CN103773475B - A kind of gas phase, Solution-Phase Combinatorial hydrogenation method - Google Patents
A kind of gas phase, Solution-Phase Combinatorial hydrogenation method Download PDFInfo
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- CN103773475B CN103773475B CN201210408376.7A CN201210408376A CN103773475B CN 103773475 B CN103773475 B CN 103773475B CN 201210408376 A CN201210408376 A CN 201210408376A CN 103773475 B CN103773475 B CN 103773475B
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Abstract
The invention discloses the circulation of a kind of gas phase, liquid phase circulation combined hydrogenation processing method.The method comprises, and poor ignition quality fuel carries out gas phase hydrogenation reaction, and reaction effluent enters hot high score and is separated, and product liquid and straight-run diesel oil enter liquid phase circulation hydrogenator and react, obtain low sulfur diesel product after being mixed into the saturated molten hydrogen of mixed hydrogen tank.Poor ignition quality fuel is after gas phase hydrogenation reaction, and the aromatic hydrocarbons contained is saturated, and the hydrogen-consuming volume of reaction is very low further, and saturated molten hydrogen amount improves; Also dissolve a large amount of unreacting hydrogen in its liquid phase stream effluent simultaneously, in liquid phase hydrogenation reactor, deep desulfuration reaction provides abundant dissolved hydrogen, and optimized two anti-feed properties, thus be conducive to the carrying out of deep hydrodesulfurizationof reaction.Present approach provides a kind of novel process being raw material production ultra-low-sulphur diesel with poor ignition quality fuel and straight-run diesel oil.
Description
Technical field
The present invention relates to a kind of hydrocarbon hydroprocessing technique, specifically a kind of gas phase circulation hydrogenation and liquid phase circulation hydrogenation combined process.
Background technology
Along with the raising of people's environmental consciousness and the increasingly stringent of environmental regulation, produce and use fuel for cleaning vehicle more and more to become a kind of development trend.And cleaning for diesel oil, desulfurization and Porous deproteinized bone are the keys that it cleans.
At present, in diesel deep desulfurization technology, hydrotreating techniques remains main, be also the most effective technique means.Hydrotreating techniques is also varied, has successively occurred the Technologies such as single hop hydrogenation, single hop serial hydrogenation and two-stage hydrogenation.In addition, along with the control of refinery to cost is more and more stricter, to invest the attention that the low liquid phase circulation hydrogen addition technology for distinguishing feature is more and more subject to refinery, so-called liquid phase circulation hydrogen addition technology is compared to conventional gas-phase circulation hydrogenation technique, liquid phase circulation hydrogenation technique reactive moieties does not arrange hydrogen gas circulating system, liquid-phase product a large amount of circulation time is relied on to carry dissolved hydrogen into reactive system to the hydrogen providing fresh feed to carry out required for hydrogenation reaction, owing to eliminating circulating hydrogen compressor, reduce plant investment and process cost.But while investment reduction, because liquid phase circulation hydrogen addition technology relies on the hydrogen be dissolved in reaction feed to provide reaction, therefore, the hydrogen amount that needs that can the hydrogen dissolved in charging meet chemical reaction affects huge on the result of use of liquid phase circulation hydrogenation technique.At present, usual employing liquid phase circulation hydrogenator effluent component loops back-mixing hydrogen tank and fresh feed are dissolved hydrogen to provide and are reacted required hydrogen in mixed hydrogen tank, due to containing foreign matter contents such as higher sulphur, nitrogen and aromatic hydrocarbons in the unconventional energy resource such as the diesel oil distillate of the secondary processing diesel oil such as catalytic diesel oil, coker gas oil and shale oil, coal tar, reaction hydrogen-consuming volume is very high, therefore, the hydrogen dissolved in oil product is difficult to meet reaction needed, in traditional liquid phase circulation hydrogenation process, be difficult to process the poor ignition quality fuel that high hydrogen consumes.
