CN102690684A - 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 the petrochemical technology field, relate to a kind of hydroprocessing technique, especially relate to a kind of oil wide fraction oil two-stage hydrogenation treatment process.
Background technology
The environmental regulation increasingly stringent, sulfur content in oil products and aromaticity content standard are revised year by year.Europe III emission standard requires the petrol and diesel oil sulphur content less than 350 μ g/g, and Europe IV emission standard requires the petrol and diesel oil sulphur content less than 50 μ g/g.Improving constantly of oil quality standard proposed severe challenge to refining of petroleum enterprise.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 technology.
The trickle bed hydroprocessing technique is in hydrogenator, and the gas, liquid, solid three-phase is also deposited, and gas phase is an external phase, is the steam of hydrogen and hydrocarbon raw material, and liquid phase is the hydrocarbon raw material that does not gasify, and solid phase is a catalyzer.Gas-liquid two-phase passes through beds with the mode of drip.For the temperature of reaction of control catalyst bed with avoid catalyst deactivation, adopt bigger hydrogen-oil ratio usually, reaction back hydrogen more than needed recycles after the circulating hydrogen compressor supercharging.
Liquid phase bed hydroprocessing treatment process is to loop back reactor drum to the part of liquid product, and the dissolved hydrogen of reactive system provides reaction needed hydrogen to rely on a large amount of circulation times of liquid product to carry into, takes away reaction heat simultaneously.The amounts of hydrogen of using is for being a bit larger tham chemical hydrogen consumption and system dissolves hydrogen amount sum, and whole process need not be provided with hydrogen gas circulating system.
The hydrogen refining process of the disclosed a kind of reformed oil of CN86108022; The disclosed a kind of inferior feedstock oil a period of hydrocracking process method of CN93101935; The method of disclosed a kind of Rifining method for catalylic cracking gasoline by adding hydrogen of CN94102955 and the disclosed a kind of serial hydrogenation explained hereafter high-quality vaseline of CN96109792; All be the trickle bed hydroprocessing technique, adopt big hydrogen-oil ratio, hydrogen-oil ratio did not wait from 300: 1～1500: 1.
CN101338220A discloses a kind of hydrogenation method for hydrocarbon oils; It is liquid phase bed hydroprocessing treatment process; Hydrogen mixes the formation mixture flow with the part of fresh feed oil and turning oil in the presence of hydrogen solvent or thinner, mixture flow gets into reactor drum and contacts with catalyzer.Another part turning oil mixes with hydrogen, gets into reactor drum between the reactor bed, and the hydrogen in the conditioned reaction device distributes.Reaction effluent carries out gas-liquid separation, and liquid phase is further isolated the hydrogen solvent 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 that dissolves hydrogen in advance, belong to liquid phase bed hydroprocessing treatment process.Hydrogen mix with raw oil and thinner (product of hydrotreatment) and/or flash distillation after, get into catalyst bed reaction, reacting required hydrogen is provided by dissolved hydrogen.Through the product circulation, regulate the hydrogen amount of entering system.
CN 101942327A has announced a kind of hydrotreatment combined technical method of producing ultra-low-sulphur diesel.This method comprises liquid phase bed hydroprocessing processing unit and trickle bed hydrotreatment unit, divides two sections solar oil carried out hydrotreatment.
Development along with society; Market is more and more to high-quality clean cargo demand, and the demand of variant prodn can make that the target of hydrogenation technique is diversified along with key element and changing such as market and season; Simple unifining or hydro-upgrading have been difficult to satisfy the demand in market.
And; The raw material variety that refining of petroleum enterprise hydrogenation technique need be handled is more and more, and the raw material boiling range that faces is more and more wideer, and current hydrogenation technique can only be handled the raw material of narrow fraction; Do not consider the processing of wide fraction raw material; Though considered two sections combinations like CN 101942327A, do not consider the processing of intermediates when wide fraction is handled, adaptability to raw material is poor.Therefore for adapting to product requirement, need to build the hydrotreatment facility of different fractions scope, make enterprise investment increase, hydrogen gas consumption is big.
Summary of the invention
The objective of the invention is to overcome the above-mentioned deficiency of existing in prior technology; And a kind of oil wide fraction oil raw material that can adapt to is provided, and product selectivity is good, and product distributes and can adjust flexibly with the season and the market requirement; The hydrogenation degree of 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 unifining; 2) oil product fractionation; 3) three steps of hydrogen recycle hydro-upgrading; The reaction product that generates oil circulation unifining step gets into the oil product fractionating step; Be separated into various product cuts and hydrogenation tail oil; Wherein part diesel oil distillate and partial hydrogenation tail oil get into hydrogen recycle hydro-upgrading step, carry out the hydro-upgrading reaction, and reaction product is returned the oil product fractionating step and carried out product separation; Said step 1) is desulfurization, denitrogenation and the aromatics saturation process of oil product, and said step 3) is hydrogen cracking, upgrading and the pour point depression process of oil product.
Step 1) is meant and loops back reactor drum to a part of liquid product; The dissolved hydrogen of reactive system provides reaction needed hydrogen to rely on a large amount of circulation times of liquid product to carry into; Take away reaction heat simultaneously; Internal circulating load is adjusted according to feedstock property and product summary, and this unit process need not be provided with hydrogen gas circulating system.The reactor feed temperature is controlled by turning oil, and the reaction heat that utilizes turning oil to carry makes reaction mass reach required temperature, and does not need extra reaction mass to be heated.Step 1) comprises thermal high and cold anticyclone two-stage oil and gas separating system and gas sweetening system, and behind the refining reaction, oil gas separates.Gas can be used as High Pressure Hydrogen and replenishes to step 3) through after the desulphurization system, reduces the pressure energy consumption of hydrogen-feeding system.Through desulphurization system, make the refining H that produces of oil hydrogenation
2S and NH
3In time discharge, reduce the inhibition of sulphur, nitride catalyst activity.
Said step 3) is meant the form that adopts hydrogen recycle, the temperature of control reaction bed, for system's hydrogen supply with slow down catalyst deactivation rate.Usually adopt bigger hydrogen-oil ratio, the hydrogen of having more than needed in the reaction back recycles after the circulating hydrogen compressor supercharging.Reaction consumption hydrogen is provided by liquid phase dissolved hydrogen, and liquid phase dissolved hydrogen is provided by gas phase hydrogen.Step 3) does not need the desulphurization of recycle hydrogen system.
Further preferred, adopt the mixed phase bed bioreactor in the said step 1), reaction consumption hydrogen is provided by liquid phase dissolved hydrogen, and raw oil directly gets into reactor bed with after turning oil and hydrogen mix, and hydrogen is scattered among the liquid phase with dissolved hydrogen and gas phase microvesicle form.There are catalyzer solid phase, fluid phase and hydrogen gas phase in the reactor bed.
Further preferred, the shared product separation column of the product of said step 1) and step 3) is selected regulation and control through separation column to raw material.
Further preferred, said step 2) the middle steam stripped that increases.
Further preferred, adopt trickle-bed reactor in the said step 3), in the reactor bed; The gas, liquid, solid three-phase is also deposited, and gas phase is the circulation hydrogen-rich gas, and liquid phase is a step 2) isolated last running oil product; Solid phase is a catalyzer, and liquid together passes through beds with drip mode and gas phase.
Further preferred, said step 3) comprises cold anticyclone and cold low two-stage oil and gas separating system and hydrogen gas circulating system, and oil and gas separating system comprises rich hydrocarbon gas tripping gear.
Further preferred, the ratio of turning oil and raw oil is 1: 1～10: 1 in the said step 1).
Further preferred, temperature of reaction is 250～400 ℃ in the said step 1), and reaction pressure is 2.0～20MPa, and volume space velocity is 0.5～2.0h
-1
Further preferred, temperature of reaction is generally 250～450 ℃ in the said step 3), and 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 of the present invention oil two-stage hydrogenation treatment process is fit to the processing of oil wide fraction oil raw material, can handle the boiling range scope and be 50 ℃～570 ℃ oil product.
Beneficial effect of the present invention:
1, oil wide fraction of the present invention oil two-stage hydrogenation treatment process steps 2) in, increasing steam stripped, sulphur, nitrogen compound that more effective removal product liquid carries reduce the influence to catalyst for hydro-upgrading of sulphur, nitrogen compound.
