CN104232154A - Distillate oil hydro-upgrading method - Google Patents
Distillate oil hydro-upgrading method Download PDFInfo
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- CN104232154A CN104232154A CN201310248094.XA CN201310248094A CN104232154A CN 104232154 A CN104232154 A CN 104232154A CN 201310248094 A CN201310248094 A CN 201310248094A CN 104232154 A CN104232154 A CN 104232154A
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Abstract
The invention relates to a distillate oil hydro-upgrading method which comprises the following steps: mixing stock oil and hydrogen at a hydrogen-oil volume ratio of (10-100):1, and feeding a mixture into a first reactor from the bottom of the first reactor; feeding generated oil and supplemental hydrogen into a second reactor from the bottom of the second reactor; and feeding the generated oil into a gas-liquid separator and performing steam stripping separation so as to separate out liquid oil and a gas, wherein a catalyst used for the first reactor is a hydrotreating catalyst mainly for denitrification over desulfuration, a catalyst used for the second reactor is the same as the catalyst used for the first reactor or is a hydrotreating catalyst mainly for desulfuration over denitrificationl, and the conditions of a hydrogenation process are as follows: the reaction pressure is 6.0-17.0 MPa, the reaction temperature is 300-400 DEG C, and the volumetric space velocity is 0.1-3.0 h<-1>. The distillate oil hydro-upgrading method disclosed by the invention can be used for producing a diesel oil product with sulfur content less than 10 micrograms/gram by virtue of hydro-upgrading of inferior diesel oil.
Description
Technical field
The present invention relates to a kind of distillate hydrogenation modification process.
Background technology
Heavy distillate is often referred to vacuum distillate (VGO), coking heavy distillate (CGO) or deasphalted oil (DAO).Because boiling range is heavier, wherein containing impurity such as more sulphur, nitrogen and heavy metals.When raw material as downstream catalytic cracking or hydrocracking, the activity of catalyzer can be reduced, time serious, even can affect the steady running of device.Generation oil after heavy distillate hydrotreatment has the low feature of the foreign matter content such as sulphur, nitrogen, can as the raw material of downstream catalytic cracking unit or hydroeracking unit.
Along with heaviness and the in poor quality of crude oil, the foreign matter contents such as the sulphur in heavy distillate, nitrogen are more and more higher, and this has considerable influence to the steady running of downstream catalytic cracking unit or hydroeracking unit and quality product.Sulphur, the foreign matter content such as nitrogen and heavy metal of the heavy distillate after hydrotreatment have obvious decline, when raw material as catalytic cracking unit, obviously product slates be can improve, light oil yield and quality product improved, reduce SOx and the NOx content in FCC flue gas, reduce environmental pollution.
Chinese patent CN102465027A discloses a kind of heavy distillate oil hydrotreating method, first stock oil and hydrogen enter gas liquid mixer through process furnace, hydrogen and stock oil are fully mixed, then enters the first reactor, contact with hydrogenation catalyst under hydroprocessing conditions; Gained reaction effluent enters stripping and mixes in hydrogen storage equipment, removes the hydrogen sulfide and ammonia that dissolve in oil, and makes hydrogen in oil, reach dissolving state of saturation, is then mixed into the second reactor with hydrogen make-up and contacts with hydrogenation catalyst.Except traditional circulating hydrogen compressor system in the method, also increase gas liquid mixer and stripping mixes hydrogen device, cost of investment increases.
Chinese patent CN101348732A discloses a kind of heavy oil hydrogenation treatment method, especially improves the heavy oil hydrogenation treatment method of diesel quality.With heavy distillate and animal-plant oil for stock oil, under hydroprocessing conditions, stock oil mixes with hydrogen by hydrotreatment reaction zone, and hydrotreatment generates the separating of oil hydrogen-rich gas recycle obtained, and is separated the liquid fractionation obtained and obtains diesel product and hydrogenation wax oil.In the method operational condition and ordinary method basically identical, can not operational condition be relaxed.
Chinese patent CN101376841A discloses a kind of heavy distillate oil hydrotreating method.Take heavy ends as stock oil, under hydroprocessing conditions, stock oil mixes by the first hydrotreatment reaction zone with hydrogen, hydrotreatment generates oil and mixes by the second hydrotreatment reaction zone with the hydrogen after circulating hydrogen compressor supercharging, hydrotreatment generates oil and is separated in high-pressure separator, and the liquid obtained obtains low sulfur light oil product and heavy oil product in separation column.There is recycle hydrogen system in the method, technique is more complicated, and cost of investment is higher.
In traditional trickle bed hydrogenation technique, hydrogen needs to be delivered to liquid phase from gas phase, and then dissolved hydrogen and sulfocompound react in the active centre of catalyzer, thus reach desulfurization object.In the process, required amounts of hydrogen is far longer than the amounts of hydrogen that hydrogenation reaction consumes.This is because on the one hand, hydrogenation reaction is a strong exothermal reaction, in order to maintain temperature of reaction, a large amount of hydrogen and stock oil is needed to take away reaction heat by beds; In addition on the one hand, in the reaction of airwater mist cooling, maintain higher hydrogen dividing potential drop and be conducive to hydrogenation reaction, suppress coke to generate, the extending catalyst life-span.In addition, be again transported to after the hydrogen not participating in reaction is improved pressure by circulating hydrogen compressor in reactor and participate in reaction.Circulating hydrogen compressor as the key equipment of hydrogenation process, investment and process cost higher.In order to cancel recycle hydrogen and circulating hydrogen compressor, reduce the cost of investment of device, liquid phase hydrogenation technology is carried out.
US Patent No. 20060144756A1 discloses a kind of two-phase hydrogenation Controlling System method and apparatus.In continuous print liquid-phase hydrogenatin process, eliminate recycle hydrogen, under solvent or thinner existent condition, by the mixing of hydrogen oil, hydrogen is greater than the solubleness in stock oil in the solubleness of solvent or thinner.Hydrogen required for hydrogenation reaction all comes from the hydrogen of liquid phase dissolved, does not need extra hydrogen.But it does not consider that the hydrogenation byproduct such as hydrogen sulfide and ammonia produced in hydrogenation process is to the restraining effect of hydrogenation reaction, causes it to accumulate in reaction system, affect the hydrogenation efficiency in the solubleness of hydrogen and reaction process.
Hydrogenation byproduct hydrogen sulfide and ammonia have certain restraining effect to hydrogenation reaction.Mainly hydrogen sulfide and ammonia and the competitive adsorption of reactant on catalyst activity position, affect hydrogenation reaction efficiency.Therefore, the impact of removal of hydrogen sulfide and ammonia is significant to raising distillate hydrogenation efficiency.Chinese patent CN101787305A discloses a kind of inner member arranging gas make-up and discharge impurities excess air between beds, is removed hydrogen sulfide and the ammonia of reaction generation by the mode of air lift.Chinese patent CN101724443A discloses and adopts inner cross-flow reactor, removes byproduct of reaction hydrogen sulfide and ammonia by air lift.The feature of these patented technologies is in reactor, remove hydrogen sulfide and ammonia, increases capital cost of reactor cost.
Summary of the invention
The object of this invention is to provide a kind of distillate hydrogenation modification process, present method technical process is simple, and stable operation, product property is good, can old device also can be utilized to transform by newly-built hydrogenation unit.
A kind of distillate hydrogenation modification process of the present invention comprises following content:
Stock oil heats afterwards and hydrogen enters hydrogen oil mixing tank, and excess hydrogen and saturated liquid phase batch mixing enter the first reactor from reactor bottom; Reaction generates oil and hydrogen make-up enters reactor from the second reactor bottom; Reaction generates oily air inlet liquid/gas separator; Isolated liquid oil enters storage tank; Isolated gas discharges system.
Described hydrogenation process conditions is: reaction pressure 6.0MPa ~ 17.0MPa, and temperature of reaction is 300 DEG C ~ 400 DEG C, and volume space velocity is 0.1h
-1~ 3.0h
-1, hydrogen to oil volume ratio 10 ~ 100:1.
The catalyzer used in first reactor take denitrogenation as the main hydrotreating catalyst taking into account desulfurization.
The catalyzer used in second reactor with the first reactor, or based on desulfurization, takes into account the hydrotreating catalyst of denitrogenation.
According to hydrogenation method of the present invention, in a kind of embodiment, the preferred high-pressure gas-liquid separator of described gas-liquid separator.
