CN102311791B - Liquid-phase circulating hydrogenation treatment method capable of reinforcing gas-liquid mass transfer - Google Patents
Liquid-phase circulating hydrogenation treatment method capable of reinforcing gas-liquid mass transfer Download PDFInfo
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Abstract
The invention discloses a liquid-phase circulating hydrogenation treatment method capable of reinforcing gas-liquid mass transfer. The process flow adopted by the method comprises: part of hydrogenation circulating oil and a fresh raw material are mixed to form a liquid-phase mixed material to be filled into supergravity gas-liquid hydrogen dissolution equipment together with hydrogen; through the drive of the high-speed rotation of a feeding rotor, gas-liquid countercurrent full contact is formed; the mixed liquid-phase material in which hydrogen is dissolved is discharge out from the bottom of the supergravity gas-liquid hydrogen dissolution equipment and contacted with a catalyst to undergo a hydrogenation reaction, and part of a liquid phase obtained after reaction is circulated. Compared with the prior art, the method has the advantages that: the rotation of the feeding rotor in the gas-liquid hydrogen dissolution equipment forms a supergravity field, so the gas-liquid mass transfer efficiency is increased greatly, and the liquid phase material can fully dissolve hydrogen; meanwhile, gas impurities such as H2S and NH3 in a reaction system can be removed efficiently, so that the hydrodesulfurization, denitrification, aromatic saturation, cracking and other reactions are promoted.
Description
Technical field
The present invention relates to a kind of hydroprocessing process of liquid phase circulation, particularly liquid phase material and dissolve fully that hydrogen is laggard to be entered reactor and carry out the method for hydrogenation reaction.
Background technology
Conventional fixed bed hydrogenation technique is the economical and effective means that remove the impurity such as sulphur, nitrogen in stock oil.In the operation of fixed bed hydrogenation device, often adopt higher hydrogen-oil ratio and hydrogen dividing potential drop,, to guarantee the catalyst runs life-span, promote the carrying out of the reactions such as hydrogenating desulfurization, denitrogenation, aromatic saturation and cracking.Yet the hydrogen gas circulating system that pressure is higher needs high investment cost and running cost, has indirectly increased the oil manufacture cost., if the hydrogen flowing quantity in the hydrotreatment process can be reduced and save hydrogen gas circulating system and circulating hydrogen compressor, can, for enterprise saves facility investment, reduce the production cost of clean fuel.
The perfect condition of fixed-bed reactor mass transfer is: stock oil is evenly distributed on the granules of catalyst surface, and hydrogen passes in the beds space.So hydrogen need to be dissolved in stock oil, could contact with catalyzer, participate in hydrogenation reaction.That is to say when the higher hydrogen pressure of fixed bed hydrogenation process using and hydrogen-oil ratio operational condition, wherein the actual amounts of hydrogen that provides is considerably beyond the required amounts of hydrogen of chemical reaction, this operator scheme is only in order to strengthen the mass transfer power of hydrogen, guarantees the hydrogen solubility in stock oil.The mass transfer apparatus that present alternate transmission aspect is the most general is mainly tower class (comprising reactor) equipment, and as tray column and packing tower etc., the operation of these equipment is all completed under gravity field, and flowing of liquid phase is mainly the effect that is subjected to gravity.Because gravity acceleration g is unalterable finite value, this has also just determined the basic act of liquid-flow from macroscopic view.On the one hand, in the mass transfer apparatus under gravity field, liquid phase fluid flows with thicker stream layer, and alternate transmission area renewal frequency is low and the transmission total area is less, makes alternate transmittance process be restricted; On the other hand, improve gas speed and can change flow state and the energy strengthening transfer process of liquid phase fluid, but be subject to the impact of liquid flooding, make the raising of gas phase velocity also very limited.
US6881326 has introduced a kind of two-phase hydrogenation preconditioning technique.Its technological process is that fresh feed oil, turning oil and hydrogen are dissolved in hydrogen in oil through a mixed hydrogen production device, and the oil that dissolves hydrogen enters less reactor and contacts and carry out hydrogenation reaction with catalyzer, deviates from the impurity in oil.After reaction, a logistics part is circulated to mixed hydrogen production device, and a part is discharged from device as product.This method is dissolved in required hydrogen in oil before adopting raw material and turning oil to enter reactor in advance, can omit the recycle hydrogen system.But this technology does not disclose the concrete mode of molten hydrogen, and after dissolving hydrogen, also is provided with the waste gas tripping device in the separator that arranged before reactor.Although can remove so a small amount of waste gas that affects hydrogenation reaction (being mainly the hydrogen sulfide that removes after reaction and ammonia etc.), but the waste gas separating effect is poor, also make the hydrogen that part has been dissolved separate from stock oil, cause the solubleness of hydrogen in stock oil to descend, finally affect hydrogenation removing impurities matter effect.
