CN1144860C - Process for hydrogenating residual oil - Google Patents
Process for hydrogenating residual oil Download PDFInfo
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- CN1144860C CN1144860C CNB011141662A CN01114166A CN1144860C CN 1144860 C CN1144860 C CN 1144860C CN B011141662 A CNB011141662 A CN B011141662A CN 01114166 A CN01114166 A CN 01114166A CN 1144860 C CN1144860 C CN 1144860C
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Abstract
The present invention relates to a hydrotreatment method of residual oil, which comprises: a first reactor in a hydrogenation reaction system of heavy residual oil is additionally provided with one or a plurality of feed inlets, and simultaneously, the original catalyst gradation is changed; when the pressure drop of an anticatalyst bed layer is 0.4 to 0.8 time higher than the maximal pressure drop designed in a device, the next feed inlet is orderly used instead of the previous feed inlet, and simultaneously, the original feed inlet can be used for feeding circulation oil or a mixture of the circulation oil and raw oil. The technology which can be used for effectively preventing the pressure drop of the bed layer and prolonging the service life of the hydrogenation catalyst for the residual oil can also be used for improving the treatment capability of the device to create high profits for refiners.
Description
The present invention relates to a kind of process for hydrogenating residual oil.This method is applicable to heavy oil residue hydrotreatment process, is specially adapted to the hydrotreatment process of fixed bed heavy oil residue.
The fixed bed residual hydrogenation is to handle main technique method bad, heavy oil residue at present, also be general, the most sophisticated most widely used technology, but also there is distinct disadvantage in it, that is exactly often because the beds differential pressure of first reactor is excessive when the processing poor quality oil, make device have to be forced to stop work, first catalyst in reactor is once cast aside the top or changed operation.So not only expend a large amount of time, and increased the device running expense.Therefore how preventing the beds pressure drop and prolonging catalyzer work-ing life is one of current the biggest problem that faces.
The reason that causes the first reactor bed pressure drop mainly is the beds fouling, stops up.The fouling of residual hydrogenation equipment can be divided into two kinds of situations, a kind of is large amount of organic and the inorganics class particulate deposition that exists in the residual oil, wherein inorganics refers to inorganic salt that Iron sulfuret, upstream device do not purify when crude oil is carried out desalination and other corrosion products etc., and organism refers to polymkeric substance that upstream device produces by radical polymerization, metal-catalyzed polymerization and non-free radical polymerization and coke etc.; Another kind is because of containing the polymerization that many complex mixtures with coke forming property at high temperature take place in the residual oil, and Conradson carbon residue promptly is to show to contain what one of index of coking tendency material in the residual oil.We once analyzed the lead reactor top bed powder dirt sample and the catalyzer of vacuum residuum device, and that finds dirty sample mainly consists of Iron sulfuret and coke, and wherein Iron sulfuret is maximum.As seen, Iron sulfuret and coke precursor are to cause the major cause of reactor fouling, and wherein Iron sulfuret is topmost, and it is self blocking catalyst bed not only, but also the reaction of the green coke of catalysis residual oil generates coke and comes the blocking catalyst bed.Iron sulfuret in the beds mainly contains two kinds of sources: the sulfur corrosion product of the iron that upstream device is come, the iron naphthenate in the crude oil generate under the condition that hydrogen exists.And the catalyst themselves in the residual hydrogenation equipment lead reactor is exactly a strainer, the mechanical impurity that enters reactor is all had filteration, so contained mechanical impurity can be deposited in the catalyzer space of reactor head bed in the residual oil raw material.The device start of run only can be tackled the macrobead greater than the catalyzer gap, forms gradually after the filter cake, and small-particle also is blocked, thereby generates the filter cake of one deck densification, causes reactor plugs, differential pressure to rise.
In order to solve the scale problems of residual hydrogenation equipment, from causing two kinds of mechanism of beds fouling, each major oil companies has taked multiple measure to solve the device scale problems.
