CN102690684B - Petroleum wide distillate oil two-section hydrogenation treatment technology - Google Patents
Petroleum wide distillate oil two-section hydrogenation treatment technology Download PDFInfo
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Abstract
The invention relates to a petroleum wide distillate oil two-section hydrogenation treatment technology, which comprises the following steps of: (1) hydrofining petroleum in a circulating way; (2) fractionating petroleum products; (3) carrying out hydrogen circulatory hydrogenation and modification, wherein reaction products generated by the step of hydrofining petroleum in a circulating way enter into the step of fractionating petroleum products, and are separated into various products fractions and hydrogenated tail petroleum, some diesel oil fractions and some hydrogenated tail petroleum enter into the step of hydrogen circulatory hydrogenation and modification, so as to have the reaction of hydrogenation and modification, the reaction products return to the step of fractionating petroleum products to be separated, the step (1) is the process of desulfuration, denitrification and aromatics saturation of the petroleum products, and the step (3) is the process of hydrocracking, modifying and pour point reducing of the petroleum products. The technology has the advantages of being good in product selectivity, high in hydrogenation depth, and small in energy consumption. The technology is applicable to the technical field of petrochemical engineering.
Description
Technical field
The invention belongs to technical field of petrochemical industry, relate to a kind of hydroprocessing technique, especially relate to a kind of oil wide fraction oil two-stage hydrogenation treatment process.
Background technology
Environmental regulation increasingly stringent, sulfur content in oil products and aromaticity content standard are revised year by year.Europe III emission standard requires that petrol and diesel oil sulphur content is less than 350 μ g/g, and Europe IV emission standard requires that petrol and diesel oil sulphur content is less than 50 μ g/g.Improving constantly of oil quality standard proposes severe challenge to oil-processing enterprises.Hydrogen addition technology is the Main Means that oil refining enterprise improves quality product.Along with oil product cleans the raising of requirement, hydrogen addition technology is more and more important.Existing hydrogen addition technology can be divided into trickle bed hydrogenation technique and liquid phase bed hydroprocessing technique.
Trickle bed hydroprocessing technique is in hydrogenator, and gas, liquid, solid three-phase is also deposited, and gas phase is external phase, is the steam of hydrogen and hydrocarbon raw material, and liquid phase is the hydrocarbon raw material do not gasified, and solid phase is catalyzer.Gas-liquid two-phase passes through beds in the mode of drip.In order to control the temperature of reaction of beds and avoid catalyst deactivation, usually adopt larger hydrogen-oil ratio, hydrogen more than needed after reaction, after circulating hydrogen compressor supercharging, recycles.
Liquid phase bed hydroprocessing treatment process is that a part for liquid product is looped back reactor, relies on liquid product a large amount of circulation time to carry dissolved hydrogen into reactive system to provide the hydrogen required for reaction, takes away reaction heat simultaneously.The amounts of hydrogen used is for being a bit larger tham chemical hydrogen consumption and system dissolves hydrogen amount sum, and whole process does not need to arrange hydrogen gas circulating system.
A kind of hydrofining technology of reformed oil disclosed in CN86108022, a kind of inferior feedstock oil a period of hydrocracking processing method disclosed in CN93101935, a kind of method of serial hydrogenation explained hereafter high-quality vaseline disclosed in a kind of Rifining method for catalylic cracking gasoline by adding hydrogen disclosed in CN94102955 and CN96109792, it is all trickle bed hydroprocessing technique, adopt larger hydrogen-oil ratio, hydrogen-oil ratio is not from 300: 1 ~ 1500: 1 etc.
CN101338220A discloses a kind of hydrogenation method for hydrocarbon oils, it is liquid phase bed hydroprocessing treatment process, hydrogen is mixed to form mixture flow with a part for fresh feed oil and turning oil under the existence of hydrogen solvent or thinner, and mixture flow enters reactor and catalyst exposure.Another part turning oil mixes with hydrogen, between reactor bed, enter reactor, regulates the olefin hydrogen in reactor.Reaction effluent carries out gas-liquid separation, and liquid phase isolates hydrogen solvent further or thinner recycles, and isolated product liquid part is as product, and part is as turning oil.
