CN1211467C - Hydrocarbon hydroconversion method - Google Patents
Hydrocarbon hydroconversion method Download PDFInfo
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- CN1211467C CN1211467C CN 02133119 CN02133119A CN1211467C CN 1211467 C CN1211467 C CN 1211467C CN 02133119 CN02133119 CN 02133119 CN 02133119 A CN02133119 A CN 02133119A CN 1211467 C CN1211467 C CN 1211467C
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Abstract
The present invention discloses a hydrogenation conversion method of hydrocarbons. A raw material contacts a catalyst having the functions of hydrodemetalization, hydrodesulfurization, hydrodenitrogenation and/or hydrocracking, a light fraction is separated out after the raw material is hydrodemetalized and hydrodesulfurized, and a hydrodenitrogenation reaction and/or a hydrocracking reaction is carried out among a heavy fraction, new hydrogen and purified hydrogen-rich gas. Compared with the prior art, the method of the present invention has the functions of hydrogenation saturation enhancement of condensed aromatics in the hydrocarbons, conversion rate improvement of a heavy raw material, impurity removal rate improvement of the heavy raw material, further drastic cracking reduction of a low boiling point fraction, hydrogen consumption reduction of a device, load reduction of a downstream lightening device, etc. The method of the present invention is most suitable for the fixed-bed hydrogenation conversion process of heavy oil and residual oil.
Description
1, technical field
The invention belongs to hydrocarbon hydrocracking technical field, a kind of improvement of hydro carbons fixed bed hydrogenation technology specifically, particularly heavy, residue fixed-bed hydrogenating conversion process.
2, background technology
As everyone knows, hydrocarbon hydrogenating conversion process is meant at high temperature, high pressure, and faces under the condition of hydrogen the conversion process of hydrocarbon raw material generation consumption hydrogen, hydrocarbon hydrogenating conversion process described herein, its raw material can be from hydro carbons of oil and/or coal and/or oil shale etc.The scope of application has the hydro-upgrading of all petroleum fractionss such as the pre-hydrotreatment of catalytic reforming raw material oil, petroleum naphtha hydrogenation processing, diesel oil hydrogenation processing, solid paraffin hydrotreatment, Vaseline hydrotreatment, lube oil hydrogenation processing and weight, residual hydrocracking.In hydroconversion process, the mixing raw material that contains hydrogen and hydro carbons contacts the generation hydrogenation reaction with catalyzer in one or more reactors, and operation condition is generally: temperature of reaction 240-450 ℃; Reaction pressure is 1.0-20.0MPa; Hydrogen to oil volume ratio is 50-2000; Volume space velocity is 0.1-7.5h during liquid
-1The typical chemical reaction that hydroconversion process takes place comprises that hydrodemetallation (HDM), hydrogenating desulfurization, hydrodenitrification, hydrogenation are saturated, hydrocracking and hydroisomerization.The hydroconversion reactions effluent contains unreacted hydrogen, conversion and unconverted hydro carbons and gas products, and these gas products comprise normally gaseous hydro carbons and foreign gas such as H
2S, NH
3Usually, the hydroconversion process resultant of reaction is separated into hydrogen-rich gas and the liquid phase hydrocarbon-type oil that is circulated to reactive system, and described liquid phase hydrocarbon-type oil can be used as the raw material or the catalytically cracked material of product or other hydroconversion process usually after separating.Realize the refining of hydrocarbon raw material and/lighting.
