CN102041069A - 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
Because petroleum resources deficient day by day and to the continuous growth of diesel oil demand in the world wide, it is increasing to derive from the shared share of the diesel oil of heavy oil cracking, causes containing in the diesel oil distillate 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 that the burning back forms is serious day by day to the pollution of environment, causes the common concern of countries in the world gradually.
At present hydrogenation remains and removes in the diesel oil distillate heteroatoms such as sulphur, nitrogen and carry out the saturated most economical effective scheme of aromatic hydrogenation.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 restraining effect Deng the gaseous impurities competitive adsorption.In addition, H
2S, NH
3Deng gaseous impurities and C
1, C
2Enter in the recycle hydrogen Deng the micro-molecular gas hydro carbons, can cause the hydrogen dividing potential drop to reduce, influence hydrogenation and take off the impurity and the saturated degree of depth of aromatic hydrocarbons.The operation of hydrogenator gas-liquid counter current can be avoided above-mentioned shortcoming, can in time remove most of H
2S, NH
3Deng gaseous impurities, increase hydrogen partial pressure, promote hydrogenation reaction, therefore more and more be subjected to researchist's attention.
In the gas-liquid counter current hydrogenator, liquid stream enters from the top of reactor, flows out from the bottom of reactor, and recycle hydrogen then enters from the bottom of reactor, flows out from the top.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 is easy to generate 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, rerum natura and fluid properties have nothing in common with each other, 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, gas-liquid two-phase interacts and strengthens, and it is smooth and easy dirty that the frictional force between ascending gas and dropping liq begins 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 liquid was withstood by gas and was difficult to flow downward this moment, and beds liquid is accumulated rapidly and finally caused liquid flooding.When liquid flooding takes place, have tangible liquid on the 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 the loading point, and spotting out is following to be the optimum operation district.Because loading point is difficult to usually determine that operating gas velocity is selected 50%～80% of spotting out gas speed on the experience.In the hydrogenation process, because upwards 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, increase so can form the gas flow on reactor top, the probability that causes liquid flooding to take place increases.
The aromatic hydrocarbons of diesel oil is saturated to be strong exothermal reaction, so the beds temperature rise is higher.Under the temperature conditions of higher, the hydrogenation of aromatic hydrocarbons can be subjected 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 that has gas, fluid path.When reactor generation liquid flooding, liquid can flow into next bed by fluid path.When gas velocity was big, beds pressure reduction was bigger, and gas can enter a last bed by the gas passage.Catalyst bed interlayer non-reaction zone is provided with inlet mouth, can play the effect of similar cold hydrogen, though 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 be provided with more gas, liquid path, reactor effective volume utilization ratio is not high, and operability is lower.
Summary of the invention
At the deficiencies in the prior art, the invention provides a kind of new diesel oil gas-liquid counter current 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 the reaction zone.Under the condition that the upper reaches gas flow increases with height for reactor, keep gas velocity relatively stable, reduce the reaction zone liquid flooding and take place, increase the reactor turndown ratio.Simultaneously at least one reducing place, reaction zone boundary the hydrops district is set, it mainly accumulates the lower liquid of wall stream temperature and the gas speed entrained liquids when big.Bottom, hydrops district or sidepiece are provided with hydrops and derive pipeline, and the liquid that hydrops district temperature is lower imports the reactor lower part reaction zone, as the cooling logistics, can reduce the temperature rise of lower catalyst bed layer reaction zone, promote the aromatic hydrocarbons saturated reaction, prolong catalyst life.
The gas-liquid counter current method of hydrotreating that diesel fuel desulfurization of the present invention, denitrogenation and aromatic hydrocarbons are saturated 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 promptly hydrogen is entered by reactor bottom, discharge from reactor head, liquid phase is entered by reactor head, contacts with hydrogen is reverse, discharges from reactor bottom.
Wherein related reactor is divided into 2 reaction zones at least, and each reaction zone is made up 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%, preferred 4%～15% than adjacent lower reaction zone diameter.The height of each reaction zone is 20%～80% of a 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 the lower liquid of wall stream temperature and the gas speed entrained liquids when big.Bottom, hydrops district or sidepiece are provided with pipeline, and the liquid that temperature is lower imports the reactor lower part reaction zone, to reduce the beds temperature rise.The amount that the hydrops district imports reactor lower part reaction zone liquid stream is 2%～15% of an inlet amount, preferred 4%～10%.If hydrops district liquid is more, hydrops district excess liq can enter liquid distributor by the overflow mode, reaction zone beds below flowing into.Can derive pipeline at hydrops in case of necessity interchanger is set, so that beds reaches optimal reaction temperature.Hydrops is derived on the pipeline can also be provided with flowrate control valve.
The wherein related conventional base metal sulfide catalyst of reactor top reaction zone filling, FF-98, FH-UDS etc. as Fushun Petrochemical Research Institute's development are mainly used in heteroatomss such as removing 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., also can be the base metal sulfide catalyst that is difficult for losing sulphur, form the high activated catalyst bed, be mainly used in the aromatic hydrocarbons saturated reaction.
The hydrogenation reaction operational 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 condition can be according to feedstock property and quality product requirement, and is simply definite by experiment.
This reactor can use in single hop list device technology, and the gas and liquid flowing reactor of also can connecting in front is applied in the single hop tandem process, and the gas and liquid flowing reactor adopts this area routine operation condition.In a kind of technology in back, can strengthen the effect of gas-liquid counter current reactor hydrogenation aromatics-removing.