It is the efficient raw material strainer of 25 μ m that Chevron company has used precision, but owing to the filter design reason, cause easily in it and leak, even design comparatively perfect strainer in addition, can not the effective elimination Iron sulfuret, the device beds fouling that still can induce reaction very soon (can be referring to " winning refining science and technology ", 1999,2,7～11).
CN1148404A discloses a kind of raising hydro carbons residual oil method for quality, this method is the organic solid particle that electrophoresis removes suspension from raw material residual oil, allow residual oil flow through one or more electrode containers that contain successively, DC electric field effect by electrode attracts to remove at least 10% inorganic solid particles, mainly is Armco magnetic iron.This method can not remove non magnetic iron class and easy green coke material, so can't avoid the problem of the fouling of residual hydrogenation equipment lead reactor beds.
Purpose of the present invention is exactly to improve the deficiency of above-mentioned residual oil method and technology, from the angle of technology own, proposes a kind of method of new residual hydrocracking, with the problem of the more economical bed pressure drop of solving device effectively.
Technical scheme of the present invention is as follows:
In the beds of first reactor that weighs the residual hydrogenation reactive system, set up the identical beds of one or more and former bed, on each newly-increased beds, offer a new opening for feed simultaneously, adopt original throat-fed at the device initial stage that goes into operation, when the first reactor catalyst bed pressure drop increases to the pressure drop upper limit, use next throat-fed successively instead.Wherein, the original operational condition of raw feed mouth and original opening for feed is identical.
The described first reactor catalyst bed pressure drop upper limit is generally 0.4-0.8 times of device design maximum pressure drop, is 0.6-0.8 times preferably.
When the mouth charging of having adopted next charging, opening for feed originally can advance the mixture of turning oil or turning oil and stock oil.
Described turning oil can be the cut between straight run or this device generate 160-540 ℃, is the distillate between 350-540 ℃ preferably.The blending ratio of described turning oil and raw material is 100%/0%-50%/50% (m), is 100%/0%-70%/30% (m) preferably.The original operational condition of opening for feed: temperature of reaction, pressure are identical during with normal running, and the 0.4-1.2 that hydrogen-oil ratio is generally normal running be 0.6-1.0 times preferably doubly, and said hydrogen-oil ratio is a hydrogen and the ratio of turning oil; The circulation oil mass is generally 0-0.8 times of device inlet amount, is 0.2-0.6 times preferably.
In order better to describe the present invention, be that example describes in detail with the fixed-bed reactor of setting up an opening for feed below.
Described catalyzer grating refers under the prerequisite that does not change original other reactor grating; the protective material or the metal remover of first reactor head are divided into two beds; the volume ratio of two beds is generally 5%/95%-50%/50% up and down, is 20%/80%-40%/60% preferably.The position of setting up opening for feed is between two beds.
The residual hydrocracking normal operating condition is: temperature of reaction 300-420 ℃, and preferably 350-410 ℃; Reaction pressure is 10-16MPa, and that best is 13-15MPa; Hydrogen to oil volume ratio is 500-2000, and that best is 700-1500; Volume space velocity is 0.1-1.0h during liquid
-1, that best is 0.2-0.4h
-1
Described heavy residual oil hydrocatalyst can be single catalyst or the series catalyst with weight, residuum hydrogenating and metal-eliminating, hydrogenating desulfurization, hydrodenitrification and hydrocracking function.These catalyzer generally all are to be carrier with porous inorganic oxide such as aluminum oxide, the oxide compound of group vib and/or VIII family metal oxide such as W, Mo, Co, Ni etc. is an active ingredient, the catalyzer that optionally adds other various auxiliary agents such as P, Si, elements such as F, B, for example heavy, residuum hydrogenating and metal-eliminating catalyst and ZTN, the ZTS catalyst series produced by first fertilizer plant of Qilu Petrochemical company by CEN, FZC series that Fushun Petrochemical Research Institute pilot scale base produces.