Purpose heavy, the initial exploitation of residual hydrocracking technology is from doctor positive crude production low sulphur fuel oil, but along with market to the reduction of oil fuel demand and to the vehicle fuel growth of requirement, the residual hydrogenation technology turns to gradually and is mainly downstream raw material lighting device such as devices such as catalytic cracking or coking are supplied raw materials, and becomes to attach most importance to, one of main means of residual oil lighting.By hydrotreatment, sulphur, nitrogen, metal impurities content and carbon residue in the poor residuum are obviously reduced, thereby obtain the charging that raw material lighting device in downstream can receive, especially be mainstream technology with residue fixed-bed hydrotreatment-RFCC combination technique in the catalytic cracking unit, therefore heavy at present, residual hydrogenation modifying process technology.But along with market to the superfluous of gasoline demand with to the extreme shortage of diesel oil demand, for being mainly used in the catalytic cracking unit of producing the gasoline lighting end, its residual oil raw material treatment capacity will increase slowly, even also reduction to some extent.But oil refining enterprise is for increasing the processing profit, will certainly more and more strengthen crude charging capacity, poor quality, the weight of heavy, residual oil output also can strengthen immediately, if strengthen the catalytic cracking treatment capacity, adapt to the increase of residual oil output, will certainly cause the market competition failure, but if go out the part amount in the residual oil is surplus, make oil fuel, not only profit is low, but also can cause the waste to petroleum resources.In view of this, make aforesaid combination technology adapt to market competition, must increase the middle runnings oil yield of this combination process and/or the transformation efficiency of increase residual oil, reduce residual oil output.For increasing the advantage of residual hydrogenation and catalytic cracking combined technique, US4,713,221 disclose on the residual hydrogenation of routine and catalytic cracking combined basis, the heavy cycle oil of catalytic cracking (comprising wax catalysis cracking and recycle stock catalytic cracking) is circulated to residual hydrogenation equipment, with carry out hydrogenation after residual oil mixes, enter catalytic cracking unit again.But this technology only improves profit by the yield that utilizes catalytic cracking turning oil to increase light oil, and does not increase the transformation efficiency of residual oil, reduces residual oil output, still has the pending problem of more residual oil.
The more employing fixed-bed reactor of residual hydrocracking technology, the catalyzer of difference in functionality are divided in different reactors or the different bed.The quick-reading flow sheets of existing this technology is: stock oil mixes before the charging process furnace with hydrogen, enters process furnace jointly, with temperature be heated to reaction temperature required after, enter reactor by the top of reactor.Stock oil and hydrogen enter each beds successively and hydrogenation reaction take place with downward stream mode and stream.After reaction finishes, the hydrogenation resultant enters gas-liquid separator, tell rich hydrogenous gas-phase product and liquid product, wherein rich hydrogenous gas-phase product Returning reactor after purifying continues to use, and liquid product goes separation column to fractionate out purpose product and non-purpose product, the purpose product goes out device, and non-purpose product can cyclic process or gone other devices of downstream to continue processing.
Generally heavy, residual oil (as the mixing oil of normal pressure residual oil, vacuum residuum, coal tar, deasphalted oil and the mink cell focus that extracts from oil-sand or shale or above-mentioned several heavy raw oils) all contains a large amount of sulphur, nitrogen and heavy metal impurity such as (as Ni, V).But residual oil is in the hydrotreatment process, its hydrogenating desulfurization is easier than hydrodenitrification and/or hydrocracking usually, therefore in the said fixing bed hydroprocessing technology, the hydrogen sulfide that hydrogenation reaction generates also can be with reactant flow successively by above-mentioned beds, hydrogenating desulfurization and hydrodenitrification to stock oil produce restraining effect, especially to hydrodenitrification and/or hydrocracking.Document ((English) applied catalysis A.General 154 (1997) 7-15) just points out that the existence of hydrogen sulfide can bring two kinds of bad influences to hydrotreatment, and promptly (1) is to the restraining effect of the part or all of function of hydrotreating catalyst; (2) blocking catalyst duct or reactor are played a driving role.Thereby cause the operational condition that hydrodenitrification and/or hydrocracking need be harsher than other hydrotreatment processes, shortened the work-ing life of hydrodenitrification and/or hydrocracking catalyst.In addition, the concurrent flow of reaction feed makes the hydrogen dividing potential drop height of easy hydro-upgrading part (hydrodemetallation (HDM), hydrogenating desulfurization etc.), and the hydrogen branch of difficult hydro-upgrading part (hydrodenitrification, removal of ccr by hydrotreating, hydrocracking etc.) forces down, and causes the low reaction rate of whole hydrogenation reaction.Moreover, the more lower boiling hydro carbons cut that generates in the hydrogenation process also flows with the reactant flow following current, has not only influenced the conversion of stock oil, has reduced the selectivity in the hydrogenation process, and conversion reaction further takes place, generation C in the high light ends fractionation meeting of added value
5 -Gaseous hydrocarbons promptly reduce refinery's profit, increased the hydrogen consumption of hydrogenation reaction again, increased the device running cost.
3, summary of the invention
At above shortcomings in the prior art, purpose of the present invention just provides a kind of improved residue fixed-bed hydrotreatment technology, can increase the impurity removal percentage and the transformation efficiency of residual hydrocracking technology, improve light oil yield, can reduce the residual oil yield again and reduce device hydrogen consumption, and make the combination of devices such as residue fixed-bed hydrotreatment technology and its downstream lighting device such as catalytic cracking, coking or hydrocracking more flexible, have market competitiveness more.
Processing method provided by the invention may further comprise the steps:
Isolatedly among A, residual oil raw material and the B enter hydrogenation unit to the small part hydrogen-rich gas, order is by hydrodemetallation (HDM) and Hydrobon catalyst or the catalyzer suitable with above-mentioned functions.Effluent separates, and isolates low boiler cut, hydrogen-rich gas and tail oil that residual oil raw material generates in reaction process.The new hydrogen that partly circulates also can enter hydrodemetallation (HDM) and Hydrobon catalyst.
Isolated tail oil hydrodenitrification and/or the hydrocracking catalyst bed that enters in the hydrogenation unit that be mixed continues reaction among B, the hydrogen (isolating hydrogen-rich gas and new hydrogen among the A through purifying) that come by circulating hydrogen compressor and the A.Reaction finishes, and reactant flow is separated, and isolates hydrogen-rich gas and liquid phase hydro carbons.The new hydrogen that enters whole apparatus system preferably all enters hydrodenitrification and/or hydrocracking catalyst bed.
C, isolated liquid phase hydro carbons further separates in B, continues the difference of lighting device at the downstream, isolates normal slag of petroleum naphtha, intermediate oil and hydrogenation or vacuum gas oil and hydrogenation and subtracts slag etc.Make downstream lighting device such as catalytic cracking, coking, hydrocracking or lube oil hydrogenation device etc. continue processing; And isolated hydrogen-rich gas is processed case part or is all gone to carry out washing, purifying, purification according to device is concrete, to improve its hydrogen purity.
Compared with prior art, the characteristics of hydrocarbons hydrogenation technology of the present invention have: the low boiler cut that (1) will enter in the raw material of high hydrocracking active catalyst (routine hydrodenitrogenation catalyst, hydrocracking catalyst etc.) bed is separated, promptly increase the hydrocracking of heavy ends, avoid the further overhydrocracking of low boiler cut again, reduce its value and increase device hydrogen consumption.(2) hydrogen that purity is high at first removes high hydrocracking active catalyst (routine hydrodenitrogenation catalyst, hydrocracking catalyst etc.) bed, the hydrogenation that increases condensed-nuclei aromatics in the hydro carbons is saturated, and then increase the hydrodenitrification rate and/or the hydrocracking rate of stock oil, also reduced the load of downstream lighting device (catalytic cracking, coking etc.).
4, description of drawings
Fig. 1 is the simple and easy schematic flow sheet of the embodiment of the invention, and Fig. 2 is a comparative example schematic flow sheet of the present invention.
