CN103789016B - Combined distillate oil hydroprocessing method - Google Patents
Combined distillate oil hydroprocessing method Download PDFInfo
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- CN103789016B CN103789016B CN201210432672.0A CN201210432672A CN103789016B CN 103789016 B CN103789016 B CN 103789016B CN 201210432672 A CN201210432672 A CN 201210432672A CN 103789016 B CN103789016 B CN 103789016B
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Abstract
The invention provides a combined distillate oil hydroprocessing method. Middle distillate oil which is difficult to remove impurities is processed by adoption of a traditional middle-high pressure hydrogenation technology. The produced material is fed into a hot high-pressure separator together with two-phase hydrogenation raw materials. Fresh hydrogen is supplemented from the bottom of the hot high-pressure separator. The gas phase separated from the top of the hot high-pressure separator is fed into a cold high-pressure separator. Mixed liquid-phase material flowing out from the hot high-pressure separator directly enters a two-phase hydrogenation reactor to be reacted. The gas phase separated from the cold high-pressure separator is adopted as circulating hydrogen. The liquid phase separated from the cold high-pressure separator is fed into a distillation system. The method organically combines the traditional hydrogenation technology and a two-phase hydrogenation technology, processes different materials according to advantages of each of the technologies, and achieves comprehensive processing effects.
Description
Technical field
The present invention relates to a kind of combination distillate hydrogenation treatment process, the particularly combined hydrogenation method of different mass distillate feedstock.
Background technology
Along with the continuous enhancing of people's environmental consciousness, environmental law Laws & Regulations requires more strict to engine exhaust emission, various standard of fuel requires that the content of S, N is also harsher.Simultaneously due to the continuous increase of Oil extraction amount and the continuous minimizing of conventional crude reserves, crude oil in poor quality trend is more and more serious, how the S of the intermediate oil that crude oil straight run distillation obtains and the middle runnings that the secondary processing such as coking, catalytic cracking obtains, N content also corresponding increase, be processed into the major issue that the product Shi Ge refinery that meets environmental requirement faces by middle runnings higher for the foreign matter content such as sulphur, nitrogen.
Hydrogenation process is the most economical effective scheme removing middle runnings impurity.Existing most of hydrogenation unit all adopts higher hydrogen-oil ratio and hydrogen dividing potential drop, to ensure the catalyst runs life-span, promotes the reactions such as hydrogenating desulfurization, denitrogenation, aromatic saturation and cracking.But the higher hydrogen gas circulating system of pressure needs high investment cost and running cost, indirectly adds oil manufacture cost.This traditional hydrogen addition technology is gas (being mainly hydrogen), liquid (stock oil), solid (catalyzer) phase reaction in reaction process, reactor types generally comprises trickle bed, ebullated bed, expanded bed, adverse current bed etc., its principal feature is amounts of hydrogen considerably beyond reaction institute expense, and a large amount of unreacting hydrogen recycles.Gas phase circulation hydrogen addition technology is referred to as in this patent.
Along with technician is to the understanding that deepens continuously of hydrogen addition technology, a kind of two-phase hydrogenation technology is developed.In raw material and thinning oil, dissolve supersaturation hydrogen, directly enter reactor and carry out hydrogenation reaction, cancel recycle hydrogen system, reduce costs.Owing to eliminating recycle hydrogen system, so the adaptability of this technique to raw material has certain limitation.This technology is mainly two-phase in reaction process, i.e. liquid phase (stock oil and thinning oil) and solid phase (catalyzer), claims this technique to be two-phase hydrogenation technology in this patent.