US6123835, US6428686 etc. disclose a kind of hydrogenation technique of molten hydrogen in advance, belong to liquid phase bed hydroprocessing treatment process.Hydrogen mixes with stock oil and thinner (product of hydrotreatment) and/or after flash distillation, enters catalyst bed reaction, and the hydrogen needed for reaction is provided by dissolved hydrogen.By product circulation, regulate the hydrogen amount of the system that enters.
CN 101942327A discloses a kind of hydrotreatment combined technical method producing ultra-low-sulphur diesel.The method comprises liquid phase bed hydroprocessing processing unit and trickle bed hydrotreating unit, divides two sections and carries out hydrotreatment to solar oil.
Along with the development of society, market gets more and more to high-quality light-end products demand, and the demand of variant production along with the key element and changing such as market and season, can make the target variation of hydrogenation technique, simple hydrofining or hydro-upgrading, be difficult to the demand meeting market.
And, oil-processing enterprises hydrogenation technique needs raw material variety to be processed to get more and more, the raw material boiling range faced is more and more wider, and current hydrogenation technique can only process the raw material of narrow fraction, do not consider the process of wide fraction raw material, though as CN 101942327A considers two sections of combinations, do not consider the process of intermediates during wide fraction process, adaptability to raw material is poor.Therefore for adapting to product requirement, need the hydrotreatment facility building different fractions scope, enterprise investment is increased, and hydrogen gas consumption is large.
Summary of the invention
The object of the invention is the above-mentioned deficiency overcome existing for prior art, and provide one can adapt to oil wide fraction oil raw material, product selectivity is good, product slates can adjust flexibly with season and the market requirement, hydrogenation depth is high, hydrogen and heat integration are reasonable, the oil wide fraction oil two-stage hydrogenation treatment process that the comprehensive method of investment is few, and its technical scheme is:
A kind of oil wide fraction oil two-stage hydrogenation treatment process, comprises 1) oil circulation hydrofining; 2) oil product fractionation; 3) hydrogen recycle hydro-upgrading three steps, the reaction product generating oil circulation hydrofining step enters oil product fractionating step, be separated into various product cut and hydrogenation tail oil, wherein part diesel oil distillate and partial hydrogenation tail oil enter hydrogen recycle hydro-upgrading step, carry out hydro-upgrading reaction, reaction product returns oil product fractionating step and carries out product separation, described step 1) be the desulfurization of oil product, denitrogenation and aromatics saturation process, described step 3) be the hydrocracking of oil product, upgrading and pour point depression process.
Step 1) refer to a part of liquid product is looped back reactor, liquid product a large amount of circulation time is relied on to carry dissolved hydrogen into reactive system to provide the hydrogen required for reaction, take away reaction heat simultaneously, internal circulating load adjusts according to feedstock property and product summary, and this unit process does not need to arrange hydrogen gas circulating system.Reactor feed temperature is controlled by turning oil, the temperature that the reaction heat utilizing turning oil to carry makes reaction mass reach required, and does not need additionally to heat reaction mass.Step 1) comprise thermal high and cold anticyclone two-stage oil and gas separating system and gas sweetening systems, after refining reaction, oil gas is separated.Gas, by after desulphurization system, can be used as High Pressure Hydrogen and supplements to step 3), reduce the pressure energy consumption of hydrogen-feeding system.By desulphurization system, oil hydrogenation is made to refine the H of generation
2s and NH
3timely release, reduces sulphur, nitride to the suppression of catalyst activity.
Described step 3) refer to and adopt the form of hydrogen recycle, control the temperature of reaction bed, for system hydrogen supply with slow down catalyst deactivation rate.The hydrogen-oil ratio that usual employing is larger, hydrogen more than needed after reaction, after circulating hydrogen compressor supercharging, recycles.Reaction consumption hydrogen is provided by liquid phase dissolved hydrogen, and liquid phase dissolved hydrogen is provided by gas phase hydrogen.Step 3) do not need desulphurization of recycle hydrogen system.
Further preferably, described step 1) middle employing mixed phase bed reactor, reaction consumption hydrogen is provided by liquid phase dissolved hydrogen, and stock oil directly enters reactor bed after mixing with turning oil and hydrogen, and hydrogen is scattered among liquid phase with dissolved hydrogen and gas phase microvesicle form.Catalytic solid, fluid phase and hydrogen gas phase is there is in reactor bed.
Further preferably, described step 1) and step 3) product share product separation column, by separation column, selection is carried out to raw material.
Further preferably, described step 2) middle increase steam stripped.
Further preferably, described step 3) middle employing trickle-bed reactor, in reactor bed, gas, liquid, solid three-phase is also deposited, gas phase is circulation hydrogen-rich gas, liquid phase is step 2) isolated last running oil product, solid phase is catalyzer, and liquid together passes through beds with trickle flow and gas phase.
Further preferably, described step 3) comprise cold anticyclone and cold low two-stage oil and gas separating system and hydrogen gas circulating system, oil and gas separating system comprises rich hydrocarbon gas releasing device.
Further preferably, described step 1) in the ratio of turning oil and stock oil be 1: 1 ~ 10: 1.
Further preferably, described step 1) in temperature of reaction be 250 ~ 400 DEG C, reaction pressure is 2.0 ~ 20MPa, and volume space velocity is 0.5 ~ 2.0h
-1.
Further preferably, described step 3) in temperature of reaction be generally 250 ~ 450 DEG C, reaction pressure is 2.0 ~ 20MPa, and volume space velocity is 0.5 ~ 2.0h
-1, hydrogen to oil volume ratio is 300: 1 ~ 1500: 1.
Oil wide fraction oil two-stage hydrogenation treatment process of the present invention, is applicable to the process of oil wide fraction oil raw material, can processes the oil product that boiling range scope is 50 DEG C ~ 570 DEG C.
Beneficial effect of the present invention:
1, oil wide fraction oil two-stage hydrogenation treatment process steps 2 of the present invention) in, increase steam stripped, sulphur, nitrogen compound that more effective removal product liquid carries, reduce sulphur, nitrogen compound to the impact of catalyst for hydro-upgrading.
2, oil wide fraction oil two-stage hydrogenation treatment process of the present invention, device degree of integration is high, does not need pre-separation unit, invests little, and can reduce investment outlay 30%-40%.
3, oil wide fraction oil two-stage hydrogenation treatment process hydrogen of the present invention, be applicable to the process of oil wide fraction oil product, adaptability to raw material strong (cuts that boiling range is 50 DEG C ~ 570 DEG C), can according to market requirement flexible hydrogenated products, hydrogenation depth is high, product sulphur content is less than 50 μ g/g, and rationally, energy consumption is little for hydrogen and heat integration.
Accompanying drawing explanation
Fig. 1 is for being oil wide fraction of the present invention oil two-stage hydrogenation processing technological flow figure.
Embodiment
Below in conjunction with concrete and embodiment, method of the present invention is described in more detail.Embodiments of the invention are not limited thereto, and raw material can be boiling range scope the be oil product of 50 DEG C ~ 570 DEG C, includes but not limited to raw naphtha, gas oil, wax oil, lubricating oil distillate and their mixed fraction.Hydrobon catalyst and catalyst for hydro-upgrading can select commercial catalyst, also can prepare according to prior art.
A kind of oil wide fraction oil of the present invention two-stage hydrogenation treatment process, for step 1) chemical hydrogen consumption of reaction process and stock oil and turning oil saturated hydrogen amount at reaction conditions can by measurings, can be estimated by empirical value, also can rule of thumb formulae discovery." hydroprocessing technique and engineering " that empirical value and experimental formula can be published with reference to Sinopec press for 2004.Hydrogen usage is generally 1 ~ 80 times of system dissolves hydrogen amount under reaction conditions.