US Patent No. 6123835 discloses a kind of liquid phase circulation hydrogenation method, and in the method, stock oil is dissolved with the hydrogen of high density in mixed hydrogen tank by mixing/flash distillation hydrogen, and then carries out liquid-phase hydrogenatin process.Effluent after liquid-phase hydrogenatin is divided into two portions, before part direct circulation back-mixing hydrogen tank, another part is then introduced into high-pressure separator and isolates unnecessary waste gas, and gained liquid continues to enter flashing tower and isolates waste gas, and the liquid after flash distillation obtains liquid product through air lift again.But for the poor ignition quality fuel hydrogenation that high hydrogen consumes, liquid-phase hydrogenatin Technology due to the molten hydrogen amount of reaction oil limited, be difficult on the one hand meet the hydrogen needed for catalytic diesel oil reaction, reaction effect is poor; The sulphur content that raw material is higher on the other hand causes the hydrogen sulfide of accumulation high density in liquid phase circulation hydrogenation component loops oil, and inhibit the carrying out that deep desulfuration reacts, reaction effect is poor.
Summary of the invention
For the deficiency of existing liquid phase circulation hydrogenation technique by the molten hydrogen amount restriction of reaction feed, the invention provides a kind of liquid phase circulation hydrogenation, gas phase circulation hydrogenation combination technique technology.The investment of this process unit is little, and energy consumption reduces, and may be used for producing ultra-low-sulphur diesel.
A kind of gas phase hydrogenation of the present invention, liquid-phase hydrogenatin combined hydrogenation technique comprise following content:
(1), after poor ignition quality fuel raw material mixes with hydrogen, enter an anti-gas phase circulation hydrogenator and carry out hydrofining reaction; At least two beds are comprised in described gas phase circulation hydrogenator;
(2) reaction effluent that step (1) obtains enters high pressure hot separator and carries out gas, liquid separation, and separation is given vent to anger, liquid two-phase; Gained gas phase portion can use through compressor compresses Posterior circle after hydrogen is isolated in process further;
(3) the hot high score liquid phase part of step (2) gained mixes with straight-run diesel oil, and enter after mixed hydrogen tank carries out mixed hydrogen, the mixing oil after saturated molten hydrogen enters in liquid phase hydrogenation reactor and carries out hydrofining reaction;
(4) step (3) obtain liquid-phase hydrogenatin reaction effluent a part through reducing valve decompression after bleeder, obtain ultra-low-sulphur diesel product, another part loops back the lower catalyst bed layer of gas phase circulation hydrogenator.
In combined hydrogenation processing method of the present invention, the poor ignition quality fuel raw material described in step (1) generally includes one or more in catalytic cracking diesel oil, coker gas oil and coal tar diesel oil distillate or shale diesel oil.Straight-run diesel oil described in step (3) is conventional straight-run diesel oil raw material in the art, and it is done and is generally no more than 385 DEG C, is generally 330 DEG C ~ 370 DEG C.
Gas phase circulation hydrogenator described in step (1) comprises at least two beds, is generally 2 ~ 4 beds, preferably two beds.Described " lower catalyst bed layer " refers to along any one in other beds except first bed of logistics direction or several beds.
In step (3), the ratio (mass ratio) of the hot high score liquid phase part of step (2) gained and straight-run diesel oil is 1:5 ~ 3:1, preferred 1:5 ~ 2:1.
One anti-gas phase circulation hydrogenator generally reacts under the temperature of reaction relaxed, low-speed and higher pressure, and two anti-liquid phase circulation hydrogenators are then at high temperature, high-speed and low pressing operation.High temperature described herein, low temperature, high-speed, low-speed and high pressure and low pressure are relative.
According to gas phase hydrogenation of the present invention, liquid-phase hydrogenatin combined hydrogenation processing method, the catalyzer loaded in gas phase hydrogenation reaction device and liquid phase hydrogenation reactor can be identical catalyzer, but preferably load the stronger catalyzer of hydrogenation capability in an anti-gas phase circulation hydrogenator, preferred W-Ni or Mo-Ni of one anti-Hydrobon catalyst is active metal, and this catalyzer has stronger hydrotreated lube base oil ability.Two anticatalyzers preferred Mo-Co type catalyzer, two anti-interior chemical reactions are based on hydrodesulfurization reaction, and chemical hydrogen consumption amount is lower.Wherein said Mo-Co type catalyzer with Mo, Co metal for active ingredient, with aluminum oxide or silicon-containing alumina for carrier; Described Mo-Ni or W-Ni type catalyzer with Mo, Ni or W, Ni for active metal component, with aluminum oxide or silicon-containing alumina for carrier.Consisting of of described Mo-Co type catalyzer, Mo-Ni or W-Ni type catalyzer: with the weight of catalyzer for benchmark, tungsten or molybdenum take oxide basis as 8wt% ~ 28wt%, and cobalt or nickel take oxide basis as 2wt% ~ 15wt%; The specific surface area of catalyzer is generally 100 ~ 650m
2/ g, pore volume is generally 0.15 ~ 0.8 mL/g.