In a kind of heavy distillate hydrogenation modifying process of the present invention method, adopt the pattern of low excess hydrogen and lower charging, be dissolved in stock oil by saturated in advance for hydrogen, the liquid mixing material being then dissolved with saturated hydrogen enters each fixed bed hydrogenation reactor and carries out liquid-phase hydrogenatin reaction.Liquid oil soaks whole beds.Avoid the problem of the reactor top air chamber that upper feeding pattern is brought.Meanwhile, excess hydrogen has two effects, and the first, the amount that postreaction consumes; The second, the impurity hydrogen sulfide that stripping reaction generates and ammonia.
In a kind of heavy distillate hydrogenation modifying process of the present invention method, hydrogenation technique operational condition and catalyzer are also close with prior art, as hydrogen dividing potential drop 4.0MPa ~ 16.0MPa; Temperature of reaction is 320 DEG C ~ 420 DEG C; Volume space velocity is 0.3h
-1~ 2.0h
-1.This hydrogen to oil volume ratio higher than the ability of the dissolved hydrogen of distillate feedstock, namely in reaction system except the hydrogen be dissolved in distillate feedstock, there is gas phase hydrogen.In hydrogenation method of the present invention, eliminate circulating hydrogen compressor system, in advance a part of hydrogen is dissolved in stock oil, compared with traditional hydrogenation technique, only there is chemical hydrogen consumption in reactive system, exists and non-chemically consume hydrogen on a small quantity.
In a kind of heavy distillate hydrogenation modifying process of the present invention method, the hydrotreating catalyst that the first reactor uses selects commercial goods hydrotreating catalyst, or is prepared according to the technology of this area.Described hydrotreating catalyst selects the conventional hydrogenation catalyst of this area, and the inventive method recommendation take denitrogenation as the main hydrotreating catalyst taking into account desulfurization, and catalyzer is not containing molecular sieve, and carrier is aluminum oxide; The hydrotreating catalyst that second reactor uses selects the conventional catalyst of this area, or identical with the catalyzer that the first reactor uses.
The inventive method, compared with conventional one section series hydrogenation refining process, needs increase gas liquid mixer, and cancel circulating hydrogen compressor system, oil property can reach the unapproachable effect of ordinary method, and reaction conditions comparatively relaxes.
The Main Function of gas liquid mixer makes the hydrogen entered in the distillate of reactor reach dissolving state of saturation.Hydrotreatment is carried out usually under gas-liquid-solid reaction condition, the factor affecting hydrogenation effect is the speed that spread to solid catalyst surface by liquid film of hydrogen mainly, because the solvability of hydrogen in distillate is very poor in conventional hydrogenation process, this mode is difficult to the hydrogen solute effect of realizing ideal, and usually needs to pass into a large amount of hydrogen.Therefore, the reaction kinetics speed of prior art is subject to obvious impact.Hydrogen is fully mixed with distillate by gas liquid mixer by present method, and greatly can improve the meltage of hydrogen in distillate, experiment shows, this mode can reach capacity solute effect substantially.Make the hydrogen needed for part reaction be dissolved in stock oil in advance to go, the speed of fast response can be added, improve the hydrogenating desulfurization effect of refining reaction device.
The inventive method is compared with liquid-phase hydrogenatin process for refining, and cancel liquid circulating pump, oil property can reach effect more better than liquid-phase hydrogenatin, and reaction conditions comparatively relaxes.
Gas-liquid separator Main Function removes the second reactor to generate hydrogen sulfide in oil and ammonia, can obtain the hydrogenated products of sulfide hydrogen and ammonia hardly.
In distillate hydrogenation treatment process method of the present invention, the boiling range of distillate is generally 65 DEG C ~ 550 DEG C, generally includes petroleum naphtha, catalytic diesel oil, coker gas oil, straight-run diesel oil, rocket engine fuel, scale wax, straight-run gas oil, vacuum distillate, wax tailings or deasphalted oil.Reactive hydrogen dividing potential drop 6.0MPa ~ 17.0MPa, temperature of reaction is 300 DEG C ~ 400 DEG C, and volume space velocity is 0.1h
-1~ 3.0h
-1, recycle ratio 0:1 ~ 6:1.
