CN1195829C - Poor heavy and residual oil weight-lightening process - Google Patents
Poor heavy and residual oil weight-lightening process Download PDFInfo
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- CN1195829C CN1195829C CNB021094209A CN02109420A CN1195829C CN 1195829 C CN1195829 C CN 1195829C CN B021094209 A CNB021094209 A CN B021094209A CN 02109420 A CN02109420 A CN 02109420A CN 1195829 C CN1195829 C CN 1195829C
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Abstract
The present invention discloses a weight-lightening method for poor-quality heavy oil and residual oil, which belongs to the processing technical field of heavy oil and residual oil. The problems of low light oil yield, difficult product utilization, etc. exist in the proposal for processing high-sulfur and poor-quality heavy oil and residual oil of the prior art. The method comprises the following steps: the hydrocracking technology of a suspension bed, the moderate hydroprocessing technology of the suspension bed and a coking technology are combined, and the poor-quality heavy oil and residual oil are processed. In the technical process, the poor-quality heavy oil and residual oil are directly hydrocracked by a metal catalyst with high activity via the suspension bed so that parts of the poor-quality heavy oil and residual oil are cracked into light-end products. Unconverted tail oil enters a moderate hydroprocessing device, and hydrogenized liquid products enter a coking device to generate dry gas, distillate oil and reusing coke with low sulfur contents. The present invention achieves the purposes for improving the yield of the poor-quality heavy oil and residual oil which are converted into the light-end products on the whole, effectively utilizing coke as a by-product and reducing environment pollution. The method can be used in the processing course of different kinds of poor-quality heavy oil and residual oil.
Description
Technical field
The present invention relates to a kind of method of heavy, residual oil lighting, particularly adopt floating bed hydrocracking, mild hydrogenation to handle and pyrogenic process integration is processed inferior heavy, residual oil.The invention belongs to the lighting processing treatment technical field of inferior heavy, residual oil, specifically the invention belongs to the technical field of the coke product that inferior heavy, residual oil thoroughly is converted into light-end products and is easy to utilize.
Background technology
Along with crude oil change weight, poor qualityization and the market demand to light-end products constantly increases, heavy, residual oil deep processing becomes the realistic problem that the refinery faces.Coking is a kind of maturation and simple heavy, residual oil lighting processing method.The residual oil of sweet crude oil adopts coking method to handle can obtain certain light oil yield, and the coke of by-product also has market.When the high poor residuum of processing sulphur, nitrogen, metal impurities content height, carbon residue content, not only coke and dry gas output are big to adopt coking process, and the liquid oil yield is low, and a large amount of inferior quality coke brings a lot of difficulties for accumulating and sale.Compare with coking process, residual hydrocracking has many advantages, can not produce coke especially when the processing high-sulfur residual oil.Yet when the inferior heavy of the conventional high nitrogen of fixed bed residual hydrogenation technical finesse, high metal, high carbon residue, residual oil, not only transformation efficiency is low but also catalyzer is poisoned easily, bed stops up easily.In order effectively to utilize poor residuum, many countries and major oil companies all adopt the floating bed hydrogenation technology of disperse type catalyzer in research.The tail oil that produces in heavy, hydrogenation of residual oil suspended bed upgrading process contains a large amount of carbon residues, sulphur, nitrogen, colloid and bituminous matter, therefore relatively is difficult to handle, and can't effectively be utilized, and has not only wasted resource but also contaminate environment.Treatment process to tail oil mainly is that tail oil is carried out coking or solvent deasphalting at present, but the effect of these methods is not very desirable.
Chinese patent CN1219569 discloses a kind of floating bed hydrogenation and the coking combination process is handled method heavy, residual oil.Although this combination process has improved the yield of light-end products, finally still be by-product coke.And this technology only is fit to processing low-sulfur raw material, and when processing high-sulfur inferior heavy, residual oil, these coke sulphur contents are higher, thereby can't directly use, and after needing coke carried out desulfurization and handle, use can act as a fuel.The common technical process of sulfur removal technology also can make the cost that utilizes of coke increase than complexity and this, even the coke cost after the processing is higher than the market value of coal far away, bring difficulty to sale,, promptly wasted resource and can produce detrimentally affect to environment again if these coke are given it up.
Chinese patent CN1143668 discloses a kind of floating bed hydrogenation and combined processing method of solvent deasphalting that adopts the oil soluble metal catalyzer.Heavy, residual oil with send into the floating bed hydrogenation reactor after the molybdenum naphthenate of 3000 μ g/g mixes, in the presence of hydrogen, be cracked into light component.Hydrogenation products obtains unconverted tail oil through distillation, this part tail oil after steps such as solvent deasphalting and the circulation of part de-oiled asphalt, the de-oiled asphalt that obtains deasphalted oil and form by bituminous matter, coke, catalyst metal.Three times the circulation after, the deasphalted oil that obtains accounts for the 50m% of relative raw material, and in de-oiled asphalt sulphur content more than 2m%, the minimum 6.6m% that also reaches of carbon residue.Catalyzer in this patent (in metal) add-on is bigger, and the catalyzer cost is significantly increased, and the de-oiled asphalt product of generation is more, second-rate owing to containing impurity, therefore is worth lower.And easy contaminate environment in the course of processing.
The EXXON oil company has announced the method for a kind of coking and floating bed hydrogenation combination process processing heavy oil in USP4569752.The advanced coking of residual oil raw material, the liquid product that coking is obtained is isolated the wax tailings less than 524 ℃ of cuts then, adds the laggard floating bed hydrogenation reactor of catalyzer and further transforms.Floating bed hydrogenation tail oil partly returns coker, and rest part throws away device.Though this technology has reduced the tail oil amount of floating bed hydrogenation process, can not fundamentally reduce the coke output of whole process, can not reduce the generation of dry gas, thereby total liquid product yield is still not high, usually below 50m%.Therefore, be restricted in industrial application.
Summary of the invention
Inferior heavy, residual oil carry out the yield that floating bed hydrocracking can improve liquid product, but the tail oil that generates is second-rate, relatively are difficult to handle, and this also is one of subject matter of this technological development of restriction.Tail oil behind inferior heavy, the dreg-oil suspension bed hydrogenation cracking contains a large amount of carbon residues, ash content, sulphur, nitrogen and metal impurities, can not directly enter coker, can cause the coke produced sulphur content higher because directly advance coker, can't utilize, cause environmental pollution easily.Owing to impurity in the tail oil is more, stop up bed easily in addition, make poisoning of catalyst, therefore can not carry out hydrofining with fixed bed comes desulfurization, denitrogenation.Acquire a certain degree of difficulty so they will be fully utilized really.
Because the C-S key in the residual oil molecule is easy to fracture, thereby causes high-sulfur residual oil to be easy to cracking, and the element sulphur that cracking is got off is present in the recycle hydrogen with the hydrogen sulfide form, this is again the prerequisite that keeps activity of hydrocatalyst.Because suspension bed does not have fixed bed, there is not the bed blockage problem simultaneously, good hydrogenation effect is arranged again.Thereby the tail oil behind the floating bed hydrocracking can be input to the floating bed hydrogenation device and carry out the demulcent hydrotreatment, remove part sulphur, nitrogen, make the part hydrogenation of unsaturated hydrocarbons saturated simultaneously.Product liquid behind the hydrogenation is carried out coking handle, can obtain more light ends oil and a spot of dry gas and coke, and the low use that can directly act as a fuel of the sulphur content of coke.Therefore the invention provides floating bed hydrocracking-floating bed hydrogenation processing-coking combination process that a kind of inferior heavy, residual oil that sulphur content is higher farthest is converted into light-end products and production low sulfur coke, can effectively address the above problem.
The invention provides the hydroprocessing process of a kind of inferior heavy, residual oil, its step comprises:
A, disperse type catalyzer and heavy, residual oil raw material are sent into the floating bed hydrocracking reactor after mixing, in the presence of hydrogen, carry out hydrocracking reaction;
B, the material that comes out from suspended-bed reactor after treatment, product liquid through water distilling apparatus cut out distillate (gasoline, diesel oil and VGO) and＞538 ℃ unconverted tail oil;
C, the said unconverted tail oil of step b is handled through the suspension bed mild hydrogenation,, reduced the content of impurity such as sulphur, nitrogen to reduce the viscosity of tail oil.Obtain hydrogenation products after isolating gas, in this technological process,, need not to add catalyzer as no special requirement;
D, the said hydrogenation tail oil of step c is sent into coker react, obtain light ends oil, dry gas and coke.The coke that generates can be used as metallurgical coke and uses or be used for combustion power generation, also can be used as fuel and is used for others.
Advantage of the present invention is:
1, adopt the process integration of dreg-oil suspension bed hydrogenation cracking, mild hydrogenation processing and coking process to handle inferior heavy, residual oil, this process integration can be when the high poor-quality heavy residuum of processing sulphur, nitrogen, metal impurities content height and carbon residue, obtains liquid oil to greatest extent and produces coke as far as possible less.
2, in hydrocracking process of suspended bed, adopt efficient disperse type catalyzer, effectively avoided the green coke of process, thereby make and do not contain solid particulate substantially in the tail oil.
3, the floating bed hydrocracking tail oil can directly be handled charging as mild hydrogenation, under than the demulcent condition, carry out hydrotreatment, to reduce the viscosity of tail oil, reduce the content of impurity such as sulphur, nitrogen, hydrogenation products can be used as the coking charging, has solved the problem that the floating bed hydrocracking tail oil is difficult to handle.
4, the suspension bed mild hydrogenation being handled the hydrogenation products input coker that obtains reacts, obtain liquid distillate oil, dry gas and coke, coke can be used as the metallurgical coke use or is used for combustion power generation, also can be used as fuel and be used for others, solved the difficult problem that high-sulfur raw material coking gained coke can't use.
5, dreg-oil suspension bed hydrogenation cracking, mild hydrogenation processing and pyrogenic process integration can make total light ends oil yield improve more than 10%, and technical process is simple, and easy to operate, facility investment is lower, and is very friendly to environment.
Embodiment
Handled heavy, the residual oil of the inventive method can be the residual oil that crude distillation obtains, as normal pressure residual oil, vacuum residuum etc., the heavy-gravity heavy crude oil, the de-oiled asphalt behind solvent extraction, also the high-sulfur inferior raw materials such as organism that obtain of oil sands bitumen, shale oil and the dry distillation of coal.
Adopt the process integration of floating bed hydrocracking, the processing of suspension bed mild hydrogenation and coking process among the present invention, handle inferior heavy, residual oil.Wherein, the employed disperse type catalyzer of floating bed hydrocracking is the compound of periodic table of elements VIB, VIIB and two or more metals of group VIII, wherein is the compound of metallic elements such as Mo, Ni, Co, W, Cr, Fe preferably.
At first with conventional dispersing method catalyzer is scattered in the stock oil, the total add-on of catalyst metal is 50～1000 μ g/g, is preferably 100～500 μ g/g, is preferably 200～400 μ g/g.Contain and enter the floating bed hydrogenation reactor after the stock oil of catalyzer and hydrogen mix.Hydrogenation and scission reaction take place in heavy, residual oil in reactor, change into low boiler cut to greatest extent.The floating bed hydrocracking reactor operating condition is common working conditions: pressure 6～20MPa, 430～450 ℃ of temperature, liquid hourly space velocity 0.5～2.0h
-1, hydrogen to oil volume ratio (under the standard pressure) 200～1500.
The treatment condition that said suspension bed mild hydrogenation is handled are: 350～430 ℃ of temperature, be preferably 380～420 ℃, and pressure 6～15MPa is preferably 8～14MPa, liquid hourly space velocity 0.1～1.0h
-1, be preferably 0.2～0.8h
-1, hydrogen to oil volume ratio (under the standard pressure) 200～1500 is preferably 500～1200.
The processing of said pyrogenic reaction is carried out under usual conditions: 450～550 ℃ of coking tower temperature ins, be preferably 480～510 ℃, tower top pressure 0.5～1.5MPa is preferably 0.7～1.0MPa, water injection rate (accounting for charging) 1.0m%～10.0m% is preferably 4.0m%～6.0m%.
For further specifying all main points of the present invention, enumerate following examples.
Embodiment 1～4
Present embodiment investigate different pressures, temperature, air speed, hydrogen-oil ratio, etc. under the operational condition, when using water-soluble molybdenum, nickel bimetal catalyzer, the dreg-oil suspension bed hydrogenation cracking response situation.Test raw material is to subtract slag in the normal slag of isolated island, husky light normal slag and the sand, and feedstock property sees Table 1.It is the poorest to subtract slag character as shown in Table 1 in the sand, and sulphur content and metal content are higher, and asphalt content reaches 8.4m%, and carbon residue surpasses 20m%, and nitrogen content is also higher, is a kind of more unmanageable poor residuum; And the normal slag in the Liaohe River is a kind of low-sulfur poor residuum; Normal slag of isolated island and husky light normal slag sulphur content are also higher, and feedstock property is also relatively poor.In the process of the test, earlier aqueous catalyst solution is joined in the residual oil, make it to stir, then mixture is carried out hydrogenation reaction on small-sized floating bed hydrocracking device, then the liquid hydrogenation products is cut into each cut with true boiling point.Test-results sees Table 2.In process of the test, the continuous apparatus running is not steadily stopped up, also can find out from continuous hydrogenation service test data: substantially not under the prerequisite of green coke, hydrogenation distillate (＜538 ℃) yield can reach more than the 70m%, and only produces a small amount of gas in the process, usually below 5m%.
Table 1 test stock oil character
Subtract slag in the husky light normal slag sand of the normal slag of the normal slag isolated island in the project Liaohe River
Density (20 ℃) kgm
-3982.9 965.3 969.4 1024.8
Carbon residue m% 13.37 8.73 9.71 20.73
Ultimate analysis m%
C 87.22 84.78 87.76 83.52
H 11.69 14.61 11.38 10.43
S 0.4 1.94 3.38 4.95
N 0.62 - 0.17 0.35
Metallic element μ g.g
-1
Fe 22.0 12.47 2.37 8.16
Ni 93.7 24.47 11.10 42.40
V 2.37 4.91 37.50 143.60
Na 5.65 26.53 1.53 -
Ca 74.0 16.92 1.25 2.88
Four proximate analysis m%
Stable hydrocarbon 30.4 31.4 40.3 9.9
Aromatic hydrocarbon 26.0 30.4 42.2 52.2
Colloid 38.5 36.6 14.3 29.5
Bituminous matter 1.0 1.6 3.2 8.4
The table 2 different catalysts aqueous solution is used for the residual hydrogenation test-results
Number 1234
In the husky light sand of raw material Liaohe River isolated island
The normal normal slag of the normal slag of slag subtracts slag
Cat add-on 350 400 400 300
μg.g
-1
Temperature ℃ 435 438 437 445
Pressure MPa 10 10 12 15
Hydrogen-oil ratio v/v 800 600 1,000 1200
Air speed h
-10.8 0.9 1.0 1.0
Product structure m9
Petroleum naphtha 12.2 13.0 12.7 11.8
Diesel oil 22.3 28.8 25.9 22.3
Wax oil 37.5 37.2 38.8 39.2
Tail oil 28.0 21.0 22.6 26.7
Embodiment 5～8
Present embodiment is the tail oil that residual oil is obtained behind floating bed hydrocracking, as the charging of mild hydrogenation treatment unit.The unconverted tail oil character of table 3 for obtaining after embodiment 1～4 hydrogenation products fractionation.Data show in the table, and the carbon residue of tail oil increases behind the hydrogenation of residual oil suspended bed, and hydrogen-carbon ratio descends.Table 4 is suspension bed mild hydrogenation treatment unit operational condition and data results.Except that generating a small amount of gas (generally being lower than 5m%), the above unconverted tail oil of 95m% can be used as the coking charging and uses in the process of the test.