US6881326 describes a kind of two-phase hydrogenation preconditioning technique.Its technological process is that hydrogen is dissolved in oil through a mixed hydrogen production device by fresh feed oil, turning oil and hydrogen, and the oil of dissolving hydrogen enters less reactor and catalyst exposure carries out hydrogenation reaction, deviates from the impurity in oil.After reaction, a logistics part is circulated to mixed hydrogen production device, and a part is discharged from device as product.Required hydrogen is dissolved in oil before adopting raw material and turning oil to enter reactor by this method in advance, can omit recycle hydrogen system.During the method process secondary processing intermediate oil, impurity extrusion rate is difficult to up to standard.In existing two-phase hydrogenation technology, all id reaction product section is circulated as turning oil, its main deficiency is the turning oil system needing to arrange High Temperature High Pressure, facility investment and running cost higher, and the hydrogen sulfide be dissolved in oil phase is difficult to effective elimination, in reactive system, circulation accumulation, causes more serious restraining effect to hydrogenation reaction.Although can adopt as the methods such as stripping remove, owing to being in High Temperature High Pressure system, facility investment and process cost can be increased equally.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of combination distillate hydrogenation treatment process.Traditional hydrogenation technique and two-phase hydrogenation technique combine by the present invention, according to respective advantage, and processing different material.
The present invention's one combination distillate hydrogenation treatment process comprises following content:
A) distillate feedstock is divided into high-sulfur distillate feedstock and low-sulfur distillate feedstock by sulphur content, high sulfur content distillate feedstock adopts conventional gas-phase circulation hydrogen addition technology to process, material after the process of conventional gas-phase circulation hydrogen addition technology and two-phase hydrogenation low-sulfur distillate feedstock are mixed into high pressure hot separator, isolated gas phase enters cold high pressure separator, and the blended liquid phase material that high pressure hot separator flows out enters two-phase hydrogenation reactor and reacts; The isolated gas phase of cold high pressure separator recycles as recycle hydrogen, and the isolated oil phase of cold high pressure separator enters fractionating system; Fresh hydrogen fills into by bottom high pressure hot separator;
B) two-phase hydrogenation device cancels turning oil system, material after low-sulfur distillate feedstock and the process of conventional gas-phase circulation hydrogen addition technology is after high pressure hot separator mixes molten hydrogen, enter two-phase hydrogenation reactor, reclaim hydrogenation after cut oil production from two-phase hydrogenation reactor reaction effluent.
Step a) described in high-sulfur distillate feedstock and low-sulfur distillate feedstock sulphur content by 1000 ~ 12000 μ g/g preferably in 2000 ~ 8500 μ g/g arbitrary value divide, higher than divide value is high-sulfur distillate feedstock, and lower than divide value is low-sulfur distillate feedstock.High-sulfur distillate feedstock comes from secondary processing distillate usually, as one or more in coking distillate, catalytic cracking distillate, coal liquefaction fraction wet goods; Low-sulfur distillate feedstock is generally the straight run wet goods that crude distillation obtains, and also can mix a small amount of secondary processing distillate.The boiling range scope of high-sulfur distillate feedstock and low-sulfur distillate feedstock is generally one or more in kerosene(oil)fraction, diesel oil distillate, reduced pressure distillate oil distillate etc., within the scope of being preferably 130 ~ 450 DEG C, most preferably is within the scope of 200 ~ 380 DEG C.
Step a) described conventional gas-phase circulation hydrogen addition technology operational condition is: temperature of reaction 200 ~ 400 DEG C, preferably 260 ~ 380 DEG C; Reaction pressure 2.5 ~ 10.0MPa, preferably 4.0 ~ 8.0MPa; Preferred conventional gas-phase circulation hydrogen addition technology reaction pressure is higher than the reaction pressure 1 ~ 4MPa of two-phase hydrogenation device; Hydrogen to oil volume ratio 50:1 ~ 1000:1, preferred 300:1 ~ 800:1; Volume space velocity 0.6 ~ 5.0h
-1, preferably 1.0 ~ 2.5h
-1.Conventional gas-phase circulation hydrogen addition technology can adopt suitable reactor types, as trickle-bed reactor, and ebullated bed reactor, expanded bed reactor, adverse current bed bioreactor etc.
Step a) in the service temperature identical with conventional gas-phase circulation hydrogenator temperature out (ignoring the calorific loss of Flow of Goods and Materials process) of high pressure hot separator, or identical lower than conventional gas-phase circulation hydrogenator temperature out, generally higher than 200 DEG C.The service temperature of cold high pressure separator is generally 40 ~ 80 DEG C.High pressure hot separator identical with the pressure of conventional gas-phase circulation hydrogenator with the working pressure of cold high pressure separator (ignoring the pressure-losses of Flow of Goods and Materials process).High pressure hot separator bottom preferably arranges filler or gas-liquid distributor, to increase the contact of hydrogen and oil phase.Low sulfur content distillate feedstock generally enters high pressure hot separator after heat exchange or heating.