The inventive method has good treatment effect to various distillate, adopt the method carry out hydro-upgrading of inferior diesel, rocket engine fuel hydrofining, petroleum naphtha hydrogenation refine, scale wax hydrofining, lubricant base weighted BMO spaces etc., can produce fine-quality diesel oil, boat coal, petroleum naphtha, paraffin, lubricant base.Adopt the method to carry out hydro-upgrading of inferior diesel and can produce the diesel product that sulphur content is less than 10 μ g/g.
The inventive method technical process is simple, and stable operation, product property is good, can old device also can be utilized to transform by newly-built hydrogenation unit.
In a kind of heavy distillate hydrogenation modifying process of the present invention method, the hydrogenation catalyst used can be commodity hydrotreating catalyst, as DZF, DZC, PHT, PHF, PHU and SD series hydrotreating catalyst that Petroleum Chemical Engineering Institute of CNPC develops.Also the catalyzer of higher hydrogenation activity can be had by art processes preparation.Concerning distillate feedstock, use common hydrotreating catalyst also can reach good effect, preferably use high-activity hydrogenation catalyst.
Accompanying drawing explanation
Fig. 1 is distillate hydrogenation process method flow chart of the present invention.
In figure: 1-stock oil, 2-process furnace, 3-hydrogen oil mixing tank, 4/5-reactor, 6-gas-liquid separator, 7-stripping gas, 8-gas meter, 9-separator lighter products exports, 10-liquid-phase product storage tank, 11-hydrogen.
Embodiment
Detailed process and the effect of distillate hydrogenation processing method of the present invention is further illustrated below in conjunction with accompanying drawing.
Liquid phase circulation hydrogenation unit of the present invention is made up of process furnace 2, mixing tank 3, reactor 4/5, separator 6, storage tank 10 and connection line.
Stock oil 1 enters process furnace 2 after heating, enters hydrogen oil mixing tank 3 with hydrogen 11, liquid phase material after mixed hydrogen and excess hydrogen enter reactor bottom the first reactor 4, first reactor 4 generates oil and enters the second reactor 5, second reactor 5 generates oil and enters separator 6, carry out stripping separation by stripping gas 7, separator 6 top is provided with gas meter 8.The isolated liquid oil of separator 6 enters storage tank 10.
It is the main hydrotreating catalyst taking into account desulfurization that first reactor uses with denitrogenation, and catalyzer is not containing molecular sieve, and carrier is aluminum oxide; Hydrotreatment/modifying catalyst that second reactor uses selects the conventional catalyst of this area, or identical with the catalyzer that the first reactor uses.According to feedstock property, load hydrogenation protecting agent and porcelain ball as required on the first reactor top.
Through the distillate feedstock of the inventive method process, the refined oil products that sulphur, nitrogen and beavy metal impurity are lower can be obtained.
Through the distillate feedstock of the inventive method process, each distillate moral character mass-energy such as the petroleum naphtha obtained, rocket engine fuel, diesel oil enough reach the unapproachable effect of ordinary method.
The hydrotreatment that experiment use catalyzer is industrial application, hydrocracking, catalyst for hydro-upgrading, be respectively the reformed pre-hydrogenated catalyzer of DZF-1 of Petroleum Chemical Engineering Institute of CNPC development and production, PHF-101 diesel hydrogenation for removal sulphur catalyst, PHT-01 heavy-oil hydrogenation pretreatment catalyst, SD-2 hydrogenation catalyst, its physico-chemical property index is in table 1.
Embodiment 1
Reformer feed through process furnace reach temperature required with hydrogen in gas liquid mixer after abundant mixed dissolution, enter the first hydrogenator, reaction conditions is: reacting system pressure 1.2MPa, temperature of reaction 256 DEG C, conversion hydrogen to oil volume ratio is 20:1, effluent 2 enters the second hydrogenator, reaction conditions is: reacting system pressure 1.2MPa, temperature of reaction 254 DEG C, conversion hydrogen to oil volume ratio is 20:1, effluent enters separator and carries out gas-liquid separation, and the liquid efflunent after separation enters storage tank.Stock oil character and product property list in table 2.
From table 2, adopt this Technology obviously can reduce sulphur, nitrogen, olefin(e) centent in reformer feed.