5, embodiment
Further specify the solution of the present invention and effect below in conjunction with accompanying drawing.As shown in Figure 1, residual oil raw material 1 mixes with hydrogen-rich gas 14 by residual hydrogenation equipment end product separation system 12, enter the reactive system of hydrogenation unit jointly, order is passed through hydrodemetallation (HDM), hydrogenating desulfurization bed 2 and 4 through pipeline 3, so far resultant of reaction no longer directly enters hydrodenitrification and/or hydrocracking catalyst bed 11, but enter intermediates separation system 5, be separated into the low boiler cut 6 and the tail oil 7 that generate in hydrogen-rich gas 8, the hydrogenation process.Low boiler cut 6 directly goes out device, and hydrogen-rich gas 8 mixes with tail oil 7 after recycle compressor 10 boosts through washing, purifying, purification system 9 and additional new hydrogen merging, enters hydrodenitrification and/or hydrocracking catalyst bed 11 together again and proceeds reaction.After residual oil raw material 1 whole hydrogenation reactions finish, reactant flow enters residual hydrogenation equipment end product separation system 12, be separated into hydrogen-rich gas 14 and liquid phase hydro carbons 13, wherein hydrogen-rich gas 14 partly or entirely directly Returning reacting systems mix with residual oil raw material 1 and carry out hydrogenation reaction, liquid phase hydro carbons 13 is then pressed the difference of downstream lighting device, carry out different fractionation cuttings, be gas generally with its fractionation, petroleum naphtha, normal slag of intermediate oil and hydrogenation or vacuum gas oil and hydrogenation subtract slag etc., so that vacuum gas oil fraction is carried out hydrocracking or produced lubricant base, residue oil fraction can carry out catalytic cracking and/or coking.
Prior art as shown in Figure 2, residual oil raw material 1 mixes with recycle hydrogen 8, enters the reactive system of hydrogenation unit jointly, the order carry out hydroconversion reactions by hydrodemetallation (HDM), hydrogenating desulfurization, hydrodenitrification and/or hydrocracking catalyst bed 2,3 and 4.After reaction finished, resultant of reaction entered separation system 5, is separated into hydrogen-rich gas 7 and liquid phase hydro carbons 6.Hydrogen-rich gas 7 merges with new hydrogen through washing, purifying, purification system 9 and mixes with residual oil raw material 1 after recycle compressor 10 boosts.6 differences of liquid phase hydro carbons by downstream lighting device, carry out different fractionation cuttings, generally be that normal slag of gas, petroleum naphtha, intermediate oil and hydrogenation or vacuum gas oil and hydrogenation subtract slag etc. with its fractionation, so that vacuum gas oil fraction is carried out hydrocracking or produced lubricant base, residue oil fraction can carry out catalytic cracking and/or coking.
Heavy, residual hydrocracking technology of the present invention can be suitable for any Residue Hydrotreating Technology technology, especially is suitable for different reactor or beds, has the residual hydrogenation technology of different depth of conversion.As fixed bed residual hydrogenation technology, boiling bed residual oil hydrogen addition technology, expanded bed residual hydrogenation technology, moving-bed residual hydrogenation technology., residual hydrogenation technology heavy with at present industrial more ripe fixed bed is example: the heavy residual oil hydrocatalyst of employing is meant the single catalyst or the combination catalyst of functions such as having weight, residuum hydrogenating and metal-eliminating, hydrogenating desulfurization, hydrodenitrification and hydrocracking.These catalyzer generally all are to be carrier with porous refractory inorganic oxides such as aluminum oxide, the oxide compound of group vib and/or VIII family metal 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 CEN, the FZC series of being produced by Fushun new and high-tech development zone catalyst plant weighs, residuum hydrogenating and metal-eliminating catalyst, and ZTN, the ZTS catalyst series produced by first fertilizer plant of Qilu Petrochemical company just belong to this class catalyzer.At present in fixed bed residual hydrogenation technology, it often is the supporting use of multiple catalyzer, Hydrodemetalation catalyst, Hydrobon catalyst, hydrodenitrogenation catalyst are wherein arranged, and the filling order generally is that stock oil is contacted with hydrodemetallation (HDM), hydrogenating desulfurization, hydrodenitrification, hydrocracking catalyst successively.Technology with these several catalyst mix fillings is also arranged certainly.Be 5-35MPa in absolute pressure normally, preferably 10-20MPa, temperature are 300-500 ℃, preferably 350-450 ℃ of operation down.Volume space velocity and hydrogen dividing potential drop are to select according to the characteristic for the treatment of material and the transformation efficiency and the refining depth of requirement during liquid.Volume space velocity is generally at 0.1-5.0h during liquid
-1, 0.15-2h preferably
-1Scope in.Hydrogen to oil volume ratio is 100-5000, is preferably 300-3000.The present invention is applicable to the combination producing of the hydrocarbon hydrogenating conversion process that the hydrocarbon raw material depth of conversion is different.The cut scope of raw material hydrocarbon up to residual oil, is particularly useful for the hydrocracking of heavy hydrocarbon oil from gasoline, kerosene, diesel oil, wax oil.
