CN1488729A - Fractional oil two-stage hydrogenation dearomatizing method - Google Patents
Fractional oil two-stage hydrogenation dearomatizing method Download PDFInfo
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Abstract
The present invention provides a distillate two-stage hydrogenation process for removing aromatic hydrocarbon. It adopts two-stage hydrogenation process, and the reactors of said two stages adopt non-metal catalyst, and between inlet and outlet of reactor of every stage a switching pipeline is set, when the activity of catalyst of second reactor is reduced, the switching operation is made, the original second reactor can be used as first reactor, the original first reactor can be used as second reactor. Said invention mainly is used for making diesel oil fraction undergo the processes of deep hydrodesulfurization and removing aromatic hydrocarbon to produce high-grade clean fuel.
Description
1, technical field
The present invention relates to the method that a kind of distillate hydrogenation takes off aromatic hydrocarbons, particularly adopt the non-precious metal catalyst two-stage hydrogenation to take off the method for aromatic hydrocarbons.
2, background technology
Along with the increasingly stringent of countries in the world environmental regulation, the production technology of exploitation low-sulfur, low aromatics diesel is the 21st century subject matter that faced of Clean Fuel Production.In recent years, countries in the world were revised diesel oil standard in succession, and the sulphur content in the diesel oil, aromaticity content, cetane value and density etc. are all proposed stricter requirement." world fuel standards II class diesel oil standard is: sulphur content ≯ 300 μ g.g
-1, cetane value ≮ 53, aromaticity content ≯ 25m%, polycyclic aromatic hydrocarbons ≯ 5m%, density (15 ℃) ≯ 0.82～0.85g.cm
-3III class diesel oil standard is: sulphur content ≯ 30 μ g.g
-1, cetane value ≮ 55, aromaticity content ≯ 15m%, polycyclic aromatic hydrocarbons ≯ 2m%, density (15 ℃) are at 0.82～0.84g.cm
-3Between.Above-mentioned standard is all adopted or be about to adopt in countries in the world at present, the method of producing low-sulfur, low aromatic fraction oil in the prior art mainly contains two kinds: a kind of is to adopt non-precious metal catalyst, at different sorts diesel oil (straight bavin, urge bavin, Jiao Chai and Medium diesel oil thereof), (carry out single hop, two sections deep hydrodesulfurizationofs under 5.0～6.0MPa), take off the technological line of aromatic hydrocarbons, can obtain the diesel oil that quality meets " world's fuel oil standard " II class at middle pressure; Another kind of technological line is to adopt triple effect noble metal catalyst (desulfurization, denitrogenation, take off aromatic hydrocarbons), and the two-stage hydrogenation quality of production meets the diesel oil of " world's fuel oil standard " III class standard under middle pressure.
Noble metal catalyst makes it apply and is subjected to certain restriction owing to factors such as its sulphur-nitrogen resistant poor performance, plant investment expense height and catalyzer cost an arm and a leg; 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, produce low-sulfur both at home and abroad, the relevant patent report of low fragrant diesel oil generally adopts two-stage method technology, promptly first section is adopted the Ni-Mo/ aluminium oxide catalyst, and employing more than second section has the noble metal catalyst of certain sulfur tolerance.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 carrying out of hydrogenation dearomatization hydrocarbon reaction.CN1267709A discloses a kind of method of fractional oil two-stage hydrogenation dearomatizing, distillate feedstock 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, in the presence of hydrogen and noble metal catalyst, react, 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.Second section of this patent adopts counter-current operation, owing to be subjected to hydromechanical restriction, counter-current process can only be moving than under the low hydrogen/gasoline ratio, and is unfavorable to deeply de-aromatizing.
In two-stage hydrogenation deeply de-aromatizing technology, 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.The noble metal catalysts that adopt in the prior art take place to avoid the problems referred to above more.
3, summary of the invention
At the deficiencies in the prior art, the present invention proposes the method for the fractional oil two-stage hydrogenation dearomatizing that a kind of turndown ratio is big, running is stable, investment is low, the catalyst runs cycle is long.
The deeply hydrodearomatized method of aromatic hydrocarbons of the present invention comprises: in the presence of distillate hydrogenation 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.Principal feature is, between two reactor inlet, between the outlet, be provided with and switch pipeline and corresponding stopping valve, when second reactor activity descends, switch the effect of two reactors, with first reactor of former second reactor as desulfurization and denitrogenation, with former first reactor as the second saturated reactor of aromatic hydrocarbons.