Summary of the invention
, for the deficiencies in the prior art, the invention provides a kind of circulation hydroprocessing process of strengthening gas-liquid mass transfer.Before stock oil enters reactor, first with the rear logistics of partial hydrogenation reaction, be mixed into the molten hydrogen storage equipment of hypergravity gas-liquid, under the hypergravity condition, with the hydrogen counter current contact, hydrogen is dissolved in liquid phase material with oversaturated state, efficiently deviates from simultaneously the H in logistics after hydrogenation reaction
2S, NH
3Deng gaseous impurities.The present invention can simplify the operation course, and saves facility investment, and good hydrogenation environment can be provided.
The method of liquid phase circulation hydrotreatment that the present invention strengthens gas-liquid mass transfer comprises following content:
After a, fresh feed oil and partial reaction, turning oil and hydrogen mix counter current contact in the molten hydrogen storage equipment of hypergravity gas-liquid, carry out molten hydrogen and deviate from gaseous impurities.Wherein, the molten hydrogen storage equipment of hypergravity gas-liquid adopts rotary packed bed hyper-gravity gas apparatus for effecting gas/liquid contact, through the H that contains of the molten hydrogen storage equipment of hypergravity gas-liquid
2S, NH
3Hydrogen Deng gaseous impurities is discharged from the molten hydrogen storage equipment of hypergravity gas-liquid top, has fully dissolved the stock oil of hydrogen and the mixture of turning oil and has discharged from the molten hydrogen storage equipment of hypergravity gas-liquid bottom;
The mixture that b, step a discharge enters hydrogenator and contacts with catalyzer and carry out the solid, liquid two-phase hydrogenation reaction;
The reacted thing of c, step b goes out a stream part as the product discharger, and another part is circulated to the molten hydrogen storage equipment of hypergravity gas-liquid.
The molten hydrogen storage equipment of the said hypergravity gas-liquid of step (a) is gas, the operation of liquid two-phase, in the molten hydrogen storage equipment of adults strength liquid, the gas-phase space volume accounts for 20%~90% of the molten hydrogen storage equipment volume of hypergravity gas-liquid, be preferably 50%~80%, can control by controlling the expellant gas amount.Hydrogen is entered by the outside housing of the molten hydrogen storage equipment of hypergravity gas-liquid, flowed out by spindle central sleeve place, stock oil and turning oil enter the molten hydrogen storage equipment of hypergravity gas-liquid by spindle central after mixing, and the high speed rotating drive by the filler rotor, form counter current contact with hydrogen., because the filler rotor forms super gravity field, make the gas-to-liquid contact place produce the universal gravity constant of 50~1000 times, thereby greatly strengthened gas-liquid mass transfer efficiency.The service temperature of the molten hydrogen storage equipment of hypergravity gas-liquid is controlled at 100~380 ℃, is preferably 150~330 ℃; Pressure 0.5~15.0MPa, be preferably 2.5~10.0MPa; Vapour-liquid ratio (volume ratio under fresh feed and entrance hydrogen standard state) is 1: 1~60: 1, is preferably 2.5: 1~15.0: 1.The volume ratio of circulation oil mass and fresh feed (recycle ratio) is 1: 1~10: 1, is preferably 2: 1~6: 1.
The said hydrogenator of step (b) is fixed-bed reactor.Its operational condition is: temperature of reaction is 200~420 ℃, volume space velocity 0.6~5.0h
-1, be preferably 2.0~4.0h
-1, reaction pressure is 0.5~15.0MPa, is preferably 2.5~10.0MPa.
The catalyzer that above-mentioned steps is used is that the fixed bed hydrogenation of this area routine processes catalyzer, wherein the reactive metal of catalyzer can for nickel, cobalt, molybdenum or tungsten etc. one or more.Form and can comprise by weight percentage as catalyzer: nickel or cobalt are 0.5%~10% (by its oxide compound, calculating), and molybdenum or tungsten are 1%~30% (by its oxide compound, calculating), and carrier can be aluminum oxide, silicon oxide, aluminium oxide-silicon oxide, titanium oxide, wait one or more.Catalyzer is extrudate or spherical.The bulk density of catalyzer is 0.5~1.1g/cm
3, granules of catalyst diameter (spherical diameter or bar shaped diameter) is 0.04~1.0mm, specific surface area is 80~400m
2/ g.