Technical characterstic of the present invention and advantage comprise:
1, adopts the Design Mode of reactor reducing, promptly can give full play to the technical superiority of counter-current operation, can guarantee whole device smooth operation again.
When 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 the process of reactor, the hydrogen dividing potential drop increases, and can improve impurity extrusion rate and aromatic hydrocarbons saturation depth.
3, adopt the gas-liquid counter current operator scheme of a plurality of beds, can so that hydrogen in the process that axially rises along reactor, take hydrogen sulfide and ammonia that reaction generates out of reactor, thereby can avoid the two influence, can obtain high-quality product for lower catalyst bed layer hydrogenation reaction effect.
4, adopt the design of reactor reducing can increase catalyst bed layer cross section space in the reaction zone (gas, liquid circulation area).Under the condition that the upper reaches gas flow increases with height for reactor, keep gas velocity relatively stable, prevent that the reaction zone liquid flooding from taking place, and increases the reactor turndown ratio.
5, the liquid of hydrops district lesser temps is gone into reactor lower part as the refrigerant conductance, can guarantee lower beds temperature rise under the condition that does not reduce air speed.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, prolongs the catalyst runs life-span.Can the liquid stream that derive in the hydrops district be carried out importing the reactor lower part reaction zone again after the heat exchange in case of necessity, with further reduction temperature.
7, the position of hydrops district importing reactor lower part reaction zone liquid stream is a meaning position, position, generally determines according to reaction zone reaction bed temperature distribution situation.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 bigger, the inventory that can suitably increase the importing reactor lower part is to reduce reaction bed temperature, this moment is owing to the catalyst activity height, so can't finally not take off the impurity degree of depth because of partial material influences through whole beds; 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, and this moment is owing to the whole beds of most of material process, so still can guarantee finally to take off the degree of depth of impurity.
Description of drawings
Fig. 1 is the saturated gas-liquid counter current method of hydrotreating gas-liquid counter current structure of reactor synoptic diagram of a kind of diesel fuel desulfurization of the present invention, denitrogenation and aromatic hydrocarbons.
Embodiment
Be explanation the solution of the present invention and effect, further specify feature of the present invention by following examples:
Present embodiment is mainly investigated hydrogenating desulfurization, denitrogenation and the aromatic hydrocarbons saturation effect of gas-liquid counter current hydrogenator of the present invention.
Present embodiment adopts the one-stage serial technical process, and 2 reactors are set, and the 1st reactor is that gas and liquid flowing is operated downwards, and the 2nd reactor is the gas-liquid counter current operation.The gas-liquid counter current reactor is made up 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 a raw material inlet amount.Hydrops district tapping heat exchange to 260 ℃ enters in the middle of the counter-current reactor lower reaction zone.
Co-current reactor and counter-current reactor top reaction zone adopt W-Mo-Ni-Co type Hydrobon catalyst (catalyst A) in the present embodiment, 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 characteristics high to the aromatic hydrogenation saturated activity under the mitigation condition.The catalyzer physico-chemical property sees Table 1.Stock oil character sees 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
| |
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 |
| Recycle hydrogen is taken oil out of | Do not have | Do not have | Do not have | Do not have |
| 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 technology, and adaptability to raw material is wide, and the device stable operation has improved the industrial applicibility of this Technology.
Claims (10)
1. gas-liquid counter current method of hydrotreating that diesel fuel desulfurization, denitrogenation and aromatic hydrocarbons are saturated, 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, discharge from reactor head, liquid phase is entered by reactor head, contacts with hydrogen is reverse, discharges from reactor bottom; It is characterized in that: reactor is divided into 2 reaction zones at least, and each reaction zone is made up 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 are provided with hydrops and derive pipeline, with the liquid importing reactor lower part reaction zone in hydrops district, as the cooling logistics.
2. in accordance with the method for claim 1, it is characterized in that: 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 a whole reactor virtual height.
3. according to claim 1 or 2 described methods, it is characterized in that: the top reaction zone diameter increases by 4%～15% than adjacent lower reaction zone diameter.
4. in accordance with the method for claim 1, it is characterized in that the hydrogenation reaction operational condition is: pressure is 2.0～10.0MPa, and volume space velocity is 0.5～5.0, and temperature of reaction is controlled at 280～370 ℃, and hydrogen to oil volume ratio is 100: 1～950: 1.
5. in accordance with the method for claim 1, it is characterized in that the hydrogenation reaction operational 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.
6. in accordance with the method for claim 1, it is characterized in that: reactor top reaction zone filling base metal sulfide catalyst, the lower reaction zone filling as-reduced metal catalyzer or the noble metal catalyst of reactor.
7. it is characterized in that in accordance with the method for claim 1: gas and liquid flowing reactor of series connection before the gas-liquid counter current reactor.
8. 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 again after the heat exchange.
9. in accordance with the method for claim 1, it is characterized in that: hydrops district excess liq enters liquid distributor by the overflow mode, reaction zone beds below flowing into.
10. it is characterized in that in accordance with the method for claim 1: hydrops is derived on the 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 |
| CN103102943A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Treating method for in-depth desulphurization and dearomatization of diesel oil fraction |
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| CN103102942A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Treating method for in-depth dearomatization of diesel oil fraction |
| 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 |
| CN103773499A (en) * | 2012-10-24 | 2014-05-07 | 中国石油化工股份有限公司 | Petroleum wax hydrofining method |
| CN103773474A (en) * | 2012-10-24 | 2014-05-07 | 中国石油化工股份有限公司 | Gas phase-liquid phase mixed hydrogenation method |
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