CN102876372B - Single-stage series hydrofinishing method of diesel oil - Google Patents
Single-stage series hydrofinishing method of diesel oil Download PDFInfo
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Abstract
The invention discloses a single-stage series hydrofinishing method of diesel oil. According to the invention, the diesel oil raw material contacts with a hydrofining catalyst at the reaction pressure of 3.0-10.0 MPa at the temperature of 220-320 DEG C at the liquid hourly space velocity of 1-10h<-1> and at the hydrogen-oil volume ratio of 100-1000; without undergoing separation, a reaction effluent contacts with the hydrofining catalyst at the temperature of 330-400 DEG C and at the liquid hourly space velocity of 0.5-6.0h<-1>; and the reaction effluent is separated, wherein a liquid product enters a fractionating system. According to the method, the diesel oil raw material firstly undergoes hydrogenation under the conditions of high space velocity and low temperature, and simple sulfide and nitride are removed; and then, hydrogenation is carried out under the conditions of low space velocity and high temperature, thus being beneficial to deep desulphurization reaction and fully utilizing formation heat of a low-temperature reactor. By the adoption of the method, diesel oil with sulfur content being less than 50 micrograms and less than 10 micrograms can be produced.
Description
Technical field
The present invention relates to a kind of hydrocarbon hdyrotreating method, specifically a kind of single hop series connection diesel oil hydrofining method that is applicable to produce ultra-low-sulphur diesel.
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.The exploitation of deep hydrodesulfurizationof of diesel oil technology becomes the focus of current research.At present, Diesel Oil Hydrofining Unit operating process is that stock oil passes through same refined diesel oil mostly, reaction product heat exchange, and be heated to after reaction requires temperature enter hydrofining reactor through process furnace, this is a kind of hydrogenation flow process of routine, its advantage is easy to operate, but produce for ultra-low-sulphur diesel, its temperature of reactor and Hydrogen distribution are very unreasonable, because industrial diesel oil hydrogenator belongs to adiabatic reactor, reactor catalyst bed exists larger axial temperature difference (the deep hydrodesulfurizationof reactor bed temperature difference is larger), often entrance feeding temperature is lower, and need in reactor, inject cold hydrogen in order to control reactor outlet temperature.Because ultra-low-sulphur diesel need of production removes dibenzothiophene and contains sterically hindered dibenzothiophene class sulfide, as 4, 6-DMDBT, and this part sulfide temperature of reaction lower than 320 ℃ of conditions under hardly reaction, therefore, cryogenic reaction zone is for 4, removing of 6-DMDBT is inoperative, and for simple sulfide as mercaptan, thioether, thiophene and simple dibenzothiophene, under lower temperature of reaction and higher volume space velocity, can remove rapidly, but just enter high temperature reaction zone after relying on the intensification of reaction heat nature need to arrive reactor middle and lower part in traditional single reactor bed, low temperature reaction conversion zone is long, make simple sulfide in cold zone cannot proceed 4 after removing completely, 6-DMDBT removes, reduced the service efficiency of cryogenic reaction zone catalyzer.Therefore, under the certain condition of cumulative volume air speed, be equivalent to increase high temperature section volume space velocity, be unfavorable for the performance of catalyzer overall performance.Simultaneously a large amount of cold hydrogen is used has also increased device hydrogen consumption, energy consumption.
Summary of the invention
For the deficiency of existing diesel oil hydrofining reaction process, the invention provides a kind of single hop series connection diesel hydrogenation process.This process unit investment is little, and Energy Intensity Reduction, can be for the production of ultra-low-sulphur diesel.
Bavin hydrogenation method of the present invention comprises following content:
(1) diesel raw material and hydrogen in the first hydrofining reactor with Hydrobon catalyst contact reacts, to remove in diesel oil distillate the impurity such as simple sulphur, nitrogen; Reaction conditions is, 220 ℃～320 ℃ of temperature of reaction, reaction pressure 3.0MPa～10.0MPa, volume space velocity 1.0h during liquid
-1～10.0h
-1, hydrogen to oil volume ratio 100～1000;
(2) first hydrofining reactor effluents enter the second hydrofining reactor without separation, contact with hydrogen, Hydrobon catalyst; Reaction conditions is, 330 ℃～400 ℃ of temperature of reaction, reaction pressure 3.0MPa～10.0MPa, volume space velocity 0.5h during liquid
-1～6.0h
-1, hydrogen to oil volume ratio 200～2000;
(3) second hydrofining reactor effluents enter cold high pressure separator after cooling, the fractionating system that isolated product liquid enters, and gas is through purifying, and hydrogen-rich gas loops back reactor.
