CN102041069B - Gas-liquid countercurrent hydrogenation method for desulfurization, denitrification and aromatic hydrocarbon of diesel - Google Patents
Gas-liquid countercurrent hydrogenation method for desulfurization, denitrification and aromatic hydrocarbon of diesel Download PDFInfo
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Abstract
The invention discloses a gas-liquid countercurrent hydrogenation method for desulfurization, denitrification and aromatic hydrocarbon of diesel. Under the condition of dydrotrating diesel fractions, hydrogen and raw material diesel countercurrent pass through catalyst bed layers, wherein a reactor is divided into at least two reaction regions, and each reaction region comprises at least one hydrogenation catalyst bed layer; and the diameters of the reaction regions of the reactor are successively increased from the lower reaction region to the upper reaction region, the boundary diameter change part of at least one reaction region is provided with an effusion region, the bottom or the side of the effusion region is provided with an effusion outlet pipeline to lead the liquid of the effusion region into the lower reaction region of the reactor to be used as cooling material flow. The gas-liquid countercurrent hydrogenation method can maintain the relatively stable gas speed, prevent the flooding of the reaction regions, and enhance the operational flexibility of the reactor. Meanwhile, the gas-liquid countercurrent hydrogenation can effectively control reaction temperature, which is favorable for the arene removing reaction of the diesel fractions.
Description
Technical field
The present invention relates to a kind of hydroprocessing process of gas-liquid counter current operation on solid catalyst, belong to the petrochemical technology field, be specially adapted to the diesel oil hydrogenation treating processes.
Background technology
Due to the day by day deficient of petroleum resources in world wide and to the continuous growth of diesel oil demand, derive from the shared share of the diesel oil of heavy oil cracking increasing, cause in diesel oil distillate containing the heteroatomss such as a large amount of aromatic hydrocarbon and sulphur, nitrogen.The increase of these materials has not only reduced diesel-fuel cetane number, and the discharge formed after burning is day by day serious to the pollution of environment, causes gradually the common concern of countries in the world.
At present hydrogenation remains and removes in diesel oil distillate the heteroatoms such as sulphur, nitrogen and carry out the most economical effective scheme that aromatic hydrogenation is saturated.In the hydrogenation unit operating process of gas and liquid flowing, the H that reaction generates
2S, NH
3On the active centre of catalyst surface, hydrogenation reaction is produced to restraining effect Deng the gaseous impurities competitive adsorption.In addition, H
2S, NH
3Deng gaseous impurities and C
1, C
2Enter in recycle hydrogen Deng the micro-molecular gas hydro carbons, can cause the hydrogen dividing potential drop to reduce, affect the degree of depth of hydrogenation removing impurities matter and aromatic saturation.The operation of hydrogenator gas-liquid counter current can be avoided above-mentioned shortcoming, can remove in time most of H
2S, NH
3Deng gaseous impurities, increase hydrogen partial pressure, promote hydrogenation reaction, therefore more and more be subject to researchist's attention.
In the gas-liquid counter current hydrogenator, liquid stream enters from the top of reactor, from the bottom of reactor, flows out, and recycle hydrogen enters from the bottom of reactor, from top, flows out.Gas-liquid is passed through beds in the mode of adverse current, realizes hydrogenation reaction.The principal element of restriction gas-liquid counter current hydrogenator development at present is that beds easily produces liquid flooding, and the turndown ratio of reactor is little.
Gas-liquid two-phase is in the beds countercurrent flow, and its hydrodynamic characteristic mainly contains liquid holdup (hold-up of liquid), loading point, flooding point and pressure degradation.Although catalyst in reactor structure, physical property and fluid properties are different, flow phenomenon varies, and basic law is identical.When catalyzer and liquid flow rate one timing, along with the upwards increase gradually of gas velocity, reactor can be through constant hold-up stage, carrier fluid stage and the liquid flooding stage of liquid.In the constant hold-up stage, reactor cross section space (gas, liquid circulation area), enough by gas, liquid two-phase, the hold-up of beds liquid and gas speed are irrelevant.Reactor is in carrier fluid during the stage, because gas velocity increases, the gas-liquid two-phase Interaction enhanced, it is smooth and easy dirty that the frictional force between ascending gas and dropping liq starts to hinder liquid, thereby cause liquid holdup significantly to increase, reactor cross section space (gas, liquid circulation area) reduces.When gas velocity further increases, reactor can be in the liquid flooding state, and now liquid is withstood and is difficult to flow downward by gas, and beds liquid is accumulated rapidly and finally caused liquid flooding.When liquid flooding occurs, have obvious liquid on beds and accumulate.Gas upwards passes through liquid layer with the form of bubbling, and resistance increases, and mass-transfer efficiency reduces.And can produce foam on reactor top, bring gas-circulating system into.Therefore the operation of reactor is generally with more than loading point, and spotting out is following is the optimum operation district.Because loading point is difficult to determine usually, on experience, operating gas velocity is selected 50%～80% of spotting out gas speed.In hydrogenation process, owing to making progress, mobile hydrogen can be the gaseous substance (H of reaction generation
2S, NH
3, C
1And C
2Deng the micro-molecular gas hydro carbons) bring gas phase into, so can form the gas flow on reactor top, increase, cause the probability that liquid flooding occurs to increase.
