CN1294239C - Two stage hydrogenation treatment method of diesel oil - Google Patents
Two stage hydrogenation treatment method of diesel oil Download PDFInfo
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- CN1294239C CN1294239C CNB2004100209282A CN200410020928A CN1294239C CN 1294239 C CN1294239 C CN 1294239C CN B2004100209282 A CNB2004100209282 A CN B2004100209282A CN 200410020928 A CN200410020928 A CN 200410020928A CN 1294239 C CN1294239 C CN 1294239C
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Abstract
The present invention relates to a method for enhancing the hydrogenating and aromatic hydrocarbon shedding stability of two sections of a non-noble metal catalyst of a diesel oil fraction. A right amount of vulcanizing agent is added into a section of generated oil according to the present invention to serve as two-back mixing feeding or hydrogen sulphide is complemented into two-reversely circulating hydrogen, and the concentration of the hydrogen sulphide in the two-reversely circulating hydrogen is controlled to be 1000 to 2000 muL/L. The problem that a second section of catalyst in the hydrogenation technology of two sections of a non-noble metal catalyst of fraction oil is easy to inactivate can be solved, and the running period of the catalyst is prolonged. Meanwhile, the present invention has the advantages of low cost and large operating flexibility, and is easy to operate and control. The present invention is mainly used for the technological processes of the deep hydrodesulphurization of the diesel oil fraction, aromatic hydrocarbon shedding and high-quality clean fuel production.
Description
Technical field
The present invention relates to a kind of distillate two-stage hydrogenation treatment process, particularly diesel oil distillate adopts non-precious metal catalyst two-stage hydrogenation treatment process, specifically improves the method for second section non-precious metal catalyst activity stability in the processing of diesel oil distillate two-stage hydrogenation.
Background technology
For solving global environmental issue, must solve the problem of engine gas discharging, the production technology of exploitation low-sulfur, low aromatics diesel is one of the main research topic of 21st century Clean Fuel Production.In recent years, countries in the world were revised diesel oil standard in succession, and the relevant indexs of environmental pollution such as the sulphur content in the diesel oil, aromaticity content, cetane value and density are all proposed stricter requirement.The content of aromatic hydroxy compound directly determines character such as diesel fuel oil density, cetane value, so its problem that removes has caused the very big concern on oil refining circle.
The diesel oil hydrogenation aromatics-removing catalyzer can divide precious metal and non-precious metal catalyst by active ingredient, and this two classes catalyzer respectively has relative merits.Noble metal catalyst arene saturating activity height, particularly mononuclear aromatics is saturated, but the anti-sulphur of noble metal catalyst, nitrogen ability, (＜50 μ g/g) can demonstrate high hydrogenation dearomatization activity when only the sulphur in charging, nitrogen content were very low under low pressure high-speed condition; Noble metal catalyst costs an arm and a leg in addition, and therefore complex process has greatly limited it and applied.
Non-precious metal catalyst desulfurizing and eliminating aromatic hydrocarbons deeply Technology has characteristics such as less investment, technical process are simple, easy handling, existing hydro-refining unit is carried out the technical requirements that appropriate reconstruction can satisfy this technology, handle sulphur-bearing crude straight-run diesel oil and coker gas oil and can obtain " world's fuel oil standard " II class diesel oil.Therefore, adopting the non-precious metal catalyst desulfurizing and eliminating aromatic hydrocarbons deeply is one of effective means that reduces in aromatic hydrocarbons.
At present, the hydrogenation technique of production low sulfur and low aromatics diesel is mainly two-stage method technology, and first section is adopted the Ni-Mo/ aluminium oxide catalyst, adopts the noble metal catalyst with certain anti-sulphur second section more.Otherwise the two-stage method key is a liquid phase to enter two and preceding hydrogen sulfide and ammonia is removed, thereby has improved the hydrogen dividing potential drop of second reactor, helps the following of hydrogenation dearomatization hydrocarbon reaction and carries out.As described in CN1267709A, the diesel oil distillate raw material enters in first reactor, in the presence of hydrogen and non-precious metal catalyst, react, the material that reaction generates enters hot high score, the material that comes out from the separator bottom enters second reactor, reacts in the presence of hydrogen and noble metal catalyst, after the material that reaction generates separates through high-pressure separator, light pressure separator successively, obtain liquid product, the hydrogen-rich gas at high-pressure separator top recycles.Because second section is used noble metal catalyst, investment cost is higher.
USP5,183,556 disclose a kind of two step hydrogenation aromatics-removing methods of diesel oil, the first step raw material and hydrogen-rich gas and stream are by a kind of non-precious metal catalyst, remove gas component in the logistics that obtains by the first step by gas-liquid separation device then, liquid phase entered for second step and new hydrogen counter current contact is carried out deep hydrogenation, and the second step catalyst system therefor can be that non-precious metal catalyst also can be a noble metal catalyst.Two step hydrogenation processes can carry out also can carrying out in two different reactors in same reactor.Do not establish high pressure hot separator in the first step and between second step, the liquid phase of coming out from the first step directly entered for second step.This patent adopts counter-current operation for second section, because hydromechanical restriction, counter-current process can only moved than under the low hydrogen/gasoline ratio, makes reaction not operate under suitable condition.
CN1351118A discloses a kind of medium-pressure hydrocracking of diesel oil and has taken off the aromatic hydrocarbons method, two reactors in series, and promptly the effluent of first reactor enters second reactor without separation, and filling is with a kind of catalyzer.Though flow process is comparatively simple, volume space velocity is low, second reactor hydrogen pressures is low than first reactor, be unfavorable for arene engaging scraping; Heteroatoms hydrocarbon (hydrogen sulfide, ammonia) is unfavorable for desulfurizing and dearomatizing diesel oil deeply in the recycle hydrogen in addition.
If second section of two-stage method is used non-precious metal catalyst, because second section the gas phase and the sulphur content of liquid phase feeding are all very low, and for non-precious metal catalyst, reactive metal has advantages of high catalytic activity in sulphided state, the sulphided state metal then will lose reaction of Salmon-Saxl under these conditions, cause catalyst activity reduction, shorten running period.Non-precious metal catalyst loses the active reduction of sulphur under the low-sulfur environment, in other hydrocarbons hydrogenation is handled, similar situation is arranged also, in the disclosed hydrorefining paraffin wax method of CN1269395A, in operation process, in hydrogenation unit, mend sulphur or sulfocompound, to recover or maintenance wax hydrofining activity of such catalysts, wherein making the concentration of hydrogen sulfide in the recycle hydrogen is 50～20000 μ L/L, preferably controlling concentration of hydrogen sulfide when wherein mending sulphur continuously is 100～700 μ L/L, and preferably controlling concentration of hydrogen sulfide behind the benefit sulphur when intermittently mending sulphur is 2000～10000 μ L/L.This method can not simply directly be applicable to second section process in the diesel oil distillate two-stage hydrogenation technology.Because both operational conditions are different with influence factor.At first, those skilled in the art will know that, it is to utilize the very low condition of sulphur, nitrogen content in stock oil and the hydrogen that the diesel oil distillate two-stage method adds second section of processing, aromatic hydrocarbons in the stock oil is carried out Deep Hydrotreating, sulphur content increases in the system has adverse influence to the aromatic hydrocarbons saturated reaction, those skilled in the art can reduce the sulphur content that enters second section reactor as far as possible, therefore can not admit again to the scheme of wherein mending sulphur.And, do not have this problem for wax hydrofining.In addition, the service temperature of diesel oil hydrogenation and wax hydrofining is different, the wax hydrofining temperature is generally about 260 ℃, and the diesel oil fraction hydrogenating temperature is generally about 360 ℃, the mistake sulphur speed of non-precious metal catalyst is different with losing the sulphur state under the condition of different temperatures, thereby the condition of both optimums benefit sulphur should be different.
Summary of the invention
At the deficiencies in the prior art, the present invention proposes the method that a kind of turndown ratio is big, running is stable, investment is low, diesel oil distillate two-stage hydrogenation that the catalyst runs cycle is long takes off aromatic hydrocarbons.
By discovering in a large number, mend a certain amount of sulphur or sulfide in second section reactor in diesel oil two-stage hydrogenation treatment process, when concentration of hydrogen sulfide is in a certain specified range in the Control Circulation hydrogen, can reach when keeping catalyst stability, control is less to the influence of aromatic hydrocarbons saturated reaction, between catalyst stability and aromatic hydrocarbons saturation exponent, find appropriate trim point, realize the long-term stability running of diesel oil distillate two-stage method hydrotreatment.