Step b) charging of described two-phase hydrogenation device reaction device can adopt the operating method of upper feeding bottom discharge, also can adopt the operating method of lower charging top discharge.Step b) described two-phase hydrogenation device operational condition is: temperature of reaction 200 ~ 400 DEG C, preferably 260 ~ 380 DEG C; Reaction pressure 1.5 ~ 8.0MPa, preferably 2.0 ~ 6.0MPa; Volume space velocity 0.6 ~ 5.0h
-1, preferably 1.0 ~ 2.5h
-1; Conventional gas-phase circulation hydrogen addition technology reaction effluent is 0.5:1 ~ 4.0:1 through the volumetric mixture ratio of liquid phase material and low-sulfur distillate feedstock that high pressure hot separator enters two-phase hydrogenation device, preferred 1.0:1 ~ 3.0:1.
The catalyzer that above-mentioned steps uses is the hydrotreating catalyst of this area routine, wherein the active metal component of catalyzer can be nickel, cobalt, molybdenum or tungsten etc. one or more, catalyzer carries out sulfidizing before use, and active metal component is converted into sulphided state.Catalyzer composition can comprise by weight percentage: nickel or cobalt are that 0.5% ~ 10%(calculates by its oxide compound), molybdenum or tungsten are that 1% ~ 25%(calculates by its oxide compound), carrier can be aluminum oxide, silicon oxide, aluminium oxide-silicon oxide, titanium oxide etc. one or more.Catalyzer is extrudate or spherical.The bulk density of catalyzer is 0.5 ~ 1.1g/cm
3, catalyst particle diameter (spherical diameter or bar shaped diameter) is 0.04 ~ 1.0mm, and specific surface area is 80 ~ 350m
2/ g.
The high pressure hot separator of conventional gas-phase circulation hydrogen addition technology of the present invention both completed gas-liquid separation, achieved again the molten hydrogen function of two-phase hydrogenation raw material.
Two-phase hydrogenation technique eliminates recycle hydrogen system, and the raw material having dissolved hydrogen contacts with hydrogenation catalyst and carries out hydrogenation reaction, so hydrogen meltage is in the feed directly connected to the degree of depth of hydrogenation reaction.The solubleness of hydrogen in hydrocarbons raises along with the rising of pressure and temperature, conventional gas-phase circulation hydrogen addition technology device recycle hydrogen system pressure of the present invention is higher than the reaction pressure of two-phase hydrogenation device, temperature simultaneously in high pressure hot separator is higher, therefore relative to two-phase hydrogenation device, liquid phase in tradition hydrogen addition technology high pressure hot separator is hydrogen hypersaturated state, more reaction hydrogen can be provided for two-phase hydrogen device, improve the impurity removal percentage of raw material.
A kind of advantage combining distillate hydrogenation treatment process of the present invention is:
1, hydrogen addition technology and the two-phase hydrogenation technique of conventional gas-phase being circulated combines, according to respective advantage, and processing different material.Two-phase hydrogenation dress eliminates High Temperature High Pressure hot oiling system and molten hydrogen system, and two covering devices can share a set of fractionating system, reduce investment outlay and process cost.
2, the dissolved hydrogen in high pressure hot separator oil phase in gas phase circulation hydrogenation unit is taken full advantage of, after two-phase hydrogenation device reaction, the hydrogen primitive reaction consumption of dissolving in oil phase is clean, the useless hydrogen amount of discharging from reaction product light pressure separator reduces greatly, reduce the hydrogen consumption of a whole set of combination process, reduce the scale of after-treatment device, reduce running cost.
3, relative to two-phase hydrogenation device, the liquid phase in conventional gas-phase circulation hydrogenation unit high pressure hot separator is hydrogen hypersaturated state, can provide more reaction hydrogen for two-phase hydrogen device, improves the impurity removal percentage of raw material.