The aromatic saturation of diesel oil is strong exothermal reaction, so the beds temperature rise is higher.In temperature, under higher condition, the hydrogenation of aromatic hydrocarbons can be subject to thermodynamical restriction, can't realize that the degree of depth is saturated.At present, general cold hydrogen or the circulation cold oil heat-obtaining of adopting of the fixed bed operation of gas and liquid flowing.If countercurrent hydrogenation also adopts cold hydrogen heat-obtaining, can cause gas phase velocity to change greatly, unfavorable to the quiet run of reactor.Adopt the air speed of circulation cold oil operation meeting reduction reactor, reduce the treatment capacity of device.
U.S. Pat 5985131 has provided the reactor structure with gas, fluid path.When reactor generation liquid flooding, liquid can flow into next bed by fluid path.When gas velocity is larger, beds pressure reduction is larger, and gas can enter a upper bed by gas passage.Catalyst bed interlayer non-reaction zone is provided with inlet mouth, can play the effect of similar cold hydrogen, although this method can reduce the temperature rise of reactor, its gas is " short circuit " easily, and cooling performance is not good.In addition, owing to being provided with more gas, liquid path, reactor effective volume utilization ratio is not high, and operability is lower.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of new diesel gas-liquid countercurrent hydroprocessing process.At least contain 2 reaction zones in gas, liquid counter-current reactor, each reaction zone diameter increases successively from the bottom to top, to increase catalyst bed layer cross section space (gas, liquid circulation area) in reaction zone.Under the condition increased with height for reactor at the upper reaches gas flow, keep gas velocity relatively stable, reduce the reaction zone liquid flooding and occur, increase the reactor turndown ratio.Simultaneously at least one reducing place, reaction zone boundary, the hydrops district is set, it mainly accumulates liquid that wall stream temperature is lower and the entrained liquids of gas speed when larger.Bottom, hydrops district or sidepiece arrange hydrops and derive pipeline, and the liquid that hydrops district temperature is lower imports the reactor lower part reaction zone, as cooling logistics, can reduce the temperature rise of lower catalyst bed layer reaction zone, promote the aromatic saturation reaction, the extending catalyst life-span.
The gas-liquid countercurrent hydrogenation method of diesel fuel desulfurization of the present invention, denitrogenation and aromatic saturation comprises following content:
Under the diesel oil fraction hydrogenating treatment condition, hydrogen and diesel raw material are passed through beds in the mode of adverse current, and hydrogen is entered by reactor bottom, from reactor head, discharge, liquid phase is entered by reactor head, with hydrogen is reverse, contacts, and from reactor bottom, discharges.
Wherein related reactor at least is divided into 2 reaction zones, and each reaction zone is comprised of at least 1 hydrogenation catalyst bed; Reactor is increased successively by lower reaction zone to top reaction zone diameter.The top reaction zone diameter increases by 2%～30% than adjacent lower reaction zone diameter, and preferably 4%～15%.The height of each reaction zone is 20%～80% of whole reactor virtual height.The virtual height of reactor refers to the height of loading catalyst partial reaction device.At at least one reducing place, reaction zone boundary, the hydrops district is set, it mainly accumulates liquid that wall stream temperature is lower and the entrained liquids of gas speed when larger.Bottom, hydrops district or sidepiece arrange pipeline, and the liquid that temperature is lower imports the reactor lower part reaction zone, to reduce the beds temperature rise.It is inlet amount 2%～15% that the hydrops district imports the amount of reactor lower part reaction zone liquid stream, preferably 4%～10%.If hydrops district liquid is more, hydrops district excess liq can enter liquid distributor by the overflow mode, flows into following reaction zone beds.Can derive the pipeline installing interchanger at hydrops in case of necessity, so that beds reaches optimal reaction temperature.Hydrops is derived on pipeline can also arrange flowrate control valve.