The concrete grammar of diesel oil distillate two-stage method of the present invention hydrotreatment comprises: in the presence of diesel oil distillate oil hydroconversion condition and hydrogen, adopt sulphur and aromatic hydrocarbons in the two-stage hydrogenation method deep removal distillate, stock oil at first enters first section reactor, mainly carry out reactions such as desulfurization and denitrogenation and part aromatic hydrocarbons are saturated, remove impurity such as hydrogen sulfide in gas and the liquid and ammonia then, enter second reactor and mainly carry out deep desulfuration, denitrogenation and aromatic hydrocarbons saturated reaction, first section and second section is all used base metal sulphided state Hydrobon catalyst.Wherein generate and add an amount of sulphur or sulfocompound in the oil at first section, or benefit is gone into hydrogen sulfide in the second reactor cycles hydrogen, the concentration of hydrogen sulfide of controlling in the second reactor cycles hydrogen is 800～2500 μ L/L, is preferably 1000～2000 μ L/L, most preferably is 1200～1800 μ L/L.
Two reactors of the present invention all use non-precious metal catalyst, compare with the noble metal catalyst two-stage method, investment cost obviously reduces, and have solved noble metal catalyst and be easy to the problem that sulphur nitrogen is poisoned, and are easy to stable operation.Because the height of concentration of hydrogen sulfide is bigger to the activity and the stability influence of hydrogenation aromatics-removing, so the present invention can assurance device the performance catalyzer the highest take off smooth operation under the active prerequisite of aromatic hydrocarbons, just make the aromatic hydrogenation temperature of reaction in helping the scope of kinetic control, thus maximum reduction aromaticity content.Because second reactor is operated under very low concentration of hydrogen sulfide for a long time, can cause the valence state of catalyst activity component to reduce, influence the activity that catalyst hydrogenation takes off aromatic hydrocarbons, so hydrogen sulfide sectional pressure can address the above problem in the Control Circulation hydrogen, prolong the catalyst runs cycle.Concentration of hydrogen sulfide in the recycle hydrogen is too high, bigger to the influence of aromatic hydrocarbons saturated reaction, and concentration of hydrogen sulfide is too low, catalyst stability there is serious disadvantageous effect, therefore, find suitable concentration of hydrogen sulfide, take into account two aspect factors, make diesel oil distillate two-stage method hydrotreater realize the long period steady running.
Embodiment
The detailed process of the inventive method is:
The non-precious metal catalyst of packing in A, first, second reactor is established three beds in all, can liquid hydrogen injection between each bed.
Take off the aromatic hydrocarbons activity though B, non-precious metal catalyst are operated to improve under very low concentration of hydrogen sulfide, catalyzer mistake sulphur speeds up under this atmosphere for a long time, the active reduction.Add in the oil behind a small amount of sulphur or the vulcanizing agent as second reactor feed by generating toward one section, in the Control Circulation hydrogen below concentration of hydrogen sulfide 1000 μ L/L to the 2000 μ L/L, prolong the work-ing life of catalyzer, also can directly in the recycle hydrogen of second reactor, mend hydrogen sulfide.Mending sulphur can carry out continuously, also may be carried out batchwise.
C, interpolation vulcanizing agent are elemental sulfur or sulfocompound.Sulfocompound is the S-contained substance that easily generates hydrogen sulfide under reaction conditions with hydrogen, as in dithiocarbonic anhydride, organic sulfide, disulphide or polysulfide, the thiophene compound etc. one or more, and preferably elemental sulfur or dithiocarbonic anhydride.
Employed distillate feedstock is one or more a mixture of straight-run diesel oil, catalytic diesel oil, coker gas oil, visbreaking diesel oil among D, the present invention, and its sulphur content is not higher than 2.0 heavy %, and heavy metal is not higher than 1 μ g/g.Can use conventional base metal diesel oil hydrofining catalyst in first, second reactor, its active master is divided into tungsten-molybdenum-nickel etc., and two reactors can use identical catalyzer, also can use different catalyzer, preferably use same catalyst.