Gas phase hydrogenation of the present invention, liquid-phase hydrogenatin combined hydrogenation processing method, the operational condition of the gas phase circulation hydrogenator in step (1) is as follows: average reaction temperature 280 DEG C ~ 380 DEG C, preferably 300 DEG C ~ 340 DEG C; Reaction pressure 4.0 MPa ~ 15.0 MPa, preferably 6.0 MPa ~ 10.0MPa; Volume space velocity 0.2 h during liquid
-1~ 3 h
-1, preferred 0.5h
-1~ 1.5h
-1, hydrogen to oil volume ratio 100 ~ 1000, preferably 300 ~ 700.
The operational condition of the liquid phase circulation hydrogenator in step (3) is as follows: average reaction temperature 320 DEG C ~ 400 DEG C, preferably 340 DEG C ~ 380 DEG C; Reaction pressure 3.0 MPa ~ 10.0 MPa, preferably 4.0 MPa ~ 8.0MPa; Volume space velocity 2.0h during liquid
-1~ 8.0h
-1, preferred 3.0h
-1~ 6.0h
-1; Liquid-phase hydrogenatin recycle ratio (i.e. liquid-phase hydrogenatin treated oil turning oil/straight-run diesel oil mass ratio) is 1:5 ~ 5:1, preferential 1:2 ~ 3:1.
In present invention process thousand process, step (1) and the middle Hydrobon catalyst used of step (3) can use commercially available prod as required, also can prepare by this area Conventional wisdom, wherein step (1) gas phase hydrogenation reaction device inner catalyst is W-Ni type or Mo-Ni type catalyzer, catalyst hydrogenation saturability is stronger, wherein step (3) liquid phase hydrogenation reactor inner catalyst is Mo-Co type catalyzer, and it is active that catalyzer has higher direct desulfurization under high-speed.
Compared with prior art, gas phase hydrogenation of the present invention, liquid-phase hydrogenatin combined hydrogenation processing method have following characteristics:
The present invention fully takes into account the features of gas phase circulation hydrogenation technique and liquid phase circulation hydrogenation technique, reasonably two kinds of techniques are combined effectively: first poor ignition quality fuel raw material enters gas phase circulation hydrogenator and carry out hydrofining reaction, and dose the stronger W-Ni type of hydrogen saturability or Mo-Ni type hydrogenation catalyst this reactor is in-built, and coordinate high pressure, low-speed, the operational condition of suitable temperature of reaction is to reach advanced nitrogen, de-virtue, the object of deoxidation, simultaneously, part eliminates space steric effect containing sterically hindered sulfide after aromatic saturation, be conducive to its anti-two in carry out deep desulfuration further.Reaction effluent is mixed into straight-run diesel oil to enter in liquid phase hydrogenation reactor after mixed hydrogen tank mixes and carries out deep desulfuration reaction after hot high score is separated.Due to after an anti-gas phase circulation hydrogenator reaction, the aromatic hydrocarbons in poor ignition quality fuel is by fully saturated, and therefore, its hydrogen-consuming volume reacted further is very low, and saturated molten hydrogen amount also increases.Simultaneously, having dissolved a large amount of unreacting hydrogens in gas phase hydrogenation reaction device reaction response effluent can be deep desulfuration reaction hydrogen supply in liquid phase hydrogenation reactor on the one hand, after instead refining through one on the other hand, diesel stream effluent has very low foreign matter content, optimize two anti-reaction feed character, be beneficial to the carrying out of two anti-deep desulfuration reactions.Two anti-chargings are treated oil after an anti-hydrogenation and straight-run diesel oil mixing oil, reaction feed hydrogen-consuming volume is low, with liquid phase circulation hydrogenation reaction utilize material dissolution hydrogen carry out reacting hydrogen meltage limited response hydrogen consume should not be excessive feature adapt, be conducive to the effective use of liquid phase hydrogenation reactor.And two anti-liquid phase hydrogenation reactor turning oils loop back anti-second bed, reduce an anti-liquid phase circulation hydrogenator temperature rise, an anti-hydrogenation reaction is carried out under close to the state of isothermal, is conducive to effective use of an anticatalyzer.Filling Mo-Co type height hydrodesulfurization activity catalyzer in liquid phase circulation hydrogenator, carries out deep desulfuration reaction, thus finally obtains ultra-low-sulphur diesel under the reaction conditions of high-speed and high temperature.