According to single hop series connection diesel oil hydrofining method of the present invention, in step (2), the first hydrofining reactor effluent first passed through process furnace before entering the second hydrofining reactor.In step (3) the second hydrofining reactor effluent through the mixture heat exchange with diesel raw material or diesel raw material and hydrogen realize cooling after, then enter cold high pressure separator.
In diesel oil hydrofining method of the present invention, the first hydrofining reactor and the second hydrofining reactor can be used identical or different Hydrobon catalysts, preferably use different Hydrobon catalysts.Preferably at the first hydrofining reactor, use active relatively low Hydrobon catalyst, the second hydrofining reactor is used active relatively high Hydrobon catalyst.The first reactor is selected the Mo-Co type catalyzer that direct desulfurization activity is higher, the Mo-Ni type Hydrobon catalyst that the second reactor use hydrogenation activity is higher or the body phase method catalyzer of high metal content.The activity of hydrogenation catalyst is main relevant to contained active metal component content, and the preparation method of catalyzer is, the use of auxiliary agent also affects the activity of catalyzer simultaneously.The consumption of the first reactor and the second reactor catalyst can according to raw material oil properties and quality product requires and catalyst property is specifically determined.Common the first reactor catalyst consumption is less than the second reactor catalyst consumption, and general volume ratio is 1: 2～1: 10, preferably 1: 4～1: 8.
The first hydrofining reactor generally reacts under low temperature, high-speed, and the second hydrofining reactor reacts under high temperature, low-speed.High temperature described herein, low temperature and high-speed are relative with low-speed.In the present invention, the liquid hourly space velocity of the second hydrofining reactor will be lower than the first hydrofining reactor, and the temperature of reaction of the second hydrofining reactor is higher than the first hydrofining reactor.The operational condition of general the first reactor is as follows: 220 ℃～320 ℃ of temperature of reaction, preferably 240 ℃～300 ℃, reaction pressure 3.0MPa～10.0MPa, preferred 4.0MPa～8.0MPa, volume space velocity 1.0h during liquid
-1～10.0h
-1, preferred 4h
-1～8.0h
-1, hydrogen to oil volume ratio 100～1000, preferably 200～800.
The operational condition of the second reactor is as follows: 330 ℃～400 ℃ of temperature of reaction, preferably 340 ℃～380 ℃, reaction pressure 3.0MPa～10.0MPa, preferred 4.0MPa～8.0MPa, volume space velocity 0.5h during liquid
-1～6.0h
-1, preferred 1.0h
-1～3.0h
-1, hydrogen to oil volume ratio 200～2000, preferably 400～1000.
In diesel oil hydrofining method of the present invention, the diesel raw material described in step (1) can be straight-run diesel oil, secondary processing diesel oil or their parallel feeding, preferably the mixing oil of secondary processing diesel oil or secondary processing diesel oil and straight-run diesel oil.
When carrying out ultra-low-sulphur diesel production, there is larger problem in conventional diesel hydrofining single hop single reactor technique.Reactor inlet temperature arranges when too low, due in reactor without external heat source heat supply, rely on separately exothermic heat of reaction to heat up, in reactor, cold zone scope is excessive, after simple sulfide removes completely, reaction still, in cold zone, cannot further complete removing of complicated sulfide.Therefore, this part superfluous cold zone catalyzer is difficult to bring into play its effect.And arrange when too high when reactor inlet temperature, having increased plant energy consumption on the one hand, the design of single hop single reactor all concentrates in a reactor diesel oil hydrogenation exothermic heat of reaction on the other hand, makes temperature out too high, is unfavorable for device long-term operation.Therefore, often in the middle of the bed liquid hydrogen injection to reduce temperature out.At this moment, compare with single hop tandem process, negative effect has been played in the heat release of simple sulfide reaction.Device hydrogen consumes, energy consumption is higher.