The processing condition of first reactor are: hydrogen dividing potential drop 3.0～10.0 MPas, volume space velocity 0.5～6.0 hour
-1, 290～400 ℃ of temperature of reaction, hydrogen to oil volume ratio 200～1000.Carry out desulfurization, the denitrogenation of distillate and take off reactions such as aromatic hydrocarbons at first reactor.
The processing condition of second reactor are: hydrogen dividing potential drop 3.0～10.0 MPas, volume space velocity 0.5～6.0 hour
-1, 290～400 ℃ of temperature of reaction, hydrogen to oil volume ratio 200～1000.Carry out deep desulfuration, the denitrogenation of distillate and take off the aromatic hydrocarbons reaction at second reactor.Two reactor can adopt the identical operations condition, also can adopt different operational conditions.
Further set forth technical scheme of the present invention below in conjunction with example.Raw materials usedly see Table 1.Catalyzer is selected the FH-98 Hydrobon catalyst for use.The composition and the quality index of FH-98 catalyzer see Table 2, and processing condition see Table 3, and refined diesel oil character sees Table 4.
Table 1, stock oil character
| Oil property | Stock oil 1 | Stock oil 2 |
| Density (20 ℃), g/cm 3Boiling range, ℃: fore-running～heat up in a steamer eventually sulphur, μ g/g nitrogen, μ g/g existent gum, the mg/100ml condensed-nuclei aromatics, the total aromatic hydrocarbons of m%, the m% cetane value | 0.8792 126～362 9900 650 270 23.9 50.7 38.9 | 0.9195 194/229 3900 711 162 20.3 71.2 22 |
The composition of table 2, catalyzer and quality index
| Catalyzer | FH-98 |
| Chemical constitution, m% WO 3 MoO 3The NiO pore volume, ml/g specific surface area, m 2/ g tap density, g/ml side pressure strength, N/cm | 20.2 9.3 4.2 0.30 140 0.96 160 |
Table 3, processing condition
| Processing condition | Example 1 | Example 2 | ||
| Stock oil | Stock oil 1 | Stock oil 2 | ||
| Reactor | One is anti- | Two is anti- | One is anti- | Two is anti- |
| Temperature of reaction, ℃ | 360 | 360 | 360 | 360 |
| Reaction pressure, Mpa | 6.0 | 7.0 | 8.0 | 8.0 |
| The volume of hydrogen oil ratio | 600 | 600 | 500 | 500 |
| Volume space velocity, h -1 | 1.8 | 1.2 | 1.5 | 1.0 |
Table 4-1 embodiment 1 refined diesel oil character
| Oil property | Oiliness 1 | Oiliness 2 | Oiliness 3 | Oiliness 4 | Oiliness 5 | Oiliness 6 | Oiliness 7 |
| Add vulcanizing agent | Add | Add | |||||
| Runtime, h | 480 | 2200 | 2400 | 4100 | 4300 | 5200 | 6000 |
| Concentration of hydrogen sulfide in the recycle hydrogen, μ l/l | 500 | 400 | 1200 | 800 | 1800 | 1600 | 1500 |
| Density (20 ℃), g/ml | 0.8335 | 0.8385 | 0.8367 | 0.8384 | 0.8330 | 0.8365 | 0.8335 |
| Boiling range, ℃/fore-running/heat up in a steamer eventually | 165/357 | 165/357 | 164/358 | 165/356 | 165/356 | 164/359 | 163/355 |
| Nitrogen, μ g/g | 1.5 | 3.5 | 1.5 | 3.8 | 1.5 | 1.7 | 1.5 |
| Sulphur, μ g/g | 19 | 23 | 21 | 25 | 22 | 24 | 24 |
| Existent gum, mg/100ml | 24 | 23 | 25 | 29 | 26 | 28 | 26 |
| Flash-point, ℃ | 70 | 68 | 68 | 68 | 69 | 67 | 69 |
| Aromatic hydrocarbons, % | 21.0 | 26.0 | 19.2 | 26.7 | 20.0 | 20.4 | 22.1 |
| The above aromatic hydrocarbons of two rings, m% | 2.1 | 2.3 | 1.9 | 2.4 | 2.2 | 2.3 | 2.5 |
| Cetane value | 53 | 48 | 53 | 46 | 52 | 51 | 51 |
Table 4-2 embodiment 2 refined diesel oil character
| Oil property | Oiliness 1 | Oiliness 2 | Oiliness 3 | Oiliness 4 | Oiliness 5 | Oiliness 6 | Oiliness 7 |