2, oil wide fraction of the present invention oil two-stage hydrogenation treatment process, the device degree of integration is high, does not need the pre-separation unit, invests for a short time, and 30%-40% can reduce investment outlay.
3, oil wide fraction oil two-stage hydrogenation treatment process hydrogen of the present invention; Be fit to the processing of oil wide fraction oil product, adaptability to raw material strong (cuts that boiling range is 50 ℃～570 ℃) can be according to market requirement flexible hydrogenated products; The hydrogenation degree of depth is high; The product sulphur content is less than 50 μ g/g, and hydrogen and heat integration are reasonable, and energy consumption is little.
Description of drawings
Fig. 1 is for being oil wide fraction oil two-stage hydrogenation processing technological flow figure of the present invention.
Embodiment
Below in conjunction with concrete and embodiment method of the present invention is done explanation in further detail.Embodiments of the invention are not limited thereto, and raw material can be that the boiling range scope is 50 ℃～570 ℃ a oil product, 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 be selected commercial catalyst, also can be according to prior art for preparing.
A kind of oil wide fraction of the present invention oil two-stage hydrogenation treatment process can be estimated by empirical value by measuring with the saturated hydrogen amount of turning oil under reaction conditions for the chemical hydrogen consumption and the raw oil of step 1) reaction process, also rule of thumb formula calculating.Empirical value and experimental formula can be with reference to " hydroprocessing technique and the engineerings " of Sinopec press publication in 2004.Hydrogen usage is generally 1～80 times of system dissolves hydrogen amount under the reaction conditions.
With reference to Fig. 1, raw oil 41 is with after hydrogen 44 mixes, and through interchanger 32 and 61 heat exchange of hydro-upgrading resultant, with after turning oil 42 mixes, entering step 1) reactor drum 11 carries out hydrofining reaction again.Unifining resultant separated into two parts, a part are as turning oil 42 Returning reactors, and a part gets into gas-liquid separator 12 and carries out gas-liquid separation.The hydrogen-rich gas 43 that gas-liquid separator 12 comes out gets into gas sweetening tower 13; After removing hydrogen sulfide and ammonia; Purified gas mixes the back and gets into hydrogen gas compressor 14 with fresh hydrogen 40, the back part of boosting is returned the step 1) reactor drum and reused, and a part is removed the step 3) reactor drum.The unifining product liquid 45 that gas-liquid separator 12 comes out gets into separation column 21 with after hydro-upgrading product liquid 66 mixes.Separation column 21 has 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.Diesel oil distillate and hydrogenation tail oil a part or all go out device as product 53 and 55, another part is as hydro-upgrading raw material 56.Hydro-upgrading raw material 56 through process furnace 36 heating, gets into step 3) reactor drum 31 with after recycle hydrogen 70 mixes then; Carry out the hydro-upgrading reaction; After hydro-upgrading resultant 61 passes through interchanger 32 and the heat exchange of unifining raw material, get into high-pressure gas-liquid separator 33, carry out high-pressure gas-liquid and separate.High score gas 62 parts discharge gas 64 dischargers as high pressure, and another part mixes with the High Pressure Hydrogen of hydrogen gas compressor 14 after circulating hydrogen compressor 34 boosts, and reuse as recycle hydrogen 70.High score liquid 63 gets into low-pressure gas-liquid separator 35, carries out low-pressure gas-liquid and separates, and further isolates non-condensable gas.The noncondensable gas that low-pressure gas-liquid separator 35 comes out discharges gas 65 as low pressure and removes subsequent technique.The liquid that low-pressure gas-liquid separator 35 comes out is hydro-upgrading product liquid 66, after unifining product liquid 45 mixes, gets into separation column 21, separates into various product cuts.
Embodiment
Press the operating process of Fig. 1, step 1) adopts the commodity catalyst for refining, and step 3) adopts the commodity modifying catalyst, is raw material with the mixing oil.The result of gained is following:
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 raw oil character
| Oil property | Raw material (mixing oil) |
| Density (20 ℃), g/cm 3 | 0.9 |
| Boiling range (ASTM D-1160), ℃ | |
| Over 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, ℃ | 320-360 | 350-400 |
| Reaction pressure, MPa | 10-18 | 7-15 |
| The TV 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 remove the step 2 among the embodiment), and before step 1) mixed phase bed bioreactor inlet, increase knockout drum, remove the gas phase hydrogen in the charging, make the mixed phase bed bioreactor change common two-phase reactor into, the gained result is following:
Table 5 comparative example product property
Comparative example and comparative example can be found out, through adopting a kind of oil wide fraction oil of the present invention two-stage hydrogenation treatment process, have increased the selectivity of purpose product, have improved the refining depth of product.