Accompanying drawing explanation
Fig. 1 is the principle process schematic diagram of diesel hydrogenation process of the present invention.
Embodiment
Below in conjunction with Fig. 1, diesel hydrogenation method of the present invention is described in detail.
As shown in Figure 1, poor ignition quality fuel stock oil is by pipeline 1, and enter hydrogenator 3 after mixing with the recycle hydrogen introduced through pipeline 2 and carry out hydrofining reaction, described hydrogenator 3 comprises at least two Hydrobon catalyst beds, reaction effluent enters hot high score 4 and carries out gas, liquid is separated, obtain gas phase and liquid phase, gas phase loops back hydrogenator entrance through circulating hydrogen compressor after pipeline 13 goes downstream separation system to isolate hydrogen further, liquid phase part is mixed into mixed hydrogen tank 7 through pipeline 5 and the straight-run diesel oil introduced through pipeline 6, in mixed hydrogen tank 7, mixing oil mixes molten hydrogen with the hydrogen introduced through pipeline 8, the exess of H2 gas is discharged through pipeline 9, saturated molten hydrogen mixing oil enters liquid phase hydrogenation reactor 10 and carries out hydrodesulfurization reaction, a liquid phase hydrogenation reactor effluent part enters the lower catalyst bed layer of hydrogenator 3 through pipeline 11 circulation, another part obtains low-sulfur clean diesel product through pipeline 12 bleeder.
Below by specific embodiment, technical scheme of the present invention and effect are described.
Embodiment 1 ~ 4
Embodiment 1 ~ 4 adopts the flow process shown in Fig. 1 of the present invention.Use the composition of catalyzer and character in table 1 in following examples.One anti-gas phase hydrogenation device is raw materials used for table 2 Raw is according to urging bavin: burnt bavin=50:50 ratio mixing raw material oil, two anti-liquid-phase hydrogenatin device straight-run diesel oil feed properties are as shown in table 3, wherein the ratio of straight-run diesel oil and an anti-high score effluent oil is 1:1, and embodiment 1 ~ 4 processing condition used list in table 4.The evaluation result of embodiment 1 ~ 4 is in table 5.
The composition of table 1 embodiment used catalyst and main character.
| Project | One anti-finishing agent | Two anti-finishing agents |
| Chemical constitution, wt% | ||
| MoO 3 | 20.3 | 18.2 |
| NiO | 6.2 | — |
| CoO | — | 6.5 |
| Carrier | Silicon-containing alumina | Silicon-containing alumina |
Table 2 stock oil character.
| Project | Catalytic diesel oil | Coker gas oil | Mixing raw material oil |
| Density (20 DEG C), g/cm 3 | 0.9308 | 0.8502 | 0.8905 |
| Boiling range, DEG C | 190～360 | 185～370 | 185～370 |
| Sulphur content, μ g/g | 12000 | 9000 | 10500 |
| Nitrogen content, μ g/g | 700 | 1000 | 850 |
| Aromaticity content, wt% | 70 | 30 | 50 |
The anti-straight-run diesel oil charging of table 3 two.
| Project | Straight-run diesel oil |
| Density (20 DEG C), g/cm 3 | 0.8308 |
| Boiling range, DEG C | 170~340 |
| Sulphur content, μ g/g | 3000 |
| Nitrogen content, μ g/g | 50 |
Table 4 embodiment operational condition.