Tail oil character that table 3 floating bed hydrogenation is unconverted
Raw material tail oil 1 tail oil 2 tail oils 3 tail oils 4
Density g.cm
-31.0310 1.0375 1.0297 1.0856
Viscosity mm
2/ s (100 ℃) 1,413 1,375 1,338 1522
Carbon residue m% 35.84 27.89 33.64 37.59
Ash content m% 0.23 0.20 0.23 0.31
Sulphur content m% 1.35 1.58 2.05 2.54
Nitrogen content m% 1.30 1.02 1.32 1.72
The data results that the mild hydrogenation of table 4 tail oil is handled
Number 5678
Raw material tail oil 1 tail oil 2 tail oils 3 tail oils 4
Temperature of reaction ℃ 410 420 410 430
Reaction pressure MPa 12.0 10.0 10.0 14.0
Air speed h
-10.6 0.5 0.4 0.2
Hydrogen-oil ratio v/v 800 1,000 1,000 1200
Viscosity mm
2/ s (100 ℃) 170.9 60.5 152.4 77.5
Sulphur content m% 0.18 0.46 0.72 0.65
Nitrogen content m% 0.70 0.50 0.68 0.81
Table 4 data show the unconverted tail oil of floating bed hydrogenation after the suspension bed mild hydrogenation is handled, and sulphur, the nitrogen content of product are lower, and viscosity is also lower.
Embodiment 9～12
Embodiment 9～12nd, and the hydrogenation products that embodiment 5～8 is obtained is as the charging of pyrogenic reaction, and carry out coking test on packaged unit, and reaction conditions and reaction result are listed in the table 5, and the character of coke produced is listed in the table 6.
Table 5 pyrogenic reaction condition and result
Number 9 10 11 12
Raw material hydrogenation products 5 hydrogenation products 6 hydrogenation products 7 hydrogenation products 8
The pyrogenic reaction condition
Coking tower temperature in ℃ 495 493 500 504
Coking tower temperature out ℃ 420 418 425 420
Furnace outlet temperature ℃ 500 505 510 510
Coking tower top pressure MPa 0.8 0.9 0.7 0.8
Treatment capacity kg/h 4.0 4.0 4.5 4.0
Water injection rate m% 6.0 5.0 5.0 5.5
Coke chemicals yield m%
Dry gas 10.5 12.0 11.6 10.3
Atmospheric distillate 22.9 24.2 26.3 25.8
Vacuum distillate 16.5 14.2 13.4 10.9
Coke 50.1 49.6 48.7 53.0
Table 6 coke property result
Number 9 10 11 12
Moisture m%＜1.0＜1.0＜1.0＜1.0
Volatile matter m% 5.0 5.8 6.5 4.9
Ash content m% 0.9 0.5 0.7 1.1
Sulphur content m% 0.84 1.17 1.63 1.85
The productive rate of coke generally accounts for the 50m% of coking product as can be seen from Table 5, and the productive rate of dry gas also accounts for about 10m%, thereby liquid product yield is lower, has only about 40m%.Product liquid is more much bigger than the value of coke and dry gas, so have only weight, residual oil is converted into liquid product as far as possible, just has industrial value.The data of table 6 show that the quality of coke can reach the standard that acts as a fuel substantially.During the low sulfur resid of processing, the coke that obtains even can be used as the charcoal element or Graphite Electrodes uses.
Listed the total recovery data results of the various cuts that adopt process integration of the present invention to handle these four kinds of residual oil in the table 7.Can find out that from table 7 coke yield that subtracts slag in normal slag in the Liaohe River and the sand is higher, liquid distillate oil yield is lower, utility value is lower by contrast, but liquid distillate oil yield also reaches more than the 75m%, is higher than the yield that only adopts coker or floating bed hydrocracking device far away.And for character normal slag of isolated island and husky light normal slag preferably, benefit is very tangible, and their liquid distillate oil yield all reaches more than the 80m%, and coke product also can be used as fuel, has utilized inferior heavy, residual oil raw material to the utmost.This shows and adopt process integration processing inferior heavy of the present invention, residual oil to have the advantage of highly significant.
Table 7 process integration is handled the data results of each cut total recovery of residual oil
Normal slag in the husky light normal slag sand of the normal slag of the normal slag isolated island in the raw material Liaohe River
Gas m% 9.0 8.2 8.4 8.8
Liquid distillate oil m% 78.3 82.4 81.7 78.4
Coke m% 12.7 9.4 9.9 12.8
Claims (7)
1, the lightening method of a kind of inferior heavy, residual oil, its step comprises:
A. disperse type catalyzer and heavy, residual oil raw material are sent into the floating bed hydrocracking reactor after mixing, in the presence of hydrogen, carry out hydrocracking reaction;
B. the product liquid that comes out from suspended-bed reactor cuts out distillate and unconverted tail oil through water distilling apparatus;
C. the said unconverted tail oil of step b is handled through the suspension bed mild hydrogenation;
D. the hydrogenation products that hydrotreatment described in the step c is obtained is sent into coker and is reacted, and obtains light ends oil, dry gas and coke;
Wherein the operational condition of said floating bed hydrocracking reactor is among the step a: pressure 6～20MPa, 430～450 ℃ of temperature, liquid hourly space velocity 0.5～2.0h
-1, hydrogen to oil volume ratio 200～1500 under the standard pressure; The treatment condition that said suspension bed mild hydrogenation is handled among the step c are: 350～430 ℃ of temperature, pressure 6～15MPa, liquid hourly space velocity 0.1～1.0h
-1, hydrogen to oil volume ratio 200～1500 under the standard pressure; The treatment condition of said pyrogenic reaction are in the steps d: 450～550 ℃ of coking tower temperature ins, tower top pressure 0.5～1.5MPa, water injection rate account for 1.0～10.0m% of charging.
2,, it is characterized in that said disperse type catalyzer is the compound of periodic table of elements VIB, VIIB and two or more metals of group VIII among the step a according to the lightening method of the described inferior heavy of claim 1, residual oil.
3,, it is characterized in that said disperse type catalyzer among the step a is two or more the compound among Mo, Ni, Co, W, Cr or the Fe according to the lightening method of the described inferior heavy of claim 1, residual oil.
4,, it is characterized in that the total add-on of said disperse type catalyzer metal is 50～1000 μ g/g according to the lightening method of claim 1,2 or 3 described inferior heavy, residual oil.
5,, it is characterized in that the total add-on of said disperse type catalyzer metal is 100～500 μ g/g according to the lightening method of the described inferior heavy of claim 1, residual oil.
6, according to the lightening method of the described inferior heavy of claim 1, residual oil, it is characterized in that the treatment condition that said suspension bed mild hydrogenation is handled among the step c are: temperature is 380～420 ℃, pressure 8～14MPa, liquid hourly space velocity 0.2～0.8h
-1, hydrogen to oil volume ratio 500～1200 under the standard pressure.
7, according to the lightening method of the described inferior heavy of claim 1, residual oil, the treatment condition that it is characterized in that said pyrogenic reaction in the steps d are: the coking tower temperature in is 480～510 ℃, tower top pressure is 0.7～1.0MPa, and water injection rate accounts for 4.0～6.0m% of charging.
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| CNB021094209A CN1195829C (en) | 2002-04-04 | 2002-04-04 | Poor heavy and residual oil weight-lightening process |
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| CNB021094209A CN1195829C (en) | 2002-04-04 | 2002-04-04 | Poor heavy and residual oil weight-lightening process |
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| CN1195829C true CN1195829C (en) | 2005-04-06 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US9644157B2 (en) * | 2012-07-30 | 2017-05-09 | Headwaters Heavy Oil, Llc | Methods and systems for upgrading heavy oil using catalytic hydrocracking and thermal coking |
| US11414607B2 (en) | 2015-09-22 | 2022-08-16 | Hydrocarbon Technology & Innovation, Llc | Upgraded ebullated bed reactor with increased production rate of converted products |
| US11414608B2 (en) | 2015-09-22 | 2022-08-16 | Hydrocarbon Technology & Innovation, Llc | Upgraded ebullated bed reactor used with opportunity feedstocks |
| US11421164B2 (en) | 2016-06-08 | 2022-08-23 | Hydrocarbon Technology & Innovation, Llc | Dual catalyst system for ebullated bed upgrading to produce improved quality vacuum residue product |
| MX2018002577A (en) | 2017-03-02 | 2018-11-09 | Hydrocarbon Tech & Innovation Llc | Upgraded ebullated bed reactor with less fouling sediment. |
| US11732203B2 (en) | 2017-03-02 | 2023-08-22 | Hydrocarbon Technology & Innovation, Llc | Ebullated bed reactor upgraded to produce sediment that causes less equipment fouling |
| CA3057131A1 (en) | 2018-10-17 | 2020-04-17 | Hydrocarbon Technology And Innovation, Llc | Upgraded ebullated bed reactor with no recycle buildup of asphaltenes in vacuum bottoms |
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