Wherein related reactor top reaction zone loads conventional base metal sulfide catalyst, and FF-98, FH-UDS etc. as Fushun Petrochemical Research Institute's development, be mainly used in removing the heteroatomss such as sulphur, nitrogen.The high catalyzer of the lower reaction zone filling saturated performance of aromatic hydrogenation of reactor, as as-reduced metal catalyzer, noble metal catalyst etc., can be also the base metal sulfide catalyst of not volatile sulphur, form the high activated catalyst bed, be mainly used in the aromatic saturation reaction.
The hydrogenation operation condition is generally: pressure is 2.0～10.0MPa, is preferably 4.0～8.0MPa; Volume space velocity is 0.5～5.0h
-1, be preferably 1.0～3.0h
-1Temperature of reaction is controlled at 280～370 ℃, is preferably 320～360 ℃; Hydrogen to oil volume ratio is 100: 1～950: 1, is preferably 300: 1～800: 1.
Other Parameter Conditions can be according to feedstock property and quality product requirement, simply definite by experiment.
This reactor can be used in single hop list device technique, and the gas and liquid flowing reactor of also can connecting in front, be applied in the single hop tandem process, and the gas and liquid flowing reactor adopts this area routine operation condition.In rear a kind of technique, can strengthen the effect of gas-liquid counter current reactor hydrogenation aromatics-removing.
Technical characterstic of the present invention and advantage comprise:
1, adopt the Design Mode of reactor reducing, can give full play to the technical superiority of counter-current operation, can guarantee again whole device smooth operation.
While 2, adopting counter-current operation to carry out the poor ignition quality fuel hydrogenation, along with liquid stream, along axially the flow downward increase of reaction depth in process of reactor, the hydrogen dividing potential drop increases, and can improve impurity extrusion rate and the aromatic saturation degree of depth.
3, adopt the gas-liquid counter current operator scheme of a plurality of beds, can so that hydrogen in the process axially risen along reactor, hydrogen sulfide and ammonia that reaction is generated are taken reactor out of, thereby can avoid the two impact for lower catalyst bed layer hydrogenation reaction effect, can obtain high-quality product.
4, adopt the design of reactor reducing can increase catalyst bed layer cross section space in reaction zone (gas, liquid circulation area).Under the condition increased with height for reactor at the upper reaches gas flow, keep gas velocity relatively stable, prevent that the reaction zone liquid flooding from occurring, and increases the reactor turndown ratio.
5, the liquid of hydrops district lesser temps enters reactor lower part as the refrigerant conductance, can, under the condition that does not reduce air speed, guarantee lower beds temperature rise.Avoid the introducing of cold hydrogen to increase gas flow, increased the gas reactor load.
6, aromatic hydrogenation is thermopositive reaction, and its reaction equilibrium constant reduces with the rising of temperature of reaction, thus lower temperature of reaction saturated to aromatic hydrogenation be favourable.The cryogenic liquid logistics thermal capacitance in hydrops district is higher, can take more reaction heat out of reactor, reduces the temperature rise of reactor, promotes the aromatic hydrogenation saturated reaction, extending catalyst running life.The liquid stream that can derive the hydrops district in case of necessity carries out importing the reactor lower part reaction zone after heat exchange again, further to reduce temperature.
7, the hydrops district imports the Wei Weiyi position, position of reactor lower part reaction zone liquid stream, generally according to reaction zone reaction bed temperature distribution situation, determines.The inventory of hydrops district liquid importing reactor lower part can be according to the response behaviour adjustment, as when the initial reaction stage, catalyst activity is higher, the beds temperature rise is larger, can suitably increase the inventory of importing reactor lower part to reduce reaction bed temperature, now because catalyst activity is high, so can't through whole beds, not affect the final removing impurities matter degree of depth because of partial material; When reacting the later stage, catalyst activity reduction, the beds temperature rise reduces, and can suitably reduce the inventory that imports reactor lower part from the hydrops district, now due to the whole beds of most of material process, so still can guarantee the degree of depth of final removing impurities matter.
The accompanying drawing explanation
The gas-liquid countercurrent hydrogenation method gas-liquid counter current structure of reactor schematic diagram that Fig. 1 is a kind of diesel fuel desulfurization of the present invention, denitrogenation and aromatic saturation.
Sequence number 1 is reactor top reaction zone, and 2 is the reactor lower part reaction zone, and 3 is stock oil, and 4 discharge hydrogen for reactor, and 5 is fresh hydrogen, and 6 for generating oil, and 7 is the hydrops district, and 8 is hydrops derivation pipeline.
Embodiment
For explanation the solution of the present invention and effect, by following examples, further illustrate feature of the present invention: embodiment 1～4
The present embodiment is mainly investigated hydrogenating desulfurization, denitrogenation and the aromatic saturation effect of gas-liquid counter current hydrogenator of the present invention.
The present embodiment adopts the one-stage serial technical process, and 2 reactors are set, and the 1st reactor is that gas and liquid flowing operates downwards, and the 2nd reactor is the gas-liquid counter current operation.The gas-liquid counter current reactor is comprised of 2 reaction zones, and the aspect ratio of two reaction zones (bottom and top ratio) is 3: 1.Reactor top reaction zone diameter increases by 6% than lower reaction zone diameter.The amount that the hydrops district imports reactor lower part reaction zone liquid stream is 4%～10% of raw material inlet amount.The tapping heat exchange to 260 ℃ of hydrops district, enter in the middle of the counter-current reactor lower reaction zone.
In the present embodiment, co-current reactor and counter-current reactor top reaction zone adopt W-Mo-Ni-Co type Hydrobon catalyst (catalyst A), and this catalyzer has the high characteristics of hydrogenating desulfurization, denitrogenation and arene saturating activity.The counter-current reactor lower reaction zone adopts Pt, Pd noble metal catalyst (catalyst B), and this catalyzer has under the mitigation condition characteristics high to the aromatic hydrogenation saturated activity.The catalyzer physico-chemical property is in Table 1.Stock oil character is in Table 2.Reaction conditions and the results are shown in Table 3.
Table 1 catalyzer physico-chemical property
Table 2 stock oil character
Table 3 hydrofining technology condition and result
| Embodiment | 1 | 2 | 3 | 4 |
| Catalyzer | A/B | A/B | A/B | A/B |
| Tapping amount/% | 4 | 6 | 8 | 10 |
| Co-current reactor (R 1) medial temperature/℃ | 360 | 360 | 360 | 360 |
| Counter-current reactor (R 2) the top reaction zone/℃ | 355 | 355 | 355 | 355 |
| Counter-current reactor (R 2) lower reaction zone/℃ | 354 | 353 | 350 | 348 |
| Reaction hydrogen pressure/MPa | 6.0 | 6.0 | 6.0 | 6.0 |
| Volume space velocity (R 1/R 2)/h -1 | 3.2/2.2 | 3.2/2.2 | 3.2/2.2 | 3.2/2.2 |
| Hydrogen to oil volume ratio | 500∶1 | 500∶1 | 700∶1 | 700∶1 |
| The recycle hydrogen band is fuel-displaced | Nothing | Nothing | Nothing | Nothing |
| Sulphur/μ gg -1 | 12.8 | 11.3 | 11.4 | 10.4 |
| Nitrogen/μ gg -1 | 1.0 | 1.0 | 1.0 | 1.0 |
| Aromatic hydrocarbons/volume % | 17.2 | 15.2 | 14.5 | 13.4 |
As seen from the experiment, the inventive method can stable operation under the higher hydrogen oil ratio, the handiness that has improved vapour-liquid countercurrent hydrogenation technique, and adaptability to raw material is wide, and the device stable operation has improved the industrial applicibility of this Technology.