Embodiment 1-3
Present embodiment with the residue fixed-bed example that is hydrogenated to, carries out the present invention's test on pilot scale residual hydrocracking device.The residue fixed-bed hydrogenation catalyst that uses in the test is heavy, the residuum hydrogenating and metal-eliminating catalyst of being produced by Fushun new and high-tech development zone of CEN, FZC series, by ZTN, ZTS series weight, residual hydrogenation denitrogenation, the desulfurization catalyst of first fertilizer plant of Qilu Petrochemical company production.The order of catalyst loading is hydrodemetallation (HDM), hydrogenating desulfurization, hydrodenitrogenation catalyst.The Hydrodemetalation catalyst that uses in this test is CEN-5, CEN-6; Protective material is CEN-2, CEN-4, FZC-16 (over current protection agent); Hydrobon catalyst ZTS-01, ZTS-02, ZTS-03; Hydrodenitrogenation catalyst ZTN-01.Filling ratio between each catalyzer is: CEN-2: FZC-16: CEN-4: CEN-5: CEN-6: ZTS-01: ZTS-02: ZTS-03: ZTN-01=1: 1.25: 1.5: 2.62: 7.8: 6.63: 0.69: 0.87: 11 (V/V).New hydrogen all enters the hydrodenitrification reactor, and hydrogen-rich gas behind the denitrification reaction and raw material are mixed into hydrodemetallation (HDM) and hydrodesulphurisatioreactors reactors.After purifying, the hydrogen-rich gas that obtains after hydrodemetallation (HDM), the desulfurization enters denitrification reactor with new hydrogen.
The stock oil that this test is used is Middle East residual oil, and character sees Table 1.Test-results sees Table-2.
Table 1 stock oil main character
| Project | Character | |
| Density (20 ℃), g/cm 3 | 1.018 | |
| Foreign matter content | S，w％ | 4.24 |
| N，w％ | 0.33 | |
| Carbon residue, w% | 20.2 | |
| Ni+V，μg/g | 120.3 | |
Table 2 residual hydrocracking result of the present invention
| Embodiment |
| 1 | 2 | 3 | |
| Operational condition | |||
| Reaction pressure, MPa | 16.0 | ||
| Reaction velocity, h -1 | 0.22 | ||
| Hydrogen-oil ratio, V/V | 761∶1 | ||
| Temperature of reaction, ℃ | 375 | 385 | 390 |
| Product distributes | |||
| H 2S+NH 3+C 4 -Loss | 1.11 | 1.58 | 2.15 |
| C 5-160℃ | 1.15 | 1.26 | 1.35 |
| 160℃-349℃ | 12.03 | 16.35 | 19.65 |
| 349℃-538℃ | 43.87 | 43.58 | 42.89 |
| 349℃ + | 85.71 | 80.81 | 76.85 |
| 349℃ +Residual oil impurity removal percentage (to stock oil) % | |||
| Desulfurization degree | 84.26 | 87.32 | 91.00 |
| Denitrification percent | 51.89 | 58.24 | 63.33 |
| Take off carbon yield | 70.65 | 74.08 | 76.99 |
| Take off (nickel+vanadium) rate | 87.22 | 90.11 | 92.78 |
Comparative example 1-3
This comparative example with the residue fixed-bed example that is hydrogenated to, has the Residue Hydrotreating Technology test now and is used for comparison on pilot scale residual hydrocracking device.The used same embodiment of catalyzer, stock oil, test conditions in the test, test-results sees Table-3.