In diesel oil hydrofining method of the present invention, in low-temp reaction device, diesel oil reacts under high-speed, low temperature, mainly removes sulfide simple in structure, nitride.Because temperature of reaction is lower, therefore, without process furnace heating, only need can reach with the second hydrofining reactor effluent heat exchange the entrance temperature of reaction of low-temp reaction device requirement; Simultaneously, can design the feed volume air speed in low-temp reaction device according to feedstock property, low-temp reaction device is removed under the prerequisite of simple sulfide and nitride satisfied, the catalyst volume taking minimizes, and takes full advantage of the feature that simple sulfide, nitride can react under low temperature, high-speed.Low-temp reaction device reaction effluent enters high-temperature reactor after mixing with circulating hydrogen and new hydrogen after process furnace heating and carries out deep desulfuration, denitrification reaction.After being positioned over to low-temp reaction device, high-temperature reactor can make full use of the Heat of Formation that in low-temp reaction device, simple sulfide, nitride react, reduce process furnace load, process furnace can also, according to two anti-reaction depth requirement and feedstock properties, be adjusted the second reactor reaction temperature after being placed on low-temp reaction device flexibly.Simultaneously, low-temp reaction heat is separated with high-temperature reaction heat, when utilizing low-temp reaction heat, low-temp reaction heat and the stack of high-temperature reaction heat in same reactor have been avoided, and bed temperature rise declines compared with single reactor bed overall temperature rise in high-temperature reactor, the even inactive cold hydrogen of usage quantity that can reduce cold hydrogen, reduces hydrogen consumption, energy consumption.
Compare with conventional diesel hydrofining single reactor technique, single hop serial hydrogenation technique has been carried out rational distribution to reaction Heat of Formation, reactive system heat, temperature distribution are more reasonable, energy consumption, hydrogen consume lower, catalyst activity is brought into play more fully, and under the same terms, the hydrofining degree of depth is darker.
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, fresh diesel feed and reactor 6 effluents are after interchanger 7 places heat exchange, after pipeline 1 mixes with the recycle hydrogen of introducing through pipeline 16, entering hydrofining reactor 3 carries out hydrofining reaction and removes simple sulfide, reactor 3 effluents enter by pipeline 5 through process furnace 4 heating and in high-temperature reactor 6, carry out deep hydrofinishing reaction after hydrogen through pipeline 15 introducings mixes, and high-temperature reactor 6 effluents enter by pipeline 8 with raw material heat exchange that gas-liquid separator 9 carries out gas, liquid is separated.After separated, gas phase effluent enters de-hydrogen sulfide column 12 through pipeline 11 and removes hydrogen sulfide and by pipeline 13 and new hydrogen through pipeline 14 introducings, mix a part and enter high-temperature reactor 6, and another part enters reactor 3.Liquid phase part goes out device as hydrogenated products through pipeline 10.
In diesel hydrogenation process of the present invention, the catalyzer of employing can be the non-noble metal hydrogenation catalyst with hydrogenating desulfurization, hydrodenitrification and aromatic saturation function, and the function of catalyzer can stress some aspect.This non-precious metal catalyst generally exists with oxidation state form, needs before use to carry out prevulcanized, makes non-noble metal oxide be converted into sulfide and just has reactive behavior.Therefore, non-precious metal catalyst in use will keep sulphided state.The anti-low temperature hydrogenation refining reaction of the present invention one device hydrogenation catalyst used adopts the desulphurizing activated stronger Mo-Co type diesel oil hydrofining catalyst of direct hydrogenolysis.Two anti-high-temperature reactors adopt stronger Mo-Ni type, W-Ni type or the W-Mo-Ni type diesel oil hydrofining catalyst of hydrogenation activity.The Hydrobon catalyst that two reactors are selected can be selected Al
2o
3or silicon-containing alumina is as carrier.In one anti-, two anti-Hydrobon catalysts of selecting, group VIB metal content is counted 8wt%～28wt% with oxide compound, and group VIII metal content is counted 2wt%～15wt% with oxide compound, and its physical properties is as follows: specific surface area is 100～650 m
2/ g, pore volume is 0.15～0.8 mL/g.
Below by specific embodiment and comparative example, 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.In following examples, use the composition of catalyzer and character in Table 1.Feedstock property used is listed in table 3 in Table 2, embodiment 1～4 processing condition used.The evaluation result of embodiment 1～4 is in Table 5.