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 easier 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 blocked operation of the present invention's one, two reactors 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; 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, and influences the activity of hydrogenation aromatics-removing, and blocked operation can address the above problem, and prolongs the catalyst runs cycle.The present invention can not influence under the ordinary production prerequisite of device, blocked operation by first and second reactor, handle in the distillate process at second reactor catalyst, make the catalyst activity component maintain higher sulfuration valence state, the work-ing life of improving the hydrogenating desulfurization of catalyzer and taking off aromatic hydrocarbons activity and catalyzer.
4, description of drawings
Fig. 1 is the inventive method principle process synoptic diagram.
Wherein 4 is first stage reactor, and 10 is second stage reactor, between two reactor inlet and the outlet switching pipeline is set.
5, embodiment
The detailed process of the inventive method is:
The non-precious metal catalyst of packing in A, first, second reactor, in establish two～four beds, 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.Therefore, the switching pipeline is set between two reactor, when second section reactor activity reduces, quality product drops to when defective, carries out blocked operation, can improve activity of such catalysts and stability.
C, distillate feedstock enter in first reactor, react in the presence of hydrogen and non-precious metal catalyst.
The material that D, first reactor generate enters high-pressure stripper and removes the hydrogen sulfide that is dissolved in the oil and ammonia after the hot high pressure oil pump enters two backheating stoves inlet, the gas that comes out from the top enters high score, in high score, carry out oil, vapour separation, the hydrogen-containing gas that comes out from the high score top enters the thionizer bottom and removes hydrogen sulfide, after circulating hydrogen compressor boosts, mix, inject second reactor process furnace inlet with hydrogen make-up.
E, the material that comes out from the high-pressure stripper bottom enter second reactor, react in the presence of hydrogen and non-precious metal catalyst.
The material that F, second reactor generate enters separation system through after the high-pressure separator, and the hydrogen-rich gas at high-pressure separator top mixes with an anti-stock oil.
Employed distillate feedstock is one or more a mixture of straight-run diesel oil, catalytic diesel oil, coker gas oil, visbreaking diesel oil among 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 non-noble metal Hydrobon 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 specify the flow process and the working method of the inventive method below in conjunction with accompanying drawing.
Distillate feedstock enters a backheating stove 2 through raw oil pump 1, enter first reactor 4 through valve 3 (valve 18 is closed), enter high-pressure stripper 6 through valve 5 (valve 20 is closed), the material that comes out from high-pressure stripper 6 bottoms enters two backheating stoves 8 through raw oil pump 7, heating is after valve 9 (valve 19 is closed) enters second reactor 10, resultant of reaction is through valve 11 (valve 21 is closed), enter high-pressure separator 12, be divided into gas-liquid two-phase, liquid product enters fractionating system 13, is divided into raw gasline and refined diesel oil by the cut weight.
The gaseous phase materials that comes out at high-pressure stripper 6 tops enters high-pressure separator 14, is divided into gas-liquid two-phase, and gaseous phase materials removes impurity such as hydrogen sulfide through thionizer 15, mix with the hydrogen make-up of boosting through make-up hydrogen compressor 17 after recycle compressor 16 boosts.The liquid phase part of high-pressure separator 12 bottoms enters fractionating system.The outlet of the incoming stock oil pump 1 of gas phase part at high-pressure separator 12 tops mixes with stock oil.
When the decline of the second reactor catalyst reactive behavior can not be satisfied the quality product requirement, valve 3,5,9,11 closed, and valve 18,19,20,21 open, and then can realize the blocked operation of first reactor and second reactor.Certainly, after the back catalyst activity as second reactor of switching descends once more, can carry out the blocked operation second time, total switching times can carry out more than twice or twice, till catalyzer is because of the other factors inactivation.
Switching pipeline between two reactor inlet and the outlet is configured to: one section has two pipelines to link with the second stage reactor inlet, article two, pipeline intersects with the interface of reactor inlet pipeline, promptly two to switch pipeline opposite with the interface front and back position of second section reactor inlet pipeline with the interface front and back position of first section reactor inlet pipeline, in the position that reaches between two connecting pipelines between reactor inlet pipeline and the switching pipeline interface stopping valve is set.The switching pipeline structure of two reactor outlet position is identical with the ingress.
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.In operation process, quality product descends in the time of can not meeting the demands, and carries out blocked operation.
Table 1, stock oil character
| Oil property | Stock oil 1 | | |
| Density (20 ℃), g/cm 3Boiling range, ℃: fore-running/10% 30%/50% 70%/90% 95%/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 | ????0.9195 ????194/229 ????257/285 ????314/346 ????359/365 ????3900 ????711 ????162 ????20.3 ????71.2 ????＜24 | ????0.8362 ????172/214 ????232/248 ????267/293 ????315/340 ????7800 ????171 ????40 ????8.0 ????30.2 ????48 | ????0.8692 ????156/231 ????253/278 ????308/343 ????350/366 ????10200 ????747 ????270 ????19.6 ????45.7 ????39.8 |
The composition of table 2, catalyzer and quality index
| Catalyzer | ????FH-98 |
| Chemical constitution, m% WO 3MoO 3The NiO pore volume, ml/g specific surface area, m 2/ g tap density, g/cm 3Side 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 | Example 3 | |||
| Stock oil | Stock oil 1 | | | |||
| Reactor | One is anti- | Two is anti- | One is anti- | Two is anti- | One is anti- | Two is anti- |
| Temperature of reaction, ℃ | 370 | ?360 | ?330 | ?350 | ????360 | ?360 |
| Reaction pressure, MPa | 9.0 | ?9.0 | ?5.0 | ?5.0 | ????7.0 | ?7.0 |
| The volume of hydrogen oil ratio | 800 | ?800 | 300 | ?300 | ????500 | ?500 |
| Volume space velocity, h -1 | 1.0 | ?1.0 | ?4.0 | ?4.0 | ????1.5 | ?1.5 |
Table 4-1 embodiment 1 refined diesel oil character
| Oil property | Before the switching | After the switching | ||
| Runtime, h | ????200 | ????2500 | ????200 | |
| Density (20 ℃), g/ml | ????0.8466 | ????0.8500 | ????0.8469 | |
| Boiling range, ℃ | Fore-running/10% | ????116/199 | ????120/200 | ????116/198 |
| ?30％/50％ | ????229/254 | ????229/255 | ????230/254 | |
| ?70％/90％ | ????285/332 | ????290/335 | ????285/332 | |
| 95%/heat up in a steamer eventually | ????352/360 | ????356/363 | ????350/361 | |
| Nitrogen, μ g/g | ????1.2 | ????1.5 | ????1.2 | |
| Sulphur, μ g/g | ????5.0 | ????10.0 | ????6.0 | |
| Existent gum, mg/100ml | ????30 | ????35 | ????32 | |
| Flash-point, ℃ | ????53 | ????56 | ????53 | |
| Aromatic hydrocarbons, % | ????21.3 | ????29.1 | ????22.4 | |
| The above aromatic hydrocarbons of two rings, m% | ????2.8 | ????6.1 | ????3.0 | |
| Cetane value | ????45 | ????40 | ????45 | |
Table 4-2 embodiment 2 refined diesel oil character
| Oil property | Before the switching | After the switching | ||
| Runtime, h | ????200 | ????3500 | ????200 | |
| Density (20 ℃), g/ml | ????0.8271 | ????0.8310 | ????0.8270 | |
| Boiling range, ℃ | Fore-running/10% | ????168/212 | ????170/212 | ????168/212 |
| ?30％/50％ | ????230/245 | ????232/246 | ????231/245 | |
| ?70％/90％ | ????265/290 | ????265/293 | ????265/290 | |
| 95%/heat up in a steamer eventually | ????312/338 | ????311/340 | ????310/337 | |
| Nitrogen, μ g/g | ????1.0 | ????1.5 | ????1.0 | |
| Sulphur, μ g/g | ????20 | ????30 | ????20 | |
| Existent gum, mg/100ml | ????2.0 | ????2.5 | ????2.0 | |
| Flash-point, ℃ | ????55 | ????55 | ????55 | |
| Aromatic hydrocarbons, m% | ????10 | ????25 | ????10 | |
| The above aromatic hydrocarbons of two rings, m% | ????1.5 | ????3.0 | ????1.6 | |
| Cetane value | ????57 | ????51 | ????57 | |
Table 4-3 embodiment 3 refined diesel oil character
| Oil property | Before the switching | After the switching | ||
| Runtime, h | ????200 | ????3000 | ????200 | |
| Density (20 ℃), g/ml | ????0.8333 | ????0.8410 | ????0.8328 | |
| Boiling range, ℃ | Fore-running/10% | ????141/218 | ????148/220 | ????140/216 |
| 30％/50％ | ????242/264 | ????242/264 | ????240/266 | |
| 70％/90％ | ????294/363 | ????294/363 | ????294/361 | |
| 95%/heat up in a steamer eventually | ????350/363 | ????355/368 | ????351/363 | |
| Nitrogen, μ g/g | ????1.8 | ????2.4 | ????1.9 | |
| Sulphur, μ g/g | ????24 | ????32 | ????25 | |
| Existent gum, mg/100ml | ????25 | ????30 | ????25 | |
| Flash-point, ℃ | ????62 | ????62 | ????62 | |
| Aromatic hydrocarbons, % | ????18.4 | ????27.0 | ????19.1 | |
| The above aromatic hydrocarbons of two rings, m% | ????2.7 | ????3.4 | ????2.7 | |
| Cetane value | ????55 | ????48 | ????55 | |
Claims (10)
1, a kind of distillate oil deep hydrogenation aromatics-removing method, in the presence of 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, remove hydrogen sulfide and ammonia in effluent gas and the liquid, enter second reactor, first reactor and second reactor all use base metal sulphided state Hydrobon catalyst, it is characterized in that between two reactor inlets, be provided with between the outlet and switch pipeline and corresponding stopping valve, when the active decline of second reactor catalyst, two reactors of blocked operation, with former second reactor as first reactor, with former first reactor as second reactor.