The raw material that the present invention processes is the hydrocarbon raw material of boiling range any cut in 130~550 ℃ of scopes.Generally include one or more mixing of spray vapour fuel, diesel oil, catalytic cracking light cycle oil (LCO), wax tailings (CGO), light vacuum gas oil (LVGO), heavy vacuum gas oil (HVGO) etc.
Advantage of the present invention is:
1, under the condition of hypergravity, because the speed of relative movement change of adverse current fluid is large, huge shearing stress can overcome surface tension, make the contact area between hydrogen and liquid phase material increase, thereby cause alternate transmittance process greatly to be strengthened, hydrogen can fully be dissolved in liquid phase material with oversaturated state.
2, in the molten hydrogen storage equipment of hypergravity gas-liquid, when liquid phase material fully dissolves hydrogen, remove H
2S, NH
3Efficiency Deng gaseous impurities improves greatly, with flash distillation or the air lift of routine, compares, and impurity removal percentage obviously improves, thereby promotes the reactions such as hydrogenating desulfurization, denitrogenation, aromatic saturation.
The reactions such as 3, hydrogenating desulfurization, denitrogenation, aromatic saturation are all thermopositive reaction, and larger circulation oil mass can be taken a large amount of reaction heat out of, prevents that the reactor temperature rise is excessive.Carry simultaneously enough hydrogen and enter reactor, guarantee the quantity of the required hydrogen of reaction.
4, do not need the recycle hydrogen system.Just use a small amount of new hydrogen when molten hydrogen, the molten hydrogen storage equipment effluent air of hypergravity gas-liquid is removed H through separating
2S, NH
3Use Deng can continue after gaseous impurities.
5, with respect to the transmission equipments such as tower under gravity field, the molten hydrogen storage equipment of hypergravity gas-liquid has that volume is little, cost is low, the efficiency advantages of higher.Owing to operating under certain pressure, therefore need easily by liquid, to be full of in the molten hydrogen storage equipment of adults strength liquid, cause gas-liquid mass transfer Efficiency Decreasing and operation energy consumption to increase, so have the essential condition that suitable gas-phase space is the assurance steady running in the molten hydrogen storage equipment of adults strength liquid.
Description of drawings
Fig. 1 is processing method schematic flow sheet of the present invention.
In figure: 1-fresh feed oil, the 2-fresh hydrogen, 3-contains H
2S, NH
3Deng the hydrogen of gaseous impurities, the molten hydrogen storage equipment of 4-hypergravity gas-liquid, 5-filler rotor, 6-fully dissolves the liquid phase material of hydrogen, and 7-fixed bed hydrogenation reactor, 8-generate oil, 9-turning oil.
Embodiment
, for further setting forth specific features of the present invention, in connection with accompanying drawing, be illustrated.
By reference to the accompanying drawings 1, a kind of technological process of the present invention is:
Fresh feed oil 1 and from the turning oil 9 of hydrogenator, from the molten hydrogen storage equipment spindle central of hypergravity gas-liquid, entering,, with fresh hydrogen 2 counter current contact, carry out the molten hydrogen of liquid phase material and deviate from simultaneously H under the condition of hypergravity
2S, NH
3Deng gaseous impurities.Wherein the service temperature of the molten hydrogen storage equipment of hypergravity gas-liquid is controlled at 100~380 ℃, is preferably 150~330 ℃; Pressure 0.5~15.0MPa, be preferably 2.5~10.0MPa; Vapour-liquid ratio (volume) is 1: 1~60: 1, is preferably 2.5: 1~15.0: 1.The volume ratio of circulation oil mass and fresh feed (recycle ratio) is 1: 1~10: 1, is preferably 2: 1~6: 1.The liquid phase material 6 that fully dissolves hydrogen enters fixed-bed reactor 7 and carries out catalytic hydrogenation reaction, and wherein the operational condition of fixed-bed reactor is: temperature of reaction is 260~420 ℃, volume space velocity (cumulative volume air speed) 0.6~5.0h
-1, be preferably 2.0~4.0h
-1, reaction pressure is 0.5~15.0MPa, is preferably 2.5~10.0MPa.Reacted part generates oil 8 and discharges as product from device, and part logistics 9 loops back the molten hydrogen storage equipment 4 of hypergravity gas-liquid.
, for further illustrating the solution of the present invention and effect, enumerate following examples and comparative example:
Embodiment 1-2
The present embodiment is a kind of embodiment that hydrocarbon oil hydrogenation is processed, and the operating process schematic diagram is with reference to accompanying drawing 1.
Fresh feed oil 1 and from the turning oil 9 of hydrogenator, from spindle central, enter the molten hydrogen storage equipment of hypergravity gas-liquid,, with fresh hydrogen 2 counter current contact, carry out the molten hydrogen of liquid phase material and deviate from H under the condition of hypergravity
2S, NH
3Deng gaseous impurities.What form after the molten hydrogen storage equipment of hypergravity gas-liquid contains H
2S, NH
3Hydrogen 3 Deng gaseous impurities is discharged from the spindle central sleeve of the molten hydrogen storage equipment of hypergravity gas-liquid, the liquid phase material 6 that fully dissolves hydrogen enters fixed-bed reactor 7 and carries out catalytic hydrogenation reaction, reacted part generates oil 8 and discharges as product from device, and part generates oil 9 and loops back the molten hydrogen storage equipment 4 of hypergravity gas-liquid.
Adopt feedstock property in Table 1-1, catalyzer is selected the FH-UDS Hydrobon catalyst of Fushun Petrochemical Research Institute's development and production.The composition of FH-UDS catalyzer and quality index are in Table 1-2, and processing condition are in Table 1-3, and refined diesel oil character is in Table 1-4.Molten hydrogen gas-liquid volume ratio is 5: 1.In the molten hydrogen storage equipment of adults strength liquid, the gas-phase space volume accounts for 30%~80% of the molten hydrogen storage equipment volume of hypergravity gas-liquid.
Table 1-1 stock oil character
Composition and the quality index of table 1-2 catalyzer
Table 1-3 processing condition
Processing condition | Condition 1 | Condition 2 |
Temperature of reaction, ℃ | 362 | 362 |
Reaction pressure, MPa | 6.0 | 6.0 |
Circulation volume ratio (turning oil: fresh feed) | 3∶1 | 6∶1 |
Volume space velocity, h -1 | 3.2 | 3.2 |
Mixed hydrogen amount/inlet amount (wt%) | 0.72 | 0.72 |
Table 1-4 treated oil character
Comparative example
Compare with embodiment, adopt common fillers tower (gas-liquid counter current contact) as molten hydrogen storage equipment, processing condition are in Table 2-1, and refined diesel oil character is in Table 2-2.
Table 2-1 processing condition
Table 2-2 treated oil character
Above result can be found out, adopt the contact area between hydrogen of the present invention and liquid phase material to increase, cause alternate transmittance process greatly to be strengthened, hydrogen can fully be dissolved in liquid phase material with oversaturated state, simultaneously the effective air lift of the impurity such as hydrogen sulfide and ammonia is discharged, make the hydrogenation reaction performance obviously improve, as desulfurization degree, improve 30 percentage points, obtained beyond thought technique effect.
Claims (4)
1. method of liquid phase circulation hydrotreatment of strengthening gas-liquid mass transfer is characterized in that comprising following content:
After a, fresh feed oil and partial reaction, turning oil and hydrogen mix counter current contact in the molten hydrogen storage equipment of hypergravity gas-liquid, carry out molten hydrogen and deviate from gaseous impurities;
The mixture that b, step a discharge enters hydrogenator and contacts with catalyzer and carry out the solid, liquid two-phase hydrogenation reaction;
The reacted logistics part of c, step b is as the product discharger, and another part is circulated to the molten hydrogen storage equipment of hypergravity gas-liquid;
Wherein: the molten hydrogen storage equipment of hypergravity gas-liquid adopts rotary packed bed hyper-gravity gas apparatus for effecting gas/liquid contact; The molten hydrogen storage equipment of hypergravity gas-liquid is gas, the operation of liquid two-phase, and in the molten hydrogen storage equipment of adults strength liquid, the gas-phase space volume accounts for 20%~90% of the molten hydrogen storage equipment volume of hypergravity gas-liquid, by controlling the expellant gas amount, controls.
2. it is characterized in that in accordance with the method for claim 1: through the H that contains of the molten hydrogen storage equipment of hypergravity gas-liquid
2S, NH
3The hydrogen of gaseous impurities is discharged from the molten hydrogen storage equipment of hypergravity gas-liquid top, has fully dissolved the stock oil of hydrogen and the mixture of turning oil and has discharged from the molten hydrogen storage equipment of hypergravity gas-liquid bottom.
3. in accordance with the method for claim 1, it is characterized in that: the service temperature of the molten hydrogen storage equipment of hypergravity gas-liquid is controlled at 100~380 ℃, pressure is 0.5~15.0MPa, volume ratio under fresh feed and entrance hydrogen standard state is 1: 1~60: 1, and the volume ratio of circulation oil mass and fresh feed is 1: 1~10: 1.
4. in accordance with the method for claim 1, it is characterized in that: the said hydrogenator of step (b) is fixed-bed reactor, and its operational condition is: temperature of reaction is 200~420 ℃, volume space velocity 0.6~5.0h
-1, reaction pressure is 0.5~15.0MPa.
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