FH-98 | |
| Reaction pressure/MPa | 8.0 | 8.0 | 8.0 | 8.0 | 10.0 | |
| Temperature of reaction/℃ | 350 | 350 | 340 | 340 | 345 | |
| LHSV/h -1 | 4.0 | 1.3 | 6.0 | 5.5 | 5.0 | |
| Hydrogen to oil volume ratio (v/v) | 500∶1 | 600∶1 | 700∶1 | 700∶1 | 700∶1 | |
| Product yield, wt% | ||||||
| 〉=145 ℃ of diesel oil distillates | 98.8 | 99.9 | 97.8 | 98.3 | 98.9 |
Table 3 embodiment gained diesel product character
| Numbering | |
Reference example 1 | |
|
|
| Density (20 ℃)/gcm -3 | 0.8525 | 0.8633 | 0.8530 | 0.8469 | 0.8455 |
| Sulphur content/μ gg -1 | 34 | 155 | 220 | 167 | 140 |
| Nitrogen content/μ gg -1 | 35 | 175 | 45 | 68 | 40 |
| Cetane value | 51.3 | 45.0 | 50.1 | 51.6 | 52.1 |
Table 4 embodiment processing condition and purpose product yield
| Numbering | |
|
|
| Stock oil | Stock oil-3 | Stock oil-3 | Stock oil-1 |
| Hydro-upgrading segment process condition | |||
| Hydro-upgrading section catalyzer | FC-18 | FH-98/3963 | FC-18 |
| Catalyst ratio (v/v) | - | 55/45 | - |
| Reaction pressure/MPa | 6.5 | 8.0 | 10.0 |
| Temperature of reaction/℃ | 350 | 365 | 360 |
| LHSV/h -1 | 1.0 | 1.2 | 1.0 |
| Hydrogen to oil volume ratio (v/v) | 700∶1 | 700∶1 | 700∶1 |
| Hydrofining segment process condition | |||
| Feed oil | Hydro-upgrading generates oil/stock oil-4 | Hydro-upgrading generates oil/stock oil-4 | Hydro-upgrading generates oil/stock oil-4 |
| Feed oil ratio (Wt/Wt) | 35/65 | 60/40 | 50/50 |
| Hydrofining section catalyzer | FH-98 | FH-98 | FH-98 |
| Reaction pressure/MPa | 6.5 | 8.0 | 10.0 |
| Temperature of reaction/℃ | 345 | 360 | 350 |
| LHSV/h -1 | 5.0 | 5.5 | 6.0 |
| Hydrogen to oil volume ratio (v/v) | 700∶1 | 700∶1 | 700∶1 |
| Product yield, wt% | |||
| 〉=145 ℃ of diesel oil distillates | 91.3 | 90.6 | 91.0 |
Table 6 embodiment diesel product main character
| Numbering | |
|
|
| Density (20 ℃)/gcm -3 | 0.8425 | 0.8488 | 0.8520 |
| Sulphur content/μ gg -1 | 160 | 55 | 149 |
| Nitrogen content/μ gg -1 | 23 | 88 | 120 |
| Aromatic hydrocarbons/wt% | 29.3 | 19.8 | 25.7 |
| Cetane value | 52.3 | 51.1 | 50.5 |
From above embodiment, come as can be seen, the maximum characteristics of this combination process are, rationally utilize the characteristics separately of hydrogenation modifying process and hydrofining technology, when keeping the diesel oil distillate yield, both reduced the content of sulphur, nitrogen, aromatic hydrocarbons significantly, also increased substantially the cetane value of diesel product, kept the nitride of a part as natural antioxidants, thereby prolonged the storage stability of diesel product, owing to be combination process, reduced the facility investment and the process cost of device.
Claims (12)
1, a kind of method for modifying of inferior distillate oil comprises the steps:
A, under the operational condition of hydro-upgrading, raw material I obtains the hydro-upgrading distillate after handling through hydro-upgrading by the catalyst for hydro-upgrading bed;
The hydro-upgrading distillate of b, step a gained mixes with raw material II by after the hydrofining bed process hydrofining processing, obtains hydrotreatment mixed fraction oil;
The separating of oil gas circulation that obtains of the hydrotreatment mixed fraction of c, step b gained is used, and separates the liquid fractionation in separation column that obtains, and obtains diesel product;
The described raw material I of step a is low cetane value poor ignition quality fuel, and its cetane value is less than 35, and aromaticity content is greater than 45wt%; The described raw material II of step b is high hexadecane value diesel oil and/or coking gasoline and diesel, high hexadecane value diesel-fuel cetane number 〉=35 wherein, aromaticity content≤45wt%.