Claims (7)
1. the gas-liquid countercurrent hydrogenation method of a diesel fuel desulfurization, denitrogenation and aromatic saturation, under the diesel oil fraction hydrogenating treatment condition, hydrogen and diesel raw material are passed through beds in the mode of adverse current, be that hydrogen is entered by reactor bottom, from reactor head, discharge, liquid phase is entered by reactor head, with hydrogen is reverse, contacts, and from reactor bottom, discharges; It is characterized in that: reactor at least is divided into 2 reaction zones, and each reaction zone is comprised of at least 1 hydrogenation catalyst bed; Reactor is increased successively by lower reaction zone to top reaction zone diameter; At at least one reducing place, reaction zone boundary, the hydrops district is set, bottom, hydrops district or sidepiece arrange hydrops and derive pipeline, the liquid in hydrops district are imported to the reactor lower part reaction zone, as cooling logistics; The top reaction zone diameter increases by 2%～30% than adjacent lower reaction zone diameter, and the height of each reaction zone is 20%～80% of whole reactor virtual height; The hydrogenation operation condition is: pressure is 2.0～10.0MPa, and volume space velocity is 0.5～5.0h
-1, temperature of reaction is controlled at 280～370 ℃, and hydrogen to oil volume ratio is 100: 1～950: 1; Reactor top reaction zone filling base metal sulfide catalyst, lower reaction zone filling as-reduced metal catalyzer or the noble metal catalyst of reactor.
2. it is characterized in that in accordance with the method for claim 1: the top reaction zone diameter increases by 4%～15% than adjacent lower reaction zone diameter.
3. in accordance with the method for claim 1, it is characterized in that the hydrogenation operation condition is: pressure is 4.0～8.0MPa, and volume space velocity is 1.0～3.0h
-1, temperature of reaction is controlled at 320～360 ℃, and hydrogen to oil volume ratio is 300: 1～800: 1.
4. it is characterized in that in accordance with the method for claim 1: a gas and liquid flowing reactor of series connection before the gas-liquid counter current reactor.
5. it is characterized in that in accordance with the method for claim 1: the liquid stream that derive in the hydrops district carries out importing the reactor lower part reaction zone after heat exchange again.
6. in accordance with the method for claim 1, it is characterized in that: hydrops district excess liq enters liquid distributor by the overflow mode, flows into following reaction zone beds.
7. it is characterized in that in accordance with the method for claim 1: hydrops is derived on pipeline flowrate control valve is set.
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| CN102041070A (en) * | 2009-10-21 | 2011-05-04 | 中国石油化工股份有限公司 | Diesel gas-liquid countercurrent hydrogenation method |
| CN103102942B (en) * | 2011-11-10 | 2015-04-01 | 中国石油化工股份有限公司 | Treating method for in-depth dearomatization of diesel oil fraction |
| CN103102943B (en) * | 2011-11-10 | 2015-05-13 | 中国石油化工股份有限公司 | Treating method for in-depth desulphurization and dearomatization of diesel oil fraction |
| CN103773499B (en) * | 2012-10-24 | 2016-01-06 | 中国石油化工股份有限公司 | A kind of hydrorefining petroleum waxes method |
| CN103773474B (en) * | 2012-10-24 | 2016-03-30 | 中国石油化工股份有限公司 | A kind of gas phase, liquid-phase mixing hydrogenation method |
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|---|---|---|---|---|
| EP0905216A2 (en) * | 1997-09-26 | 1999-03-31 | Exxon Research And Engineering Company | Countercurrent reactor with interstage stripping in gas/liquid contacting zones |
| CN1488715A (en) * | 2002-10-10 | 2004-04-14 | 中国石油化工股份有限公司 | Diesel oil deep-hydro-desulfurizing-dearomatizing method |
| CN2761258Y (en) * | 2004-10-29 | 2006-03-01 | 中国石油化工股份有限公司 | Gas-liquid counterflow reactor |
| CN101376837A (en) * | 2007-08-27 | 2009-03-04 | 中国石油化工股份有限公司 | Diesel deep desulfurization and dearomatization hydrotreating process |
-
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- 2009-10-16 CN CN2009101879299A patent/CN102041069B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0905216A2 (en) * | 1997-09-26 | 1999-03-31 | Exxon Research And Engineering Company | Countercurrent reactor with interstage stripping in gas/liquid contacting zones |
| CN1488715A (en) * | 2002-10-10 | 2004-04-14 | 中国石油化工股份有限公司 | Diesel oil deep-hydro-desulfurizing-dearomatizing method |
| CN2761258Y (en) * | 2004-10-29 | 2006-03-01 | 中国石油化工股份有限公司 | Gas-liquid counterflow reactor |
| CN101376837A (en) * | 2007-08-27 | 2009-03-04 | 中国石油化工股份有限公司 | Diesel deep desulfurization and dearomatization hydrotreating process |
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