Described residual oil can be crude oil, by the long residuum and the vacuum residuum of crude oil gained, various oil that obtain by coal, tar sand, resinous shale and pitch and their mixture.
The present invention can be used for different structure reactor, preferably fixed-bed reactor.
Fig. 1 is material a kind of embodiment schema of mobile fixed bed reaction system from the top down that the present invention sets up an opening for feed.
As shown in Figure 1, the residual oil raw material is through after the heat exchange, reach temperature required form of mixing with hydrogen 02 with the upper reaches through pipeline 01 and enter the first reactor 1, then enter subsequent reactor 2 through pipeline 06, reaction enters in the high-temperature high-pressure separator 3 by pipeline 07, isolated lighter hydrocarbons gas enters cryogenic high pressure separator 4 through the washings washing of being injected by 08 pipeline by 09 pipeline, separator 3 and 4 isolated oil enter in the fractionating column 5 through pipeline 10, separator 4 isolated gases return hydrogen 02 pipeline through pipeline 11, and fractionating column 5 is separated into oil 13 at the bottom of the tower, gas oil 14, diesel oil 15 and naphtha 16 to oil. After reactor 1 pressure reduction arrived to a certain degree, raw material entered through 03 pipeline, and pipeline 04 changes into into the mixture of recycle oil or recycle oil and feedstock oil. Dotted line represents with the diesel oil 15, gas oil 14 or their mixture that self the generate a kind of embodiment as recycle oil among the figure.
Compared with prior art, advantage of the present invention is: 1) at utmost reduce the fouling of residual oil hydrogenation reaction system reactor, effectively prevent bed pressure drop; 2) help following reaction district reaction mass and hydrogen well distributed from the material flow of raw material material that mouth advances behind catalyst bed reaction; 3) recycle oil can adopt more bad straight-run, has increased the disposal ability of device; 4) greatly prolonged service life of hydrogenation catalyst.
Embodiment 1-4
The present invention carries out on 3 liter fixed bed hydrogenation Processing Test devices of design voluntarily, this device adopts three reactors in series, the top-down technical process of stock oil, wherein one instead set up a beds along the logistics direction, simultaneously offered an opening for feed above this bed, the position is at 1/3 place of reactor along the logistics direction.The complete series catalyst for hydrotreatment of residual oil of Fushun Petrochemical Research Institute's exploitation is adopted in this test; wherein; CEN, FZC series weight, residual hydrogenation protective material, catalyst for demetalation are produced by Fushun Petrochemical Research Institute pilot scale base; ZTN, ZTS series hydrogenating desulfurization agent, denitrfying agent are produced by first fertilizer plant of Qilu Petrochemical company, and the main physico-chemical property of catalyzer sees Table 1.
Table 1: the main physico-chemical property of catalyst system therefor of the present invention
| Catalyzer | Shape | Pore volume, ml/g | Specific surface, m 2/g | Tap density, g/ml | Metal is formed, m% | ||
| NiO | MoO 3 | ||||||
| Protective material | CEN-2 | Ellipsoid | 1.18 | 150 | 0.41 | 2.5 | - |
| CEN-4 | Spherical | 1.22 | 133 | 0.42 | 2.0 | - | |
| FZC-16 | Spherical | 0.49 | 156 | 0.76 | 2.5 | - | |
| Metal remover | CEN-5 | Cylinder | 0.66 | 136 | 0.55 | 3.1 | - |
| CEN-6 | Cylinder | 0.62 | 150 | 0.60 | 3.1 | 8.9 | |
| Sweetening agent | ZTS-01 | Cylinder | 0.38 | 145 | 0.85 | 19.0 | 4.5 |
| ZTS-02 | Cylinder | 0.39 | 145 | 0.85 | 18.5 | 4.5 | |
| Denitrfying agent | ZTN-01 | Cylinder | 0.40 | 210 | 0.85 | 22.5 | 9.1 |
The filling situation of each anticatalyzer is: one instead is divided into two bed fillings from top to bottom, two bed catalyst loadings order, each catalyst loading volume ratio are identical up and down, the filling order is CEN-2, CEN4, FZC-16, CEN-5, CEN6 from top to bottom, filling ratio (V) is: 1: 1.5: 2.2: 2.4: 13, two bed catalyzer cumulative volume ratios were 1: 2 up and down; Two instead load ZTS01 and ZTS02 from top to bottom, and filling ratio (V) is: 7.5: 1; Three instead load ZTN01 from top to bottom, and the filling ratio (V) of three reactors is 45: 25: 30.