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| One is anti- | ||||
| Temperature of reaction, DEG C | 300 | 320 | 320 | 300 |
| Reaction pressure, MPa | 6.0 | 6.0 | 8.0 | 8.0 |
| Volume space velocity, h -1 | 0.5 | 1.0 | 0.8 | 1.2 |
| Hydrogen to oil volume ratio | 500 | 500 | 500 | 500 |
| Two is anti- | ||||
| Temperature of reaction, DEG C | 360 | 360 | 370 | 370 |
| Reaction pressure, MPa | 6.0 | 6.0 | 4.0 | 4.0 |
| Volume space velocity, h -1 | 4.0 | 4.0 | 6.0 | 6.0 |
| Liquid-phase hydrogenatin recycle ratio | 1：2 | 1：2 | 1：1 | 1：1 |
Table 5 embodiment 1 ~ 4 evaluation result
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Sulphur content, μ g/g | 8 | 10 | 3 | 5 |
| Nitrogen content, μ g/g | <1 | <1 | <1 | <1 |
Claims (10)
1. gas phase, a Solution-Phase Combinatorial hydrogenation method, comprises following content:
(1), after poor ignition quality fuel raw material mixes with hydrogen, enter an anti-gas phase circulation hydrogenator and carry out hydrofining reaction; At least two beds are comprised in described gas phase circulation hydrogenator;
(2) reaction effluent that step (1) obtains enters high pressure hot separator and carries out gas, liquid separation, and separation is given vent to anger, liquid two-phase;
(3) the hot high score liquid phase of step (2) gained mixes with straight-run diesel oil, and enter after mixed hydrogen tank carries out mixed hydrogen, the mixing oil after saturated molten hydrogen enters in liquid phase hydrogenation reactor and carries out hydrofining reaction;
(4) step (3) obtain liquid-phase hydrogenatin reaction effluent a part through reducing valve decompression after bleeder, obtain ultra-low-sulphur diesel, another part loops back the lower catalyst bed layer of described gas phase circulation hydrogenator.
2. according to processing method according to claim 1, it is characterized in that, the poor ignition quality fuel raw material described in step (1) comprises one or more in catalytic cracking diesel oil, coker gas oil, coal tar diesel oil distillate or shale diesel oil.
3. according to processing method according to claim 1, it is characterized in that, doing of the straight-run diesel oil described in step (3) is no more than 385 DEG C.
4. according to processing method according to claim 3, it is characterized in that, doing of the straight-run diesel oil described in step (3) is 330 DEG C ~ 370 DEG C.
5. according to processing method according to claim 1, it is characterized in that, in step (3), the mass ratio of the hot high score liquid phase of step (2) gained and straight-run diesel oil is 1:5 ~ 3:1.
6. according to processing method according to claim 1, it is characterized in that, the operational condition of the gas phase circulation hydrogenator in step (1) is: average reaction temperature 280 DEG C ~ 380 DEG C, reaction pressure 4.0 MPa ~ 15.0 MPa, volume space velocity 0.2h during liquid
-1~ 3h
-1, hydrogen to oil volume ratio 100 ~ 1000.
7. according to processing method according to claim 1, it is characterized in that, in step (3), the operational condition of liquid phase circulation hydrogenator is: average reaction temperature 320 DEG C ~ 400 DEG C, reaction pressure 3.0 MPa ~ 10.0 MPa, volume space velocity 2.0h during liquid
-1~ 8.0h
-1.
8. according to processing method according to claim 1, it is characterized in that, the liquid-phase hydrogenatin reaction effluent of circulation and the mass ratio 1:5 ~ 5:1 of straight-run diesel oil in step (4).
9. according to processing method according to claim 1, it is characterized in that, the catalyst choice W-Ni type in described gas phase circulation hydrogenator or Mo-Ni type catalyzer, the catalyst choice Mo-Co type catalyzer in two anti-liquid phase hydrogenation reactors.
10. according to processing method according to claim 9, it is characterized in that, consisting of of described Mo-Co type catalyzer, Mo-Ni or W-Ni type catalyzer: with the weight of catalyzer for benchmark, tungsten or molybdenum take oxide basis as 8wt% ~ 28wt%, and cobalt or nickel take oxide basis as 2wt% ~ 15wt%.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1033377A (en) * | 1987-12-02 | 1989-06-14 | 戴维·麦基(伦敦)有限公司 | Catalytic hydrogenation method |
| CN101942327A (en) * | 2009-07-09 | 2011-01-12 | 中国石油化工股份有限公司抚顺石油化工研究院 | Hydrotreatment combination technology for producing ultra low sulfur diesel |
| CN102311794A (en) * | 2010-07-07 | 2012-01-11 | 中国石油化工股份有限公司 | Diesel hydrogenation method |
-
2012
- 2012-10-24 CN CN201210408376.7A patent/CN103773475B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1033377A (en) * | 1987-12-02 | 1989-06-14 | 戴维·麦基(伦敦)有限公司 | Catalytic hydrogenation method |
| CN101942327A (en) * | 2009-07-09 | 2011-01-12 | 中国石油化工股份有限公司抚顺石油化工研究院 | Hydrotreatment combination technology for producing ultra low sulfur diesel |
| CN102311794A (en) * | 2010-07-07 | 2012-01-11 | 中国石油化工股份有限公司 | Diesel hydrogenation method |
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