2, in accordance with the method for claim 1, the cetane value that it is characterized in that described low cetane value poor ignition quality fuel is less than 30, and aromaticity content is greater than 50wt%; Described high hexadecane value diesel-fuel cetane number is greater than 40, and aromaticity content is less than 35wt%, and the boiling range of described coking gasoline and diesel is 64～380 ℃.
3,, it is characterized in that described low cetane value poor ignition quality fuel is selected from catalytic diesel oil, straight(-run) diesel distillate inferior, one or more the mixing oil in the diesel oil distillate of the diesel oil distillate that obtains by the gelatin liquefaction process and coal tar according to claim 1 or 2 described methods; Described high hexadecane value diesel oil is selected from coker gas oil and the straight-run diesel oil one or both.
4, in accordance with the method for claim 1, the feed weight ratio that it is characterized in that described raw material I of step a and the described raw material II of step b is 10: 90～90: 10.
5, in accordance with the method for claim 1, the feed weight ratio that it is characterized in that described raw material I of step a and the described raw material II of step b is 20: 80～80: 20.
6, in accordance with the method for claim 1, it is characterized in that the described hydro-upgrading of step a adopts method by single-stage hydrogenation technique, single hop series process hydrogenation technique or two-phase method hydrogenation technique.
7, according to claim 1 or 6 described methods, it is characterized in that used Hydrobon catalyst is an active ingredient with group vib and/or group VIII metal, with aluminum oxide or siliceous aluminum oxide is carrier, and wherein the group vib metal is Mo and/or W, and the group VIII metal is Co and/or Ni.
8, in accordance with the method for claim 7, it is characterized in that, in the weight of catalyzer, the group vib metal content is counted 10wt%～35wt% with oxide compound in the described Hydrobon catalyst, and the group VIII metal content is counted 3wt%～15wt% with oxide compound; The character of catalyzer is as follows: specific surface is 100～650m
2/ g, pore volume are 0.15～0.6ml/g.
9, according to claim 1 or 6 described methods, it is characterized in that described hydrorefined operational condition is stagnation pressure 3.0MPa～18.0MPa, temperature of reaction is 300 ℃～440 ℃, volume space velocity 0.3h during liquid
-1～6.0h
-1, hydrogen to oil volume ratio is 100: 1～2000: 1.
10, in accordance with the method for claim 1, it is characterized in that described catalyst for hydro-upgrading is an active ingredient with group vib and/or group VIII metal, the group vib metal is Mo and/or W, the group VIII metal is Co and/or Ni, the carrier of this catalyzer be in aluminum oxide, siliceous aluminum oxide and the molecular sieve one or more, described molecular sieve is Y, β or ZSM type molecular sieve.
11, in accordance with the method for claim 1, it is characterized in that weight in catalyzer, the group vib metal content is counted 10wt%～35wt% with oxide compound in the described catalyst for hydro-upgrading, the group VIII metal content is counted 3wt%～15wt% with oxide compound, molecular sieve content is 5wt%-40wt%, alumina content is 10wt%～80wt%, and its specific surface is 100m
2/ g～650m
2/ g, pore volume are 0.15ml/g～0.50ml/g.
12, in accordance with the method for claim 1, it is characterized in that the operational condition of described hydro-upgrading is: stagnation pressure 3.0MPa～18.0MPa, temperature of reaction is 300 ℃～440 ℃, volume space velocity 0.3h during liquid
-1～4.0h
-1, hydrogen to oil volume ratio is 100: 1～2000: 1.
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| CN104667995B (en) * | 2013-11-26 | 2017-03-29 | 中国石油化工股份有限公司 | A kind of diesel oil hydrogenation modification catalyst carrier and preparation method thereof |
| CN105733675B (en) * | 2014-12-06 | 2017-05-17 | 中国石油化工股份有限公司 | Combined process for producing light aromatic hydrocarbons |
| 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4971680A (en) * | 1987-11-23 | 1990-11-20 | Amoco Corporation | Hydrocracking process |
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2006
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4971680A (en) * | 1987-11-23 | 1990-11-20 | Amoco Corporation | Hydrocracking process |
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