Embodiment 2
Medium diesel oil raw material through process furnace reach temperature required with hydrogen in gas liquid mixer after abundant mixed dissolution, enter the first hydrogenator, reaction conditions is: reacting system pressure 8.0MPa, temperature of reaction 350 DEG C, conversion hydrogen to oil volume ratio is 76:1, effluent enters the second hydrogenator, reaction conditions is: reacting system pressure 8.0MPa, temperature of reaction 350 DEG C, conversion hydrogen to oil volume ratio is 76:1, effluent enters separator and carries out gas-liquid separation, and the liquid efflunent after separation enters storage tank.Stock oil character and product property list in table 3.
From table 3, adopt that this Technology can make the sulphur in Medium diesel oil, nitrogen content obviously reduces.
Embodiment 3
Paraffinic base heavy distillate (mix refining wax tailings) through process furnace reach temperature required with hydrogen in gas liquid mixer after abundant mixed dissolution, enter the first hydrogenator, reaction conditions is: reacting system pressure 15.0MPa, temperature of reaction 385 DEG C, conversion hydrogen to oil volume ratio is 350:1, and effluent enters the second hydrogenator; Reaction conditions is: reacting system pressure 15.0MPa, temperature of reaction 383 DEG C, and conversion hydrogen to oil volume ratio is 350:1, and effluent enters separator and carries out gas-liquid separation, and the liquid efflunent after separation enters storage tank.Stock oil character and product property list in table 4.
From table 4, adopt that this Technology can make the sulphur in heavy distillate, nitrogen content obviously reduces.
Embodiment 4
64# scale wax raw material through process furnace reach temperature required with hydrogen in gas liquid mixer after abundant mixed dissolution, enter the first hydrogenator, reaction conditions is: reacting system pressure 6.5MPa, temperature of reaction 255 DEG C, conversion hydrogen to oil volume ratio is 310:1, effluent enters the second hydrogenator, reaction conditions is: reacting system pressure 6.5MPa, temperature of reaction 245 DEG C, conversion hydrogen to oil volume ratio is 310:1, effluent enters separator and carries out gas-liquid separation, and the liquid efflunent after separation enters storage tank.Stock oil character and product property list in table 5.
From table 5, adopt this Technology can improve color and the light stability of paraffin wax product.
Comparative example 1
The Medium diesel oil raw material of process same nature, adopts the correlation data of present method and ordinary method in table 6.As can be seen from Table 6, present method temperature of reaction is high 5 DEG C compared with ordinary method, and the hydrogen to oil volume ratio after conversion is only 76, be 15% of ordinary method, and product property is better than ordinary method.
Comparative example 2
The Medium diesel oil raw material of process same nature, adopts the correlation data of present method and liquid-phase hydrogenatin in table 6.As can be seen from Table 6, present method temperature of reaction is low 3 DEG C compared with liquid-phase hydrogenatin, and product property is better than liquid-phase hydrogenatin.
The physico-chemical property index of table 1 catalyzer
Table 2 embodiment 1 reformer feed oil nature and test-results
Table 3 embodiment 2 Medium diesel oil character and test-results
Table 4 embodiment 3 paraffinic base heavy ends oil nature and test-results
Table 5 embodiment 4 stock oil character and test-results
Table 6 comparative example 1 stock oil character and test-results
Claims (1)
1. a distillate hydrogenation method for modifying, is characterized in that:
Boiling range is after the stock oil heating of 65 DEG C ~ 550 DEG C and hydrogen enters hydrogen oil mixing tank, hydrogen to oil volume ratio 10 ~ 100:1, and excess hydrogen and saturated liquid phase batch mixing enter the first reactor from reactor bottom; Reaction generates oil and hydrogen make-up enters reactor from the second reactor bottom; Reaction generates oily air inlet liquid/gas separator; Isolated liquid oil enters storage tank; Isolated gas discharges system;
The catalyzer used in first reactor for denitrogenation be the main hydrotreating catalyst taking into account desulfurization;
The catalyzer used in second reactor with the first reactor, or based on desulfurization, takes into account the hydrotreating catalyst of denitrogenation;
Hydrogenation process conditions is: reaction pressure 6.0MPa ~ 17.0MPa, and temperature of reaction is 300 DEG C ~ 400 DEG C, and volume space velocity is 0.1h
-1~ 3.0h
-1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108203600A (en) * | 2016-12-16 | 2018-06-26 | 中国石油天然气股份有限公司 | A kind of method for improving kerosene oxidation stability |
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