2, in accordance with the method for claim 1, it is characterized in that described first reactor uses identical Hydrobon catalyst with second reactor.
3, in accordance with the method for claim 1, it is characterized in that described distillate feedstock is selected from one or more mixture of straight-run diesel oil, catalytic diesel oil, coker gas oil, visbreaking diesel oil.
4, according to claim 1 or 2 described methods, the active ingredient that it is characterized in that described Hydrobon catalyst is tungsten-molybdenum-nickel.
5, in accordance with the method for claim 1, it is characterized in that described first reactor operating condition is: 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.
6, in accordance with the method for claim 1, it is characterized in that described second reactor operating condition is: 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.
7, in accordance with the method for claim 1, it is characterized in that the operational condition of described first reactor and second reactor is identical or different.
8, in accordance with the method for claim 1, it is characterized in that described blocked operation drops in quality product carries out when defective.
9,, it is characterized in that described blocked operation can carry out secondary or more than twice according to claim 1 or 8 described methods.
10, in accordance with the method for claim 1, it is characterized in that described switching pipeline between two reactors is configured to: one section has two pipelines to link with second stage reactor inlet, article two, pipeline intersects with the interface of reactor inlet pipeline, in between two connecting pipelines and the position between reactor inlet pipeline and the switching pipeline interface stopping valve is set, the switching pipeline structure of two reactor outlet position is identical with the ingress.
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| CN 02133133 CN1197939C (en) | 2002-10-10 | 2002-10-10 | Fractional oil two-stage hydrogenation dearomatizing method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1323141C (en) * | 2004-08-31 | 2007-06-27 | 中国石油化工股份有限公司 | Pour-point depressing method for increasing diesel product yield and quality |
| CN102311787A (en) * | 2010-07-07 | 2012-01-11 | 中国石油化工股份有限公司 | Method of hydrogenating liquefied petroleum gas to prepare ethylene cracking feed |
| CN103055766A (en) * | 2012-12-12 | 2013-04-24 | 烟台万华聚氨酯股份有限公司 | Two-section type switchable tubular reactor and method for preparing alcohol through aldehyde gas phase hydrogenation by using same |
| CN113088329A (en) * | 2019-12-23 | 2021-07-09 | 中国石油天然气股份有限公司 | Method and device for viscosity reduction and modification of inferior heavy oil |
-
2002
- 2002-10-10 CN CN 02133133 patent/CN1197939C/en not_active Expired - Lifetime
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1323141C (en) * | 2004-08-31 | 2007-06-27 | 中国石油化工股份有限公司 | Pour-point depressing method for increasing diesel product yield and quality |
| CN102311787A (en) * | 2010-07-07 | 2012-01-11 | 中国石油化工股份有限公司 | Method of hydrogenating liquefied petroleum gas to prepare ethylene cracking feed |
| CN102311787B (en) * | 2010-07-07 | 2014-05-21 | 中国石油化工股份有限公司 | Method of hydrogenating liquefied petroleum gas to prepare ethylene cracking feed |
| CN103055766A (en) * | 2012-12-12 | 2013-04-24 | 烟台万华聚氨酯股份有限公司 | Two-section type switchable tubular reactor and method for preparing alcohol through aldehyde gas phase hydrogenation by using same |
| CN103055766B (en) * | 2012-12-12 | 2014-12-31 | 万华化学集团股份有限公司 | Two-section type switchable tubular reactor and method for preparing alcohol through aldehyde gas phase hydrogenation by using same |
| CN113088329A (en) * | 2019-12-23 | 2021-07-09 | 中国石油天然气股份有限公司 | Method and device for viscosity reduction and modification of inferior heavy oil |
| CN113088329B (en) * | 2019-12-23 | 2023-02-24 | 中国石油天然气股份有限公司 | Method and device for viscosity reduction and modification of inferior heavy oil |
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|---|---|
| CN1197939C (en) | 2005-04-20 |
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