4, in conventional gas-phase circulation hydrogenation unit high-pressure separator, owing to there is a large amount of hydrogen, the hydrogen sulfide major part in liquid phase can be carried discharge, less to the catalysts influence of two-phase hydrogenation reactor.And employing has in the two-phase hydrogenation technology of liquid phase circulation system, the hydrogen sulfide in turning oil is difficult to effective elimination, on deep hydrodesulfurizationof impact obviously.
Accompanying drawing explanation
Fig. 1 is a kind of schematic flow sheet combining distillate hydrogenation treatment process of the present invention.
Wherein: 1 is conventional gas-phase circulation hydrogenation unit reactor, 2 is conventional gas-phase circulation hydrogenation unit high pressure hot separator, 3 is conventional gas-phase circulation hydrogenation unit cold high pressure separator, 4 is two-phase hydrogenation device reaction device, 5 is fresh hydrogen, and 6 is conventional gas-phase circulation hydrogenation unit raw material, and 7 is two-phase hydrogenation device raw material, 8 is two-phase hydrogenation device reaction generation oil, and 9 is conventional gas-phase circulation hydrogenation unit cold high pressure separator liquid effluent phase materials.
Embodiment
For setting forth specific features of the present invention further, will be illustrated by reference to the accompanying drawings.
The intermediate oil of more difficult imurity-removal is adopted traditional mesohigh hydrogenation technique processing by the present invention, generation material and two-phase hydrogenation raw material together enter high pressure hot separator, fresh hydrogen fills into bottom high pressure hot separator, high pressure hot separator top portion enters cold high pressure separator from going out gas phase, and the blended liquid phase material that high pressure hot separator flows out directly enters two-phase hydrogenation reactor and reacts.The isolated gas phase of cold high pressure separator is as recycle hydrogen, and the isolated liquid phase of cold high pressure separator enters fractionating system.
By reference to the accompanying drawings 1, the present invention combines distillate hydrogenation treatment process process: conventional gas-phase circulation hydrogenation unit raw material 6(and high sulfur content distillate feedstock) and recycle hydrogen mixing after, enter conventional gas-phase circulation hydrogenation unit reactor 1, logistics and two-phase hydrogenation raw material 7(and low sulfur content distillate feedstock after hydrogenation) together enter conventional gas-phase circulation hydrogenation unit high pressure hot separator 2, fresh hydrogen 5 fills into bottom conventional gas-phase circulation hydrogenation unit high pressure hot separator 2, conventional gas-phase circulation hydrogenation unit high pressure hot separator 2 top portion enters conventional gas-phase circulation hydrogenation unit cold high pressure separator 3 from going out gas phase, the following feeding manner of blended liquid phase material that conventional gas-phase circulation hydrogenation unit high pressure hot separator 2 flows out directly enters two-phase hydrogenation reactor 4 and reacts.The isolated gas phase of conventional gas-phase circulation hydrogenation unit cold high pressure separator 3 is as recycle hydrogen, and the isolated liquid phase 9 of conventional gas-phase circulation hydrogenation unit cold high pressure separator 3 enters fractionating system.Two-phase hydrogenation reaction generates oil 8 and is discharged by two-phase hydrogenation reactor 4 top.
For further illustrating the solution of the present invention and effect, enumerate following examples:
Embodiment 1
The present embodiment is a kind of embodiment of combination distillate hydrogenation treatment process, and operating process schematic diagram is with reference to accompanying drawing 1.
After conventional gas-phase circulation hydrogenation unit raw material 6 and recycle hydrogen mix, enter conventional gas-phase circulation hydrogenation unit reactor 1, after hydrogenation, logistics and two-phase hydrogenation raw material 7 together enter high pressure hot separator, fresh hydrogen 5 fills into bottom high pressure hot separator, high pressure hot separator top portion enters cold high pressure separator from going out gas phase, and the following feeding manner of blended liquid phase material that high pressure hot separator flows out directly enters two-phase hydrogenation reactor 4 and reacts.The isolated gas phase of cold high pressure separator is as recycle hydrogen, and the isolated liquid phase 9 of cold high pressure separator enters fractionating system.Two-phase hydrogenation reaction generates oil 8 and is discharged by two-phase hydrogenation reactor 4 top.