Install airtight qualified after, beginning feeding temperature-raising sulfuration, after catalyst activity was stable, (hydrogen-oil ratio was 758 (v/v) for reaction pressure 15.7MPa, 385 ℃ of temperature of reaction, volume space velocity 0.2h during liquid in the standard operation condition
-1) under to subtract slag with blended Iran be raw material, adopt former opening for feed to advance stock oil, the main character of stock oil is listed in following table 2.In the steady running of slag input oil after 4000 hours, one anticatalyzer bed pressure drop is upgraded to 0.6 times of device design maximum pressure drop, use instead and set up opening for feed and advance stock oil, simultaneously former opening for feed improves various turning oils or do not advance turning oil, and the operational condition of improving turning oil is: 15.7MPa, 385 ℃, hydrogen-oil ratio are that original 0.5 times, circulation oil mass are 20% of device inlet amount.Turning oil has two kinds, and a kind of is direct-distilled intermediate oil and vacuum gas oil, and another kind is intermediate oil and the vacuum gas oil that self generates, and the main character of turning oil sees Table 3.
Table 2: test raw material oil main character
| Density (20 ℃) Kg/m 3 | 981.6 |
| S，m％ | 3.12 |
| N，m％ | 0.30 |
| Carbon residue, m% | 13.49 |
| (Ni+V)，μg/g | 115.0 |
| Four components, m% | |
| Stable hydrocarbon | 30.1 |
| Aromatic hydrocarbon | 47.5 |
| Colloid | 19.2 |
| Bituminous matter | 3.2 |
Wherein, the test of embodiment 1 for not advancing turning oil; Embodiment 2 is the into test of straight run intermediate oil; Embodiment 3 is the into test of straight run vacuum gas oil; Embodiment 4 is the middle runnings oil test that into self generates; The vacuum gas oil test of embodiment 5 for self generating.The test-results of each embodiment gathers lists in the table 4.
Table 3: the main character of turning oil
| Turning oil | A | B | C | D |
| The source | Straight run | Self generates | ||
| Density (20 ℃), Kg/m3 | 846.5 | 911.6 | 865.0 | 899.2 |
| S，μg/g | 12400 | 15500 | 41.0 | 683 |
| N，μg/g | 201.4 | 1468 | 88.5 | 568 |
| Boiling range ASTM, ℃ | D-86 | D-1160 | D-86 | D-1160 |
| Initial boiling point | 198 | 362 | 192 | 358 |
| 10％ | 265 | 401 | 230 | 395 |
| 30％ | 286 | 431 | 265 | 421 |
| 50％ | 301 | 459 | 288 | 450 |
| 70％ | 317 | 495 | 304 | 482 |
| 90％ | 341 | 533 | 319 | 523 |
| 95％ | 351 | 545 | 325 | 536 |
| Do | 361 | 555 | 335 | 543 |
Table 4: test-results
| The turning oil operational condition: | |||||||
| Reaction pressure, MPa | 15.7 | ||||||
| Temperature of reaction, ℃ | 385 | ||||||
| The multiple * of hydrogen-oil ratio | 0.4 | ||||||
| The multiple * of internal circulating load | 0.2 | ||||||
| Stock oil | Former opening for feed | Residual oil | - | A | B | C | D |
| Set up opening for feed | - | Residual oil | Residual oil | Residual oil | Residual oil | Residual oil | |
| Runtime, h | 4000 | 4100 | 4250 | 4400 | 4550 | 4700 | |
| Desulfurization degree, % | 86.3 | 86.3 | 86.4 | 85.7 | 86.1 | 85.5 | |
| Denitrification percent, % | 52.5 | 52.4 | 52.6 | 52.2 | 52.2 | 52.3 | |
| Take off carbon yield, % | 66.1 | 66.0 | 66.0 | 65.9 | 65.8 | 65.8 | |
| Take off (Ni+V) rate, % | 87.4 | 87.3 | 87.4 | 87.0 | 87.2 | 87.0 | |
| The multiple of indication item when * multiple index standard is operated | |||||||
Embodiment 5-8
Testing apparatus, catalyst loading, standard operation condition are with embodiment 1, and changing former throat-fed is stock oil and turning oil, the test that embodiment 5 advances 50%A/50% residual oil for former opening for feed; The test that embodiment 6 advances 70%B/30% residual oil for former opening for feed; The test that embodiment 7 advances 60%C/40% residual oil for former opening for feed; The test that embodiment 8 advances 80%D/20% residual oil for former opening for feed, each embodiment concrete operations condition and test-results gather and see Table 5.
Table 5: test-results
| The turning oil operational condition: | ||||||
| Reaction pressure, MPa | 15.7 | |||||
| Temperature of reaction, ℃ | 385 | |||||
| The multiple * of hydrogen-oil ratio | - | 0.4 | 0.6 | 0.6 | 1.0 | |
| The multiple * of internal circulating load | 0 | 0.2 | 0.3 | 0.2 | 0.4 | |
| Stock oil | Former opening for feed | Residual oil | 50%A/ 50% residual oil | 70%B/30 % residual oil | 60%C/ 40% residual oil | 80%D/20 % residual oil |
| Set up opening for feed | - | Residual oil | Residual oil | Residual oil | Residual oil | |
| Runtime, h | 5000 | 5100 | 5300 | 5500 | 5700 | |
| Desulfurization degree, % | 86.2 | 84.6 | 85.3 | 84.3 | 85.2 | |
| Denitrification percent, % | 53.6 | 52.1 | 52.8 | 52.4 | 52.7 | |
| Take off carbon yield, % | 64.7 | 63.2 | 63.9 | 63.3 | 63.6 | |
| Take off (Ni+V) rate, % | 86.9 | 83.5 | 85.2 | 83.3 | 84.5 | |
| The multiple of indication item when * multiple index standard is operated | ||||||
Claims (9)
1. one kind weighs process for hydrogenating residual oil, it is characterized in that in the beds of first reactor of original weight residual hydrogenation reactive system, setting up the identical beds of one or more and former bed, on each newly-increased beds, offer a new opening for feed simultaneously, adopt original throat-fed at the device initial stage that goes into operation, when the first reactor catalyst bed pressure drop increases to the pressure drop upper limit, use next throat-fed successively instead, wherein, the original normal operating condition of raw feed mouth and former opening for feed is identical; Said normal operating condition is: temperature of reaction 300-420 ℃; Reaction pressure is 10-16MPa; Hydrogen to oil volume ratio is 500-2000; Volume space velocity is 0.1-1.0h during liquid
-1
2. according to the described treatment process of claim 1, it is characterized in that the said pressure drop upper limit, for installing 0.4-0.8 times that designs maximum pressure drop.
3. according to the described treatment process of claim 1, it is characterized in that when having adopted next throat-fed that opening for feed originally can advance the mixture of turning oil or turning oil and stock oil.
4. according to the described treatment process of claim 3, it is characterized in that said turning oil is the distillate between straight run or this device generate 160-540 ℃.
5. according to the described treatment process of claim 3, the blending ratio that it is characterized in that said turning oil and raw material is 100m%/0m%-50m%/50m%.
6. according to the described treatment process of claim 5, the blending ratio that it is characterized in that said turning oil and raw material is 100m%/0m%-70m%/30m%.