| Add vulcanizing agent | Add | Add | Desulphurization of recycle hydrogen | ||||
| Runtime, h | 400 | 1500 | 1700 | 2800 | 3000 | 3100 | 4100 |
| Concentration of hydrogen sulfide in the recycle hydrogen, μ l/l | 500 | 400 | 1100 | 1000 | 3000 | 1800 | 1700 |
| Density (20 ℃), g/ml | 0.8506 | 0.8576 | 0.8514 | 0.8574 | 0.8588 | 0.8522 | 0.530 |
| Boiling range, ℃/fore-running/heat up in a steamer eventually | 121/360 | 124/362 | 122/360 | 125/362 | 125/363 | 122/360 | 123/361 |
| Nitrogen, μ g/g | 1.2 | 2.0 | 1.3 | 2.1 | 2.6 | 1.3 | 1.4 |
| Sulphur, μ g/g | 1.2 | 5.0 | 1.5 | 5.2 | 6.3 | 1.4 | 1.6 |
| Existent gum, mg/100ml | 32 | 35 | 32 | 36 | 38 | 35 | 36 |
| Aromatic hydrocarbons, % | 16.5 | 23.2 | 16.8 | 24.0 | 26.4 | 16.6 | 16.8 |
| The above aromatic hydrocarbons of two rings, m% | 2.0 | 4.2 | 2.2 | 4.4 | 5.2 | 2.1 | 2.2 |
| Cetane value | 44.7 | 40.2 | 44.5 | 40.0 | 39.4 | 44.6 | 44.0 |
Claims (8)
1, a kind of diesel oil distillate two-stage method hydroprocessing process, comprise: diesel oil fraction hydrogenating condition and hydrogen exist down, adopt sulphur and aromatic hydrocarbons in the two-stage hydrogenation method deep removal distillate, stock oil at first enters first section reactor, carry out reactions such as desulfurization and denitrogenation and part aromatic hydrocarbons are saturated, remove hydrogen sulfide and ammonia impurity in gas and the liquid then, enter second reactor and mainly carry out deep desulfuration, denitrogenation and aromatic hydrocarbons saturated reaction, first section and second section is all used base metal sulphided state Hydrobon catalyst; It is characterized in that generating an amount of sulphur of interpolation or sulfocompound in the oil at first section, or mend hydrogen sulfide in the second reactor cycles hydrogen, the concentration of hydrogen sulfide of controlling in the second reactor cycles hydrogen is 800～2500 μ L/L.
2, in accordance with the method for claim 1, it is characterized in that the concentration of hydrogen sulfide in the described second reactor cycles hydrogen is 1000～2000 μ L/L.
3, in accordance with the method for claim 1, it is characterized in that the concentration of hydrogen sulfide in the described second reactor cycles hydrogen is 1200～1800 μ L/L.
4, in accordance with the method for claim 1, the benefit sulphur that it is characterized in that described second reactor carries out continuously or intermittently carries out.
5, in accordance with the method for claim 1, it is characterized in that the sulfocompound that adds in the generation oil in described first reactor is selected from one or more in dithiocarbonic anhydride, organic sulfide, disulphide or polysulfide, the thiophene compound.
6, in accordance with the method for claim 1, it is characterized in that described diesel oil distillate raw material is selected from one or more mixture of straight-run diesel oil, catalytic diesel oil, coker gas oil, visbreaking diesel oil, its sulphur content is not higher than 2.0 heavy %, and heavy metal is not higher than 1 μ g/g.
7, in accordance with the method for claim 1, the processing condition that it is characterized in that described first reactor are: hydrogen dividing potential drop 3.0～10.0 MPas, volume space velocity 0.5～6.0 hour
-1, 290～400 ℃ of temperature of reaction, hydrogen to oil volume ratio 200～1000.