Table 3 has the residual hydrocracking result now
| Comparative example | 1 | 2 | 3 |
| Operational condition | |||
| Reaction pressure, MPa | 16.0 | ||
| Reaction velocity, h -1 | 0.22 | ||
| Hydrogen-oil ratio, V/V | 761∶1 | ||
| Temperature of reaction, ℃ | 375 | 385 | 390 |
| Product distributes | |||
| H 2S+NH 3+C 4 -Loss | 1.07 | 1.21 | 2.65 |
| C 5-160℃ | 0.84 | 1.38 | 1.45 |
| 160℃-349℃ | 4.63 | 8.39 | 9.86 |
| 349℃-538℃ | 44.41 | 42.84 | 39.66 |
| 349℃ + | 93.46 | 89.02 | 86.04 |
| 349℃ +Residual oil impurity removal percentage (to stock oil) % | |||
| Desulfurization degree | 80.03 | 84.32 | 87.73 |
| Denitrification percent | 43.26 | 48.63 | 52.78 |
| Take off carbon yield | 62.31 | 67.35 | 71.28 |
| Take off (nickel+vanadium) rate | 83.37 | 85.22 | 87.19 |
By table-2 with show-3 as seen, light oil yield of the present invention, bottoms conversion and impurity removal percentage are all much larger than existing residual hydrocracking Technology.
Claims (5)
1, a kind of heavy, residue fixed-bed hydrogenating conversion process may further comprise the steps:
(1) isolatedly in residual oil raw material and the step (2) enters hydrogenation unit to the small part hydrogen-rich gas, order is by hydrodemetallation (HDM) and Hydrobon catalyst, effluent separates, and isolates low boiler cut, hydrogen-rich gas and tail oil that residual oil raw material generates in reaction process;
(2) isolated tail oil hydrodenitrification and/or the hydrocracking catalyst bed that enters in the hydrogenation unit that be mixed continues to react in the hydrogen that is come by circulating hydrogen compressor and the step (1), reactant flow is separated, isolate hydrogen-rich gas and liquid phase hydro carbons, wherein the hydrogen that comes of circulating hydrogen compressor comprises and separates the hydrogen-rich gas of purifying and new hydrogen in the step (1) through purifying;
(3) isolated liquid phase hydro carbons further separates in step (2), isolates normal slag of petroleum naphtha, intermediate oil and hydrogenation or vacuum gas oil and hydrogenation and subtracts slag;
Described operational condition heavy, residue fixed-bed hydrocracking is: absolute pressure is 5-35MPa, and temperature is 300-500 ℃, and volume space velocity is 0.1-5.0h during liquid
-1, hydrogen to oil volume ratio is 100-5000.
2, in accordance with the method for claim 1, the hydrogen that it is characterized in that entering in the step (1) hydrodemetallation (HDM) and Hydrobon catalyst comprises the part new hydrogen that circulates.
3, in accordance with the method for claim 1, it is characterized in that the described new hydrogen that enters hydrodenitrification and/or hydrocracking catalyst bed of step (2) is the whole new hydrogen that enters total system.
4, in accordance with the method for claim 1, it is characterized in that the described reaction effluent of step (2) separates the hydrogen-rich gas that obtains and partly or entirely carries out washing, purifying, purification.
5, in accordance with the method for claim 1, it is characterized in that described operational condition heavy, residue fixed-bed hydrocracking is: absolute pressure is that 10-20MPa, temperature are 350-450 ℃, and volume space velocity is 0.15-2h during liquid
-1, hydrogen to oil volume ratio is 300-3000.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02133119 CN1211467C (en) | 2002-10-10 | 2002-10-10 | Hydrocarbon hydroconversion method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02133119 CN1211467C (en) | 2002-10-10 | 2002-10-10 | Hydrocarbon hydroconversion method |
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| CN1488730A CN1488730A (en) | 2004-04-14 |
| CN1211467C true CN1211467C (en) | 2005-07-20 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103131469B (en) * | 2011-11-25 | 2015-05-13 | 中国石油天然气股份有限公司 | Fixed bed residue oil hydrotreating method |
| CN105524655B (en) * | 2014-10-24 | 2017-02-15 | 中国石油化工股份有限公司 | Heavy oil hydrodenitrogenation method |
| CN105586082B (en) * | 2014-10-24 | 2017-03-22 | 中国石油化工股份有限公司 | Hydro-denitrification method for heavy oil |
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