Claims (10)
1. an oil wide fraction oil two-stage hydrogenation treatment process is characterized in that, comprises 1) oil circulation unifining; 2) oil product fractionation; 3) three steps of hydrogen recycle hydro-upgrading; The reaction product that generates oil circulation unifining step gets into the oil product fractionating step; Be separated into various product cuts and hydrogenation tail oil; Wherein part diesel oil distillate and partial hydrogenation tail oil get into hydrogen recycle hydro-upgrading step, carry out the hydro-upgrading reaction, and reaction product is returned the oil product fractionating step and carried out product separation; Said step 1) is desulfurization, denitrogenation and the aromatics saturation process of oil product, and said step 3) is hydrogen cracking, upgrading and the pour point depression process of oil product.
2. oil wide fraction oil two-stage hydrogenation treatment process according to claim 1; It is characterized in that; Adopt the mixed phase bed bioreactor in the said step 1), reaction consumption hydrogen is provided by liquid phase dissolved hydrogen, and raw oil is with after turning oil and hydrogen mix; Directly get into reactor bed, hydrogen is scattered among the liquid phase with dissolved hydrogen and gas phase microvesicle form.There are catalyzer solid phase, fluid phase and hydrogen gas phase in the reactor bed.
3. oil wide fraction oil two-stage hydrogenation treatment process according to claim 1 is characterized in that the shared product separation column of the product of said step 1) and step 3) is selected regulation and control through separation column to raw material.
4. oil wide fraction oil two-stage hydrogenation treatment process according to claim 1 is characterized in that said step 2) the middle steam stripped that increases.
5. oil wide fraction oil two-stage hydrogenation treatment process according to claim 1 is characterized in that, adopts trickle-bed reactor in the said step 3); In the reactor bed; The gas, liquid, solid three-phase is also deposited, and gas phase is the circulation hydrogen-rich gas, and liquid phase is a step 2) isolated last running oil product; Solid phase is a catalyzer, and liquid together passes through beds with drip mode and gas phase.
6. oil wide fraction oil two-stage hydrogenation treatment process according to claim 1 is characterized in that said step 3) comprises cold anticyclone and cold low two-stage oil and gas separating system and hydrogen gas circulating system, and oil and gas separating system comprises rich hydrocarbon gas tripping gear.
7. oil wide fraction oil two-stage hydrogenation treatment process according to claim 1 is characterized in that the ratio of turning oil and raw oil is 1: 1～10: 1 in the said step 1).
8. oil wide fraction oil two-stage hydrogenation treatment process according to claim 1 is characterized in that temperature of reaction is 250～400 ℃ in the said step 1), and reaction pressure is 2.0～20MPa, and volume space velocity is 0.5～2.0h
-1
9. oil wide fraction oil two-stage hydrogenation treatment process according to claim 1 is characterized in that temperature of reaction is generally 250～450 ℃ in the said step 3), and 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.
10. according to each described oil wide fraction oil two-stage hydrogenation treatment process of claim 1-9, it is characterized in that, be fit to the processing of oil wide fraction oil raw material, can handle the boiling range scope and be 50 ℃～570 ℃ oil product.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07166176A (en) * | 1993-12-16 | 1995-06-27 | Nippon Oil Co Ltd | Production of low-sulfur gas oil |
| 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 |
| CN101117594A (en) * | 2006-07-31 | 2008-02-06 | 中国石油化工股份有限公司 | Hydrogenation method for producing clean diesel oil |
-
2011
- 2011-11-29 CN CN201110385561.4A patent/CN102690684B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07166176A (en) * | 1993-12-16 | 1995-06-27 | Nippon Oil Co Ltd | Production of low-sulfur gas oil |
| 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 |
| CN101117594A (en) * | 2006-07-31 | 2008-02-06 | 中国石油化工股份有限公司 | Hydrogenation method for producing clean diesel oil |
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