CN102453525B - Multi-stage boiling bed hydrogenation process - Google Patents
Multi-stage boiling bed hydrogenation process Download PDFInfo
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- CN102453525B CN102453525B CN201010522203.9A CN201010522203A CN102453525B CN 102453525 B CN102453525 B CN 102453525B CN 201010522203 A CN201010522203 A CN 201010522203A CN 102453525 B CN102453525 B CN 102453525B
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Abstract
The invention discloses a multi-stage boiling bed hydrogenation process. The method comprises the following steps of: mixing a hydrocarbon raw material and hydrogen, making the mixture enter a boiling bed reactor through the bottom of the boiling bed reactor; and reacting under the hydrotreatment conditions, wherein the boiling bed reactor comprises two or more than two internal circulation areas, and the internal circulation areas are provided with different operating sections. A plurality of internal circulation areas are formed in the boiling bed reactor, and different operating sections are formed, so that the whole boiling bed reactor is more flexible in operation, the properties of a reaction material flow can be reasonably matched with the performance of a catalyst, the activity of the catalyst is fully exerted, and the light oil yield and product quality are improved.
Description
Technical field
The present invention relates to a kind of Multi-stage boiling bed hydrogenation process, specifically in same ebullated bed reactor, form a plurality of different operatings interval, hydrocarbon feed carries out the processing method of hydrocracking between the operational zone with different operating condition.
Background technology
Boiling bed hydrogenation is gas, liquid, solid phase reaction process, hydrocarbon feed and hydrogen enter the pressurizing chamber of ebullated bed reactor after mixing from reactor bottom with upflowing, then along the reactor axis gas-liquid distributing disc of upwards flowing through, enter the comfort zone of ebullated bed reactor.Solid catalyst particle in reactor bed is promoted by the gas-liquