CN102041082A - Process of hydrogenation of heavy oil feedstock - Google Patents
Process of hydrogenation of heavy oil feedstock Download PDFInfo
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- CN102041082A CN102041082A CN2009101879316A CN200910187931A CN102041082A CN 102041082 A CN102041082 A CN 102041082A CN 2009101879316 A CN2009101879316 A CN 2009101879316A CN 200910187931 A CN200910187931 A CN 200910187931A CN 102041082 A CN102041082 A CN 102041082A
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Abstract
The invention discloses a process of hydrogenation of heavy oil feedstock, especially the process of hydrogenation of heavy oil feedstock using combination of boiling bed and fixed bed technologies. The process comprises the following steps: mixing heavy oil feedstock and the product obtained from the fixed bed hydrogenation; adding the mixture into boiling bed hydrogenation reactor, separating the materials obtained from boiling bed hydrogenation into to hydrogen-rich gas and liquid; recycling the hydrogen-rich gas; loading the liquid into the fractionate tower and for fractioning to obtain lightweight product and tail oil; mixing the tail oil and hydrogen, and adding the mixture into the fixed bed hydrogenation reactor; and adding all the materials obtained from fixed bed hydrogenation into the boiling bed hydrogenation reactor. Compared with existing technology, the method of the invention effectively combines the boiling bed and the fixed bed hydrogenation technology characteristics, allows the product obtained from fixed bed hydrogenation directly to enter the boiling bed reactor, thereby improves the flow state of the boiling bed feed, and enhances heat and mass transfer effects among gas, liquid and solid. Simultaneously, product properties are obviously improved after the tail oil obtained from the boiling bed hydrogenation is hydrogenated by the fixed bed. Employing the operation mode of the heavy oil hydrogenation can improve the product quality significantly and increase yield of the light oil obviously.
Description
Technical field
The present invention relates to the high inferior heavy of a kind of processing method of heavy oil feedstock hydrocracking, particularly metal, carbon residue and asphalt content, residual oil raw material combined technical method through ebullated bed and fixed bed hydrogenation process for producing light Fuel.
Background technology
Along with the variation of petroleum products demand structure in the exploitation energetically of heavy crude and the world wide, market maintains sustained and rapid growth to the demand of light-weight fuel oil, demand to heavy fuel oil (HFO) reduces rapidly, and the deep process technology of heavy oil has become the emphasis of petroleum refining industry's exploitation.Hydrogen addition technology is the important means of heavy oil lighting, and it can remove heteroatomss such as most of sulphur, nitrogen and metal when realizing higher yield of light oil, satisfy the environmental requirement of increasingly stringent.According to the beds difference of using, the heavy-oil hydrogenation technology can be divided into fixed bed hydrogenation, floating bed hydrogenation, moving-bed hydrogenation and boiling bed hydrogenation technology etc.Wherein, fixed bed heavy-oil hydrogenation technology is the most ripe, develops the most soon, but this technology is subjected to the feedstock property restriction, and the operational cycle is short; The boiling bed hydrogenation technology is used the online drainage technique that adds of catalyzer, it is wide to have adaptability to raw material, and the operational cycle is long, characteristics such as flexible operation, therefore this technical development is rapid, but this technology is owing to adopt the operator scheme of full back-mixing, and catalyst reactor is in boiling state, and raw material contacts not tight with catalyzer, mass transfer effect was undesirable between gas-liquid was solid, so, to compare with the fixed bed hydrogenation technology, it is relatively poor that this technology hydrogenation takes off the impurity effect.Ebullated bed is combined with the fixed bed hydrogenation technology, performance technical superiority separately can so that combination process both to have had an adaptability to raw material wide, running period is long, can improve the quality of products again.
In the combination process field of existing ebullated bed and fixed bed heavy-oil hydrogenation, common combination process process is: heavy oil feedstock is mixed into ebullated bed reactor with new hydrogen and carries out hydrogenation reaction, reacted whole logistics removes impurity after filtration or obtains distillate through distillation carries out hydrogenation reaction with the fixed bed hydrogenation device that new hydrogen is mixed into the downstream, this combination process only requires the design technology assembled scheme according to device to liquid phase feeding, not with the different process feature, logistics characteristic under the response behaviour and mass-and heat-transfer effect and final quality product organically combine, so fail to give full play to the sharpest edges of combination process.The process characteristic of ebullated bed reactor is: stock oil and hydrogen enter from reactor bottom, and the solid catalyst in the reactor is kept it and is at random boiling state by having the make progress lifting of mobile gas-liquid mixture of certain flow rate.In ebullated bed reactor, service temperature is higher, and liquid phase stream is that external phase and catalyzer are in boiling state, must guarantee gas-liquid fully contact admittedly, mass transfer and heat-transfer effect between the enhancing gas-liquid is solid so want to improve the hydrogenation reaction performance.Heavy hydrocarbon feeds especially condensed-nuclei aromatics, colloid and the asphalt content of vacuum residuum feed is higher, and viscosity is big, the mass transfer and the reaction of conducting heat between this restriction gas-liquid is solid.Address the above problem and to realize by the gas flow rate that reduces charging viscosity and increase in the reactor.How carry out the technical process appropriate design and at energy-conservation, production high-quality liquid fuel or for downstream unit provides charging under the condition efficiently, and the characteristic that can give full play to ebullated bed and fixed bed device flexible operating is the important developing direction in this area according to feedstock property.
US6277270 has introduced a kind of technological process of using fixed bed hydrogenation, boiling bed hydrogenation and catalytic cracking combined technique to handle the heavy crude hydrocarbon feed.Process description: residual oil raw material obtains decompressed wax oil and vacuum residuum through underpressure distillation, and wherein all or part of fixed bed hydrogenation treatment unit that enters of decompressed wax oil reacts, and the hydrogenation wax oil obtains distillate and hydrogenation tail oil (a) through the normal pressure distillation; Wherein vacuum residuum directly or be mixed into the ebullated bed device with the part decompressed wax oil and carry out hydrocracking reaction, generate oil and obtain atmospheric distillate and long residuum (b) through air distillation, wherein atmospheric distillate enters fixed bed hydrogenation reactor and carries out hydrogenation reaction, long residuum (b) or circulation enter the boiling bed hydrogenation device, the oily remover that perhaps acts as a fuel perhaps is mixed into heavy oil catalytically cracking equipment with hydrogenation tail oil (a).Heavy oil fluid catalytic cracking is come out slurry constituents can discharger, perhaps loops back the boiling bed hydrogenation conversion system.This combination process just requires to carry out the use of uniting of device according to the liquid feeding of different device, not specifically in conjunction with polytechnic feature, brings into play the sharpest edges of each technology as far as possible.
Summary of the invention
At the deficiencies in the prior art, the invention provides a kind of hydrogenating conversion process of heavy oil feedstock.Present method adopts ebullated bed and fixed bed combination process hydrocracking heavy oil to produce light ends oil, can give full play to two kinds of technology features, form and have complementary advantages, can improve the turndown ratio and the hydrogenation effect of combination process, can guarantee quality product and device smooth operation again.
The processing method of heavy oil feedstock hydrocracking of the present invention comprises:
(1) heavy oil feedstock and fixed bed hydrogenation reaction effluent enter ebullated bed reactor jointly and carry out hydrogenation reaction, and reaction effluent obtains hydrogen-rich gas and liquid product after separating;
(2) liquid product fractionation in separation column of obtaining of step (1) obtains gas, light Fuel and hydrogenation tail oil;
(3) all or part of hydrogenation tail oil and the hydrogen that obtain of step (2) is mixed into fixed bed hydrogenation reactor, and the fixed bed hydrogenation reactor reaction effluent enters the boiling bed hydrogenation reactor.
In the inventive method, the described heavy oil feedstock of step (1) comprises one or more in the inferior raw materials such as long residuum, vacuum residuum, deasphalted oil, oil sands bitumen, consistency crude oil, coal tar and gelatin liquefaction heavy oil.Wherein the boiling bed hydrogenation reactor is the known conventional ebullated bed reactor of this area professional, the gas phase that reaction back generates and liquid phase can be distinguished or discharge from reactor simultaneously, and gas phase need be provided with different outlets when discharging reactor respectively with liquid phase.Boiling bed hydrogenation catalyst is the hydrotreating catalyst of this area routine, and wherein the activity of such catalysts metal can be in nickel, cobalt, molybdenum or the tungsten one or more.Can comprise by weight percentage as the catalyzer composition: nickel or cobalt are 0.5%～15% (calculating by its oxide compound), molybdenum or tungsten are 1%～30% (calculating by its oxide compound), and carrier can be in aluminum oxide, silicon oxide, aluminium oxide-silicon oxide or the titanium oxide one or more.The shape of catalyzer is extrudate or sphere, and bulk density is 0.3～1.0g/cm
3, particle diameter (spherical diameter or bar shaped diameter) is 0.1～1.0mm, specific surface area is 80～300m
2/ g.The reaction conditions of boiling bed hydrogenation is: reaction pressure 6～30MPa, and temperature of reaction is 350～500 ℃, air speed is 0.1～5h
-1, the gas and oil volume ratio is 400～3000.The hydrogen-rich gas that step (1) obtains is used for fixing the bed hydroprocessing reactor through the circulation of processing such as depriving hydrogen sulphide back.Replenish new hydrogen and also can enter fixed bed hydrogenation reactor.
The cut point of described light Fuel of step (2) and hydrogenation tail oil is in 260～450 ℃ of scopes, preferably in 330～390 ℃ of scopes.Hydrogenation tail oil can all enter fixed-bed reactor, also can partly enter fixed bed hydrogenation reactor, and part is used for the raw material of other technological process, as the charging of catalytic cracking unit.
The described fixed bed hydrogenation reactor of step (3) is the known fixed bed residual hydrogenation of a this area professional reactor, the catalyzer that uses can be the hydrogenating desulfurization or the hydrodenitrogenation catalyst of single type, or be broad variety catalyzer grading loading, as FZC-101, FZC-34, FZC-41 or the FZC-42 etc. that use Fushun Petrochemical Research Institute to develop, it loads than being: FZC-101: FZC-34: FZC-41 (or FZC-42)=1～15: 20～70: 20～70.The reaction conditions of fixed bed hydrogenation is: reaction pressure 6～30MPa, and temperature of reaction is 350～420 ℃, air speed is 0.1～5h
-1, hydrogen to oil volume ratio is 400～2000.
Compared with prior art, the advantage of heavy-oil hydrogenation method for transformation of the present invention is:
1, adopts ebullated bed and fixed bed hydrogenation combination process processing inferior heavy oil raw material, can give full play to process characteristic separately, have complementary advantages, obtain hydrogenation effect and quality product preferably, the treating processes of having passed through ebullated bed enters the tail oil of fixed bed owing to can realize the long period smooth operation.
2, total overall reaction effluent and heavy oil feedstock behind the fixed bed hydrogenation are mixed into ebullated bed reactor, can effectively reduce the viscosity of ebullated bed liquid phase feeding, significantly improve the contact situation of gas-liquid-solid three-phase in the ebullated bed reactor, improve the hydrogenation reaction performance.
3, fixed bed hydrogenation reaction back effluent all enters the boiling bed hydrogenation reactor, helps the further post-refining of hydrogenation products, improves the quality of products.
4, the fractionation in a fractionation zone of ebullated bed and fixed bed hydrogenation product also together goes out system, can reduce facility investment, and simplifies technical process.
5, ebullated bed adopts different operational conditions with fixed bed, can realize operating method flexibly, realizes different processing purpose.
Description of drawings
Fig. 1 is a kind of process flow diagram of the present invention.
Embodiment
For further setting forth concrete feature of the present invention, will be illustrated in conjunction with the accompanying drawings.
In conjunction with the accompanying drawings 1, a kind of specific embodiment of the present invention is:
Effluent and recycle hydrogen are mixed into ebullated bed reactor 2 and carry out hydrogenation reaction behind heavy oil feedstock 1, the fixed bed hydrogenation, and the hydrogenation resultant that obtains obtains hydrogen-rich gas 4 and product liquid 12 through high-pressure separator 3.Hydrogen-rich gas 4 uses as recycle hydrogen through desulfurization or direct compressed machine supercharging; Product liquid 12 fractionation in separation column 7 obtains gas 8, gasoline 9, diesel oil 10 and hydrogenation tail oil 11, all or part of hydrogenation tail oil 11 is mixed in the fixed bed hydrogenation reactor 6 with new hydrogen 5 and recycle hydrogen, the fixed bed hydrogenation effluent that obtains directly and heavy oil feedstock 1 be mixed into the boiling bed hydrogenation reactor.
For further specifying the solution of the present invention and effect, enumerate following examples.The per-cent that wherein relates to all is weight percentage.
The residual oil raw material character that test is used is listed in table 1.This residual oil raw material carbon residue is 14.3% as shown in Table 1, and metal content is 218.9 μ g.g
-1, bituminous matter is 7.6%, and S content is 2.5%, and N content is 0.8%, is with the unmanageable inferior raw material of ordinary method.
Embodiment 1～2 and comparative example
Embodiment 1～2 is a kind of embodiment of boiling bed hydrogenation of the present invention and fixed bed hydrogenation combination process, and the operating process synoptic diagram is with reference to Fig. 1.
Comparative example is that heavy oil feedstock at first enters ebullated bed reactor, reaction back effluent obtains gasoline, diesel oil and hydrogenation tail oil behind separation and fractionation plant, wherein hydrogenation tail oil enters fixed bed hydrogenation reactor, reaction back logistics obtains gasoline, diesel oil and fixed bed hydrogenation tail oil through separation and water distilling apparatus, the fixed bed hydrogenation tail oil loops back ebullated bed reactor, and the corresponding light ends oil that fixed bed and ebullated bed obtain mixes discharges from system as product.
The boiling bed hydrogenation catalyst that process of the test is used as microspheroidal with the tungsten-nickel catalyzator of aluminum oxide as carrier, wherein contain WO in the catalyzer
3Be 8wt%, containing NiO is 3wt%.The bulk density of catalyzer is 0.60g/cm
3, surface-area is 150m
2/ g, the granules of catalyst mean diameter is 0.63mm.
The fixed bed hydrogenation catalyzer that process of the test is used is the FZC catalyst series of Fushun Petrochemical Research Institute's exploitation, wherein volume ratio FZC-101: FZC-34: FZC-41=5: 45: 50.
Reaction conditions and the results are shown in sees Table 2 and table 3.
Table 1 test residual oil raw material character
| Project | Data |
| Density (20 ℃), kg.m -3 | 1003.2 |
| Carbon residue, wt% | 14.3 |
| Viscosity (100 ℃), mm 2/s | 543.3 |
| Condensation point, ℃ | 42 |
| Ultimate analysis, wt% | |
| C/H | 85.3/11.2 |
| S/N | 2.5/0.8 |
| Metallic element, μ g.g -1 | |
| Fe/Ni/V | 2.9/38.6/177.4 |
| Four proximate analyses, wt% | |
| Stable hydrocarbon | 29.4 |
| Aromatic hydrocarbon | 33.1 |
| Colloid | 29.9 |
| Bituminous matter | 7.6 |
Table 2 reaction conditions
*The gas and oil volume ratio is the volume ratio of gas phase and stock oil, contains a large amount of light hydrocarbons in the gas phase except that hydrogen.
Table 3 reaction result
| Numbering | Embodiment 1 | |
Comparative example 1 |
| Gasoline | |||
| S/μg.g -1 | 150 | 133 | 220 |
| N/μg.g -1 | 4.1 | 2.3 | 19.7 |
| Yield, wt% | 19.7 | 21.7 | 31.6 |
| Diesel oil | |||
| S/μg.g -1 | 260 | 180 | 305 |
| N/μg.g -1 | 11.7 | 9.7 | 18.6 |
| Yield, wt% | 74.1 | 73.8 | 57.6 |
| Total liquid is received % | 93.8 | 95.5 | 89.2 |
By the data of embodiment and comparative example as can be seen, by hydrogenation combination technique of the present invention, under the condition of the operating severity that reduces device, improved the quality of light Fuel product, and total liquid is received higher.
Claims (10)
1. the processing method of a heavy oil feedstock hydrocracking is characterized in that comprising:
(1) heavy oil feedstock and fixed bed hydrogenation reaction effluent enter ebullated bed reactor jointly and carry out hydrogenation reaction, and reaction effluent obtains hydrogen-rich gas and liquid product after separating;
(2) liquid product fractionation in separation column of obtaining of step (1) obtains gas, light Fuel and hydrogenation tail oil;
(3) all or part of hydrogenation tail oil and the hydrogen that obtain of step (2) is mixed into fixed bed hydrogenation reactor, and the fixed bed hydrogenation reactor reaction effluent enters the boiling bed hydrogenation reactor.
2. it is characterized in that in accordance with the method for claim 1: the described heavy oil feedstock of step (1) comprises one or more in long residuum, vacuum residuum, deasphalted oil, oil sands bitumen, consistency crude oil, coal tar and the gelatin liquefaction heavy oil.
3. it is characterized in that in accordance with the method for claim 1: the boiling bed hydrogenation in the step (1) reacts the gas phase and the liquid phase difference of back generation or discharges from reactor simultaneously.
4. in accordance with the method for claim 1, it is characterized in that: the reactive metal of boiling bed hydrogenation catalyst is one or more in nickel, cobalt, molybdenum or the tungsten, catalyzer is formed and to be comprised by weight percentage: nickel or cobalt by nickel or cobalt/cobalt oxide are 0.5%～15%, are 1%～30% by the molybdenum or the tungsten of molybdenum or tungsten oxide.
5. in accordance with the method for claim 1, it is characterized in that: the reaction conditions of boiling bed hydrogenation is: reaction pressure 6～30MPa, and temperature of reaction is 350～500 ℃, air speed is 0.1～5h
-1, the gas and oil volume ratio is 400～3000.
6. it is characterized in that in accordance with the method for claim 1: the hydrogen-rich gas that step (1) obtains is handled the back circulation through depriving hydrogen sulphide and is used for fixing the bed hydroprocessing reactor.
7. it is characterized in that in accordance with the method for claim 1: the cut point of described light Fuel of step (2) and hydrogenation tail oil is in 260～450 ℃ of scopes.
8. according to claim 1 or 7 described methods, it is characterized in that: the cut point of described light Fuel of step (2) and hydrogenation tail oil is in 330～390 ℃ of scopes.
9. in accordance with the method for claim 1, it is characterized in that: the catalyzer that the described fixed bed hydrogenation reactor of step (3) uses is the hydrogenating desulfurization or the hydrodenitrogenation catalyst of single type, perhaps is broad variety catalyzer grading loading.
10. in accordance with the method for claim 1, it is characterized in that: step (3) fixed bed hydrogenation reaction conditions is: reaction pressure 6～30MPa, and temperature of reaction is 350～420 ℃, air speed is 0.1～5h
-1, hydrogen to oil volume ratio is 400～2000.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103102981A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Treating method for heavy raw material |
| CN105051163A (en) * | 2013-03-14 | 2015-11-11 | 鲁姆斯科技公司 | Integration of residue hydrocracking and hydrotreating |
| CN105733668A (en) * | 2014-12-06 | 2016-07-06 | 中国石油化工股份有限公司 | Coal tar hydrogenation treatment method |
| CN109913252A (en) * | 2017-12-13 | 2019-06-21 | 中国石油化工股份有限公司 | A kind of coal tar combined hydrogenation technique start-up method |
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| US6277270B1 (en) * | 1998-03-23 | 2001-08-21 | Institut Francais Du Petrole | Process for converting heavy petroleum fractions that comprise a fixed-bed hydrotreatment stage, an ebullated-bed conversion stage, and a catalytic cracking stage |
| CN1382776A (en) * | 2001-04-28 | 2002-12-04 | 中国石油化工股份有限公司 | Process for hydrogenating residual oil and catalytically cracking heavy oil |
| CN101007966A (en) * | 2006-01-12 | 2007-08-01 | 波克股份有限公司 | Heavy oil hydroconversion process |
| CN101376834A (en) * | 2007-08-27 | 2009-03-04 | 中国石油化工股份有限公司 | Bubbling bed combined process |
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2009
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US6277270B1 (en) * | 1998-03-23 | 2001-08-21 | Institut Francais Du Petrole | Process for converting heavy petroleum fractions that comprise a fixed-bed hydrotreatment stage, an ebullated-bed conversion stage, and a catalytic cracking stage |
| CN1295112A (en) * | 2000-11-02 | 2001-05-16 | 中国石油天然气股份有限公司 | Normal pressure suspension bed hydrogenation process adopting liquid multiple-metal catalyst |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103102981A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Treating method for heavy raw material |
| CN103102981B (en) * | 2011-11-10 | 2015-10-21 | 中国石油化工股份有限公司 | A kind of working method of heavy feed stock |
| CN105051163A (en) * | 2013-03-14 | 2015-11-11 | 鲁姆斯科技公司 | Integration of residue hydrocracking and hydrotreating |
| CN105733668A (en) * | 2014-12-06 | 2016-07-06 | 中国石油化工股份有限公司 | Coal tar hydrogenation treatment method |
| CN105733668B (en) * | 2014-12-06 | 2017-08-22 | 中国石油化工股份有限公司 | A kind of Hydrotreatment method for coal tar |
| CN109913252A (en) * | 2017-12-13 | 2019-06-21 | 中国石油化工股份有限公司 | A kind of coal tar combined hydrogenation technique start-up method |
| CN109913252B (en) * | 2017-12-13 | 2020-12-08 | 中国石油化工股份有限公司 | Coal tar combined hydrogenation process starting method |
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