7. according to the described treatment process of claim 1, it is characterized in that the operational condition of former opening for feed when adopting next throat-fed is: temperature of reaction is identical during with reaction pressure and normal running, and hydrogen-oil ratio is 0.4-1.2 a times of normal running; The circulation oil mass is 0-0.8 a times of device inlet amount.
8. according to the described treatment process of claim 1, it is characterized in that the operational condition of former opening for feed when adopting next throat-fed is: temperature of reaction is identical during with reaction pressure and normal running, and hydrogen-oil ratio is 0.6-1.0 a times of normal running; The circulation oil mass is 0.2-0.6 a times of device inlet amount.
9. according to the described treatment process of claim 1, it is characterized in that said normal operating condition is: temperature of reaction 350-410 ℃; Reaction pressure is 13-15MPa; Hydrogen to oil volume ratio is 700-1500; Volume space velocity is 0.2-0.4h during liquid
-1
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| CNB011141662A CN1144860C (en) | 2001-07-02 | 2001-07-02 | Process for hydrogenating residual oil |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102816595A (en) * | 2011-06-10 | 2012-12-12 | 中国石油天然气股份有限公司 | Residual oil hydrotreating and catalytic cracking combined process |
| CN102816598A (en) * | 2011-06-10 | 2012-12-12 | 中国石油天然气股份有限公司 | Method for reducing carbon deposition of carbon residue removal catalyst of residual oil hydrotreater |
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| CN101768468B (en) * | 2008-12-31 | 2013-11-06 | 中国石油化工股份有限公司 | Hydrogenation method for residual oil |
| CN102311764B (en) * | 2010-07-07 | 2013-12-04 | 中国石油化工股份有限公司 | Method for grading catalyst for hydrogenation treatment |
| CN102443415B (en) * | 2010-10-12 | 2013-12-04 | 中国石油化工股份有限公司 | Grading distribution scheme for hydrogenation treatment catalysts |
| CN102443411B (en) * | 2010-10-13 | 2013-12-04 | 中国石油化工股份有限公司 | Process method for prolonging operation period of hydrogenation device |
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| CN102952579B (en) * | 2011-08-26 | 2015-11-18 | 中国石油天然气股份有限公司 | Inferior heavy oil hydrotreating process for maximally improving catalyst utilization rate |
| CN102952581B (en) * | 2011-08-26 | 2015-05-27 | 中国石油天然气股份有限公司 | Hydrotreating process for inferior heavy oil |
| CN103059931B (en) * | 2011-10-21 | 2014-12-31 | 中国石油化工股份有限公司 | Residual oil hydrotreating method |
| CN103102958B (en) * | 2011-11-10 | 2015-01-14 | 中国石油化工股份有限公司 | Residual oil hydrogenation method for high quality diesel oil yield increase |
| CN106701172B (en) | 2015-11-12 | 2018-06-12 | 中国石油化工股份有限公司 | A kind of process for hydrogenating residual oil |
| CN107875978B (en) * | 2016-09-29 | 2021-06-11 | 中国石油化工股份有限公司 | Grading filling method and application of hydrogenation catalyst |
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2001
- 2001-07-02 CN CNB011141662A patent/CN1144860C/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102816595A (en) * | 2011-06-10 | 2012-12-12 | 中国石油天然气股份有限公司 | Residual oil hydrotreating and catalytic cracking combined process |
| CN102816598A (en) * | 2011-06-10 | 2012-12-12 | 中国石油天然气股份有限公司 | Method for reducing carbon deposition of carbon residue removal catalyst of residual oil hydrotreater |
| CN102816598B (en) * | 2011-06-10 | 2014-06-04 | 中国石油天然气股份有限公司 | Method for reducing carbon deposition of carbon residue removal catalyst of residual oil hydrotreater |
| CN102816595B (en) * | 2011-06-10 | 2014-06-04 | 中国石油天然气股份有限公司 | Residual oil hydrotreating and catalytic cracking combined process |
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