With reference to Fig. 1, after stock oil 41 mixes with hydrogen 44, by interchanger 32 and hydro-upgrading resultant 61 heat exchange, then after mixing with turning oil 42, enter step 1) reactor 11, carries out hydrofining reaction.Hydrofining resultant is divided into two portions, and a part is as turning oil 42 Returning reactor, and a part enters gas-liquid separator 12 and carries out gas-liquid separation.Gas-liquid separator 12 hydrogen-rich gas 43 out enters gas sweetening tower 13, after removing hydrogen sulfide and ammonia, purified gas enters hydrogen gas compressor 14 after mixing with fresh hydrogen 40, and boosting rear portion returns step 1) reactor reuses, a part goes step 3) reactor.After gas-liquid separator 12 hydrofining product liquid 45 out mixes with hydro-upgrading product liquid 66, enter separation column 21.Separation column 21 with reboiler, and is provided with stripped vapor 54.After separation column 21 fractionation, hydrogenation products is divided into non-condensable gas 51, petroleum naphtha 52, diesel oil 53 and hydrogenation tail oil.Part or all of diesel oil distillate and hydrogenation tail oil goes out device as product 53 and 55, and another part is as hydro-upgrading raw material 56.After hydro-upgrading raw material 56 mixes with recycle hydrogen 70, heat through process furnace 36, then enter step 3) reactor 31, carry out hydro-upgrading reaction, hydro-upgrading resultant 61, by after interchanger 32 and the heat exchange of hydrofining raw material, enters high-pressure gas-liquid separator 33, carries out high-pressure gas-liquid separation.High score gas 62 part is as high pressure release gas 64 discharger, and another part, after circulating hydrogen compressor 34 boosts, mixes with the High Pressure Hydrogen of hydrogen gas compressor 14, reuses as recycle hydrogen 70.High score liquid 63 enters low-pressure gas-liquid separator 35, carries out low-pressure gas-liquid separation, isolates non-condensable gas further.Low-pressure gas-liquid separator 35 noncondensable gas out removes subsequent technique as low pressure release gas 65.Low-pressure gas-liquid separator 35 liquid is out hydro-upgrading product liquid 66, after mixing, enters separation column 21, be separated into various product cut with hydrofining product liquid 45.
Embodiment
By the operating process of Fig. 1, step 1) adopt commodity catalyst for refining, step 3) and adopt commodity modifying catalyst, take mixing oil as raw material.The result of gained is as follows:
The composition of table 1 catalyzer and quality index
| Catalyst type | Finishing agent | Modification agent |
| Physical properties: | ||
| Shape | Trifolium | Cylinder |
| Particle diameter, mm | 1.1～1.3 | 1.45～1.65 |
| Length, mm | 3～8 | 3～8 |
| Recommend packing density, g/cm 3 | 0.82～0.9 | 0.80～0.90 |
| Intensity, N/mm | ≥14 | ＞18.5 |
| Chemical constitution, m% | Mo-Ni-P | W-Ni |
| MoO 3 | 22.5～25.5 | |
| NiO | 3.3～3.8 | 5.2～6.4 |
| WO 3 | 20.0～24.0 |
Table 2 stock oil character
| Oil property | Raw material (mixing oil) |
| Density (20 DEG C), g/cm 3 | 0.9 |
| Boiling range (ASTM D-1160), DEG C | |
| Initial boiling point | 120 |
| 50％ | 280 |
| 90％ | 400 |
| Do | 550 |
| Sulphur, μ g/g | 12400 |
| Nitrogen, μ g/g | 985 |
Table 3 processing condition
| Processing condition | Step 1) | Step 3) |
| Temperature of reaction, DEG C | 320-360 | 350-400 |
| Reaction pressure, MPa | 10-18 | 7-15 |
| Cumulative volume air speed, h -1 | 6-8 | 1-3 |
| Oil circulation than (V/V) | 3-5 | - |
| Hydrogen-oil ratio (V/V) | - | 300-1000 |
Table 4 product property
Comparative example
According to the operational condition of embodiment, but the step 2 removed in embodiment), and in step 1) increase knockout drum before mixed phase bed reactor inlet, remove the gas phase hydrogen in charging, make mixed phase bed reactor change common two-phase reactor into, acquired results is as follows:
Table 5 comparative example product property
Comparative example and comparative example can be found out, by adopting a kind of oil wide fraction oil of the present invention two-stage hydrogenation treatment process, adding the selectivity of object product, improve the refining depth of product.