Composition and the main character of table 1 embodiment used catalyst
| Project | One anti-finishing agent | Two anti-finishing agents |
| Chemical constitution, quality % | ? | ? |
| MoO 3 | 18.2 | 6.2 |
| NiO | — | 12.3 |
| CoO | 7.5 | — |
| WO 3 | — | 15.2 |
| Carrier | Aluminum oxide | Silicon-containing alumina |
| Physical properties | ? | ? |
| Pore volume, mL/g | 0.45 | 0.40 |
| Specific surface area, m 2/g | 201 | 250 |
Table 2 stock oil character
| Project | Stock oil |
| Density (20 ℃), g/cm 3 | 0.8632 |
| Boiling range, ℃ | 199～375 |
| Sulphur content, μ g/g | 12000 |
| Nitrogen content, μ g/g | 406 |
comparative example 1～2
Comparative example adopts old process: the mixed hydrogen of fresh feed heats by process furnace, then, enter hydrofining reactor and carry out hydrofining reaction, reaction effluent carries out gas, liquid is separated, after separated, after gas phase depriving hydrogen sulphide, as recycle hydrogen, use, liquid phase goes out device as diesel product.
Stock oil is identical with embodiment, and Hydrobon catalyst is selected two anticatalyzers in embodiment.Comparative example 1 and 2 operational condition, respectively with embodiment 1 and 2, are listed in table 4, and experimental result is listed in table 5.
Table 3 embodiment operational condition
| ? | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Low-temp reaction device | ? | ? | ? | ? |
| Temperature of reaction, ℃ | 260 | 280 | 260 | 280 |
| Reaction pressure, MPa | 6.0 | 6.0 | 8.0 | 8.0 |
| Volume space velocity, h -1 | 6.0 | 6.0 | 5.0 | 5.0 |
| Hydrogen to oil volume ratio | 200 | 200 | 100 | 100 |
| High-temperature reactor | ? | ? | ? | ? |
| Temperature of reaction, ℃ | 360 | 360 | 350 | 350 |
| Reaction pressure, MPa | 6.0 | 6.0 | 8.0 | 8.0 |
| Volume space velocity, h -1 | 2.0 | 1.5 | 2.0 | 1.5 |
| Hydrogen to oil volume ratio | 500 | 500 | 400 | 400 |
Table 4 comparative example operational condition
| ? | Comparative example 1 | Comparative example 2 |
| Temperature of reaction, ℃ | 335 | 344 |
| Reaction pressure, MPa | 6.0 | 6.0 |
| Volume space velocity, h -1 | 1.5 | 1.2 |
| Hydrogen to oil volume ratio | 500 | 500 |
Note: in comparative example 1,2, temperature of reaction is average reaction temperature, and identical with embodiment 1,2 average reaction temperature.Comparative example 1,2 feed volume air speeds are respectively average-volume air speed in embodiment 1,2.
Table 5 embodiment 1～4, comparative example 1～2 evaluation result
| ? | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 | Comparative example 2 |
| Sulphur content, μ g/g | 45 | 8 | 52 | 12 | 55 | 18 |
| Nitrogen content, μ g/g | 5 | <1 | 7 | <1 | 12 | 4 |
As can be seen from Table 5, comparative example 1 and 2 is under employing and embodiment 1 and 2 same reaction chargings and same reaction conditions, while selecting embodiment high-temperature reactor high metals content catalysts used, comparative example 1,2 generates oily sulphur, nitrogen content still higher than embodiment 1 and 2.This explanation is when reducing hydrogen consumption, energy consumption, and diesel oil hydrogenation technical process of the present invention distributes by rational allotment temperature of reactor, has better brought into play the activity of Hydrobon catalyst, and reaction effect is better.
Claims (9)
1. a single hop series connection diesel oil hydrofining method, comprises the following steps:
(1) diesel raw material and hydrogen in the first hydrofining reactor with Hydrobon catalyst contact reacts, to remove in diesel oil distillate the impurity such as simple sulphur, nitrogen; Reaction conditions is, 220 ℃～320 ℃ of temperature of reaction, reaction pressure 3.0MPa～10.0MPa, volume space velocity 1.0h during liquid
-1～10.0h
-1, hydrogen to oil volume ratio 100～1000;
(2) first hydrofining reactor effluents enter the second hydrofining reactor without separation, contact with hydrogen, Hydrobon catalyst; Reaction conditions is, 330 ℃～400 ℃ of temperature of reaction, reaction pressure 3.0MPa～10.0MPa, volume space velocity 0.5h during liquid
-1～6.0h
-1, hydrogen to oil volume ratio 200～2000; Wherein, during the liquid of the second hydrofining reactor, volume space velocity is lower than the first hydrofining reactor, and the temperature of reaction of the second hydrofining reactor is higher than the first hydrofining reactor;
(3) second hydrofining reactor effluents enter cold high pressure separator after cooling, and isolated product liquid enters fractionating system, and gas is through purifying, and hydrogen-rich gas loops back reactor.
2. according to hydrofinishing process claimed in claim 1, it is characterized in that, in step (2), the first hydrofining reactor effluent first passed through process furnace before entering the second hydrofining reactor.
3. according to hydrofinishing process claimed in claim 1, it is characterized in that, in step (3), the second hydrofining reactor effluent is through realizing cooling with the mixture heat exchange of diesel raw material or diesel raw material and hydrogen.
4. according to hydrofinishing process claimed in claim 1, it is characterized in that, in step (1), reaction conditions is: 240 ℃～300 ℃ of temperature of reaction, reaction pressure 4.0MPa～8.0MPa, volume space velocity 4h during liquid
-1～8h
-1, hydrogen to oil volume ratio 200～800; In step (2), reaction conditions is as follows: 340 ℃～380 ℃ of temperature of reaction, reaction pressure 4.0MPa～8.0MPa, volume space velocity 1.5h during liquid
-1～4.0h
-1, hydrogen to oil volume ratio 400～1000.
5. according to hydrofinishing process claimed in claim 1, it is characterized in that, the diesel raw material described in step (1) is straight-run diesel oil, secondary processing diesel oil or their parallel feeding.
6. according to hydrofinishing process claimed in claim 1, it is characterized in that, the Hydrobon catalyst described in step (1) is Mo-Co type catalyzer, and the Hydrobon catalyst described in step (2) is Mo-Ni type, W-Ni type or W-Mo-Ni type catalyzer.
7. according to hydrofinishing process claimed in claim 6, it is characterized in that, it is carrier that described Hydrobon catalyst be take aluminum oxide or silicon-containing alumina, in catalyzer, group VIB metal content is counted 8wt%～28wt% with oxide compound, group VIII metal content is counted 2wt%～15wt% with oxide compound, and its physical properties is as follows: specific surface area is 100～650 m
2/ g, pore volume is 0.15～0.8 mL/g.
8. according to hydrofinishing process claimed in claim 1, it is characterized in that, the volume ratio of the Hydrobon catalyst in the first reactor and the second reactor is 1: 2～1: 10.
9. according to hydrofinishing process claimed in claim 8, it is characterized in that, the volume ratio of the Hydrobon catalyst in the first reactor and the second reactor is 1: 4～1: 8.
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|---|---|---|---|
| CN201110192767.5A CN102876372B (en) | 2011-07-11 | 2011-07-11 | Single-stage series hydrofinishing method of diesel oil |
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| CN102876372B true CN102876372B (en) | 2014-10-15 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1668723A (en) * | 2002-06-11 | 2005-09-14 | 日本凯金株式会社 | A process for the hydroprocessing of heavy hydrocarbon feeds using at least two reactors |
| CN102041063A (en) * | 2009-10-21 | 2011-05-04 | 中国石油化工股份有限公司 | Method for carrying out deep hydrogenation and desulfurization on diesel |
| EP2316908A1 (en) * | 2009-10-27 | 2011-05-04 | IFP Energies nouvelles | Process for hydrotreating renewable sources with indirect heating |
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- 2011-07-11 CN CN201110192767.5A patent/CN102876372B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1668723A (en) * | 2002-06-11 | 2005-09-14 | 日本凯金株式会社 | A process for the hydroprocessing of heavy hydrocarbon feeds using at least two reactors |
| CN102041063A (en) * | 2009-10-21 | 2011-05-04 | 中国石油化工股份有限公司 | Method for carrying out deep hydrogenation and desulfurization on diesel |
| EP2316908A1 (en) * | 2009-10-27 | 2011-05-04 | IFP Energies nouvelles | Process for hydrotreating renewable sources with indirect heating |
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