Test uses feedstock property in table 1.Tradition hydrogenator and two-phase hydrogenation reactor adopt identical catalyzer, and catalyst property is in table 2.Conventional gas-phase circulation hydrogenation unit, two-phase hydrogenation device reaction condition and generation oil nature are in table 3.
Comparative example
The raw material of two-phase hydrogenation device, with the charging of embodiment two-phase hydrogenation device, adopts the operating method of id reaction product circulation.
Table 1 stock oil character
| Oil property | Conventional gas-phase circulation hydrogenation unit raw material | Two-phase hydrogenation device raw material |
| Density (20 DEG C)/gcm -3 | 0.8554 | 0.8378 |
| Boiling range scope/DEG C | 170～372 | 159～346 |
| Sulphur/μ gg -1 | 9746 | 5728 |
| Nitrogen/μ gg -1 | 366 | 129 |
Table 2 catalyzer physico-chemical property
| Project | Data |
| Catalyst activity component | Mo、Ni、W |
| Active component content (in oxide weight), % | 29 |
| Carrier | Aluminum oxide |
| Shape | Trifolium |
| Diameter | 3.1 |
| Pore volume/mLg -1 | 0.41 |
| Specific surface area/m2g -1 | 235 |
Table 3 hydrofining technology condition
| Processing condition | Tradition hydrogenation unit | Two-phase hydrogenation device | Comparative example |
| Reaction pressure/MPa | 6.5 | 4.0 | 4.0 |
| Temperature of reaction/DEG C | 360 | 360 | 360 |
| Two-phase hydrogenation charge ratio | 2:1* | 2:1** | |
| Hydrogen to oil volume ratio | 550:1 | ||
| Volume space velocity/h -1(relative fresh feed) | 1.5 | 1.5 | 1.5 |
| Generate oil nature: | |||
| S，μg/g | 4.9 | 457.5 | |
| N，μg/g | 2.2 | 35.7 | |
| Boiling range scope, DEG C | 150～364 | 150～342 |
* conventional gas-phase circulation hydrogen addition technology reaction effluent enters the volume ratio of the liquid phase material/two-phase hydrogenation device fresh feed of two-phase hydrogenation device through high pressure hot separator.* two-phase hydrogenation reactor discharges the volume ratio of liquid phase internal circulating load and the fresh feed of two-phase hydrogenation device.
Claims (16)
1. combine a distillate hydrogenation treatment process, it is characterized in that comprising the following steps:
A) distillate feedstock is divided into high-sulfur distillate feedstock and low-sulfur distillate feedstock by sulphur content, high sulfur content distillate feedstock adopts conventional gas-phase circulation hydrogen addition technology to process, material after the process of conventional gas-phase circulation hydrogen addition technology and two-phase hydrogenation low-sulfur distillate feedstock are mixed into high pressure hot separator, isolated gas phase enters cold high pressure separator, and the blended liquid phase material that high pressure hot separator flows out enters two-phase hydrogenation reactor and reacts; The isolated gas phase of cold high pressure separator recycles as recycle hydrogen, and the isolated oil phase of cold high pressure separator enters fractionating system; Fresh hydrogen fills into by bottom high pressure hot separator; Described high-sulfur distillate feedstock and the sulphur content of low-sulfur distillate feedstock divide by arbitrary value in 1000 ~ 12000 μ g/g;
B) two-phase hydrogenation device cancels turning oil system, material after low-sulfur distillate feedstock and the process of conventional gas-phase circulation hydrogen addition technology is mixed and after molten hydrogen at high pressure hot separator, enter two-phase hydrogenation reactor, reclaim hydrogenation after cut oil production from two-phase hydrogenation reactor reaction effluent.
2. method according to claim 1, it is characterized in that: step a) described in high-sulfur distillate feedstock and low-sulfur distillate feedstock sulphur content by 2000 ~ 8500 μ g/g arbitrary value divide, higher than divide value is high-sulfur distillate feedstock, and lower than divide value is low-sulfur distillate feedstock.
3. method according to claim 1 and 2, is characterized in that: high-sulfur distillate feedstock comes from secondary processing distillate, and low-sulfur distillate feedstock is the straight run oil that crude distillation obtains.
4. method according to claim 3, is characterized in that: high-sulfur distillate feedstock and low-sulfur distillate feedstock are one or more in kerosene(oil)fraction, diesel oil distillate, reduced pressure distillate oil distillate.