Claims (1)
1. an oil wide fraction oil two-stage hydrogenation treatment process, is characterized in that, comprise 1) oil circulation hydrofining; 2) oil product fractionation; 3) hydrogen recycle hydro-upgrading three steps, the reaction product of oil circulation hydrofining step enters oil product fractionating step, be separated into various product cut and hydrogenation tail oil, wherein part diesel oil distillate and partial hydrogenation tail oil enter hydrogen recycle hydro-upgrading step, carry out hydro-upgrading reaction, reaction product returns oil product fractionating step and carries out product separation, described step 1) be the desulfurization of oil product, denitrogenation and aromatics saturation process, described step 3) be the hydrocracking of oil product, upgrading and pour point depression process;
Described step 1) middle employing mixed phase bed reactor, reaction consumption hydrogen is provided by liquid phase dissolved hydrogen, after stock oil mixes with turning oil and hydrogen, directly enter reactor bed, hydrogen is scattered among liquid phase with dissolved hydrogen and gas phase microvesicle form, there is catalytic solid, fluid phase and hydrogen gas phase in reactor bed;
After stock oil mixes with hydrogen, by interchanger and the heat exchange of hydro-upgrading resultant, then after mixing with turning oil, enter step 1) reactor, carries out hydrofining reaction; Hydrofining resultant is divided into two portions, and a part is as turning oil Returning reactor, and a part enters gas-liquid separator and carries out gas-liquid separation; Gas-liquid separator hydrogen-rich gas out enters gas sweetening tower, after removing hydrogen sulfide and ammonia, enter hydrogen gas compressor after purified gas mixes with fresh hydrogen, boosting rear portion returns step 1) reactor reuses, a part goes step 3) reactor; After gas-liquid separator hydrofining product liquid out mixes with hydro-upgrading product liquid, enter separation column; Separation column with reboiler, and is provided with stripped vapor; After separation column fractionation, hydrogenation products is divided into non-condensable gas, petroleum naphtha, diesel oil and hydrogenation tail oil; A part for diesel oil distillate and hydrogenation tail oil goes out device as product, and another part is as hydro-upgrading raw material; After hydro-upgrading raw material mixes with recycle hydrogen, through process furnace heating, then enter step 3) reactor, carry out hydro-upgrading reaction, hydro-upgrading resultant, by after interchanger and the heat exchange of hydrofining raw material, enters high-pressure gas-liquid separator, carries out high-pressure gas-liquid separation; A high score gas part is as high pressure release gas discharger, and another part is after circulating hydrogen compressor boosting, and the High Pressure Hydrogen come with hydrogen gas compressor mixes, and reuses as recycle hydrogen; High score liquid enters low-pressure gas-liquid separator, carries out low-pressure gas-liquid separation, isolates non-condensable gas further; Low-pressure gas-liquid separator noncondensable gas out removes subsequent technique as low pressure release gas; Low-pressure gas-liquid separator liquid is out hydro-upgrading product liquid, after mixing, enters separation column with hydrofining product liquid, is separated into various product cut;
Described step 1) and step 3) product share product separation column, by separation column to raw material carry out selection regulation and control;
Described step 2) middle increase steam stripped;
Described step 3) middle employing trickle-bed reactor, in reactor bed, gas, liquid, solid three-phase is also deposited, gas phase is circulation hydrogen-rich gas, liquid phase is step 2) isolated diesel oil distillate and hydrogenation tail oil, solid phase is catalyzer, and liquid phase together passes through beds with trickle flow and gas phase;
Described step 1) in the ratio of turning oil and stock oil be 1: 1 ~ 10: 1;
Described step 1) in temperature of reaction be 250 ~ 400 DEG C, reaction pressure is 2.0 ~ 20MPa, and volume space velocity is 0.5 ~ 2.0h
-1;
Described step 3) in temperature of reaction be generally 250 ~ 450 DEG C, reaction pressure is 2.0 ~ 20MPa, and volume space velocity is 0.5 ~ 2.0h
-1, hydrogen to oil volume ratio is 300: 1 ~ 1500: 1;
Be applicable to the process of oil wide fraction oil raw material, the oil product that boiling range scope is 50 DEG C ~ 570 DEG C can be processed.
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| CN1600840A (en) * | 2003-09-28 | 2005-03-30 | 中国石油化工股份有限公司 | Method of mild hydrocracking raw material heavy oil |
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