8, in accordance with the method for claim 1, the processing condition that it is characterized in that described second reactor are: hydrogen dividing potential drop 3.0～10.0 MPas, volume space velocity 0.5～6.0 hour
-1, 290～400 ℃ of temperature of reaction, hydrogen to oil volume ratio 200～1000.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11118123B2 (en) | 2020-02-11 | 2021-09-14 | Saudi Arabian Oil Company | Processes and systems for petrochemical production integrating coking and deep hydrogenation of coking products |
| US11124716B2 (en) | 2020-02-11 | 2021-09-21 | Saudi Arabian Oil Company | Processes and systems for petrochemical production integrating coking and deep hydrogenation of coking reaction products |
| US11142708B2 (en) | 2020-02-11 | 2021-10-12 | Saudi Arabian Oil Company | Processes and systems for petrochemical production integrating deep hydrogenation of hydrotreated diesel |
| US11142711B2 (en) | 2020-02-11 | 2021-10-12 | Saudi Arabian Oil Company | Processes and systems for petrochemical production integrating deep hydrogenation of middle distillates |
| US11142706B2 (en) | 2020-02-11 | 2021-10-12 | Saudi Arabian Oil Company | Processes and systems for petrochemical production integrating fluid catalytic cracking and deep hydrogenation of fluid catalytic cracking reaction products |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100594231C (en) * | 2006-06-16 | 2010-03-17 | 中国石油化工股份有限公司 | One-stage serial hydrocraking process |
| CN100590181C (en) * | 2006-06-16 | 2010-02-17 | 中国石油化工股份有限公司 | Two-stage hydrocracking process |
| CN101619239B (en) * | 2008-07-04 | 2012-05-30 | 中国石油化工股份有限公司 | Method for hydrotreatment of heavy fraction of pyrolysis gasoline |
| CN101942330B (en) * | 2009-07-09 | 2013-06-19 | 中国石油化工股份有限公司 | Method for deep hydrogenation, sulfur removal and aromatics removal of diesel oil |
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| US6251262B1 (en) * | 1998-10-05 | 2001-06-26 | Nippon Mitsubishi Oil Corporation | Process for hydrodesulfurization of diesel gas oil |
| CN1485413A (en) * | 2002-09-28 | 2004-03-31 | 中国石油化工股份有限公司 | Process of desulfurizing and eliminating aromatic hydrocarbons deeply for diesel oil |
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| US6251262B1 (en) * | 1998-10-05 | 2001-06-26 | Nippon Mitsubishi Oil Corporation | Process for hydrodesulfurization of diesel gas oil |
| CN1485413A (en) * | 2002-09-28 | 2004-03-31 | 中国石油化工股份有限公司 | Process of desulfurizing and eliminating aromatic hydrocarbons deeply for diesel oil |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11118123B2 (en) | 2020-02-11 | 2021-09-14 | Saudi Arabian Oil Company | Processes and systems for petrochemical production integrating coking and deep hydrogenation of coking products |
| US11124716B2 (en) | 2020-02-11 | 2021-09-21 | Saudi Arabian Oil Company | Processes and systems for petrochemical production integrating coking and deep hydrogenation of coking reaction products |
| US11142708B2 (en) | 2020-02-11 | 2021-10-12 | Saudi Arabian Oil Company | Processes and systems for petrochemical production integrating deep hydrogenation of hydrotreated diesel |
| US11142709B2 (en) | 2020-02-11 | 2021-10-12 | Saudi Arabian Oil Company | Processes and systems for petrochemical production integrating deep hydrogenation of middle distillates from gas oil hydroprocessing |
| US11142707B2 (en) | 2020-02-11 | 2021-10-12 | Saudi Arabian Oil Company | Processes and systems for petrochemical production integrating deep hydrogenation of middle distillates |
| US11142711B2 (en) | 2020-02-11 | 2021-10-12 | Saudi Arabian Oil Company | Processes and systems for petrochemical production integrating deep hydrogenation of middle distillates |
| US11142710B2 (en) | 2020-02-11 | 2021-10-12 | Saudi Arabian Oil Company | Processes and systems for petrochemical production integrating deep hydrogenation of middle distillates obtained from residue hydrocracking |
| US11142706B2 (en) | 2020-02-11 | 2021-10-12 | Saudi Arabian Oil Company | Processes and systems for petrochemical production integrating fluid catalytic cracking and deep hydrogenation of fluid catalytic cracking reaction products |
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