5. method according to claim 4, is characterized in that: the boiling range scope of high-sulfur distillate feedstock and low-sulfur distillate feedstock is within the scope of 130 ~ 450 DEG C.
6. method according to claim 4, is characterized in that: the boiling range scope of high-sulfur distillate feedstock and low-sulfur distillate feedstock is within the scope of 200 ~ 380 DEG C.
7. method according to claim 1, is characterized in that: step a) described conventional gas-phase circulation hydrogen addition technology operational condition is: temperature of reaction 200 ~ 400 DEG C; Reaction pressure 2.5 ~ 10.0MPa; Hydrogen to oil volume ratio 50:1 ~ 1000:1; Volume space velocity 0.6 ~ 5.0h
-1.
8. method according to claim 7, is characterized in that: step a) described conventional gas-phase circulation hydrogen addition technology operational condition is: temperature of reaction 260 ~ 380 DEG C; Reaction pressure 4.0 ~ 8.0MPa; Hydrogen to oil volume ratio 300:1 ~ 800:1; Volume space velocity 1.0 ~ 2.5h
-1.
9. method according to claim 7, is characterized in that: conventional gas-phase circulation hydrogen addition technology reaction pressure is higher than the reaction pressure 1 ~ 4MPa of two-phase hydrogenation device.
10. method according to claim 1, is characterized in that: step a) described conventional gas-phase circulation hydrogen addition technology adopts trickle-bed reactor, ebullated bed reactor, expanded bed reactor, or adverse current bed bioreactor.
11. methods according to claim 1, it is characterized in that: step a) in the service temperature of high pressure hot separator identical with conventional gas-phase circulation hydrogenator temperature out, or identical lower than conventional gas-phase circulation hydrogenator temperature out, and higher than 200 DEG C; The service temperature of cold high pressure separator is 40 ~ 80 DEG C.
12. methods according to claim 1, is characterized in that: high pressure hot separator is identical with the pressure of conventional gas-phase circulation hydrogenator with the working pressure of cold high pressure separator.
13. methods according to claim 1, is characterized in that: high pressure hot separator bottom arranges filler or gas-liquid distributor, to increase the contact of hydrogen and oil phase.
14. methods according to claim 1, is characterized in that: step b) described two-phase hydrogenation device reaction device charging adopts the operating method of upper feeding bottom discharge, or adopts the operating method of lower charging top discharge; Step b) described two-phase hydrogenation device operational condition is: temperature of reaction 200 ~ 400 DEG C; Reaction pressure 1.5 ~ 8.0MPa; Volume space velocity 0.6 ~ 5.0h
-1; Conventional gas-phase circulation hydrogen addition technology reaction effluent is 0.5:1 ~ 4.0:1 through the volumetric mixture ratio of liquid phase material and low-sulfur distillate feedstock that high pressure hot separator enters two-phase hydrogenation device.
15. methods according to claim 14, is characterized in that: step b) described two-phase hydrogenation device operational condition is: temperature of reaction 260 ~ 380 DEG C; Reaction pressure 2.0 ~ 6.0MPa; Volume space velocity 1.0 ~ 2.5h
-1; Conventional gas-phase circulation hydrogen addition technology reaction effluent is 1.0:1 ~ 3.0:1 through the volumetric mixture ratio of liquid phase material and low-sulfur distillate feedstock that high pressure hot separator enters two-phase hydrogenation device.
16. methods according to claim 1, it is characterized in that: the hydrotreating catalyst that the catalyzer that step (a) conventional gas-phase circulation hydrogen addition technology and the process of step (b) two-phase hydrogenation use is this area routine, wherein the active metal component of catalyzer be nickel, cobalt, molybdenum or tungsten one or more, catalyzer carries out sulfidizing before use, and active metal component is converted into sulphided state; Catalyzer composition comprises by weight percentage: nickel or cobalt are calculated as 0.5% ~ 10% by its oxide compound, and molybdenum or tungsten are calculated as 1% ~ 25% by its oxide compound, and carrier is aluminum oxide, silicon oxide, aluminium oxide-silicon oxide, one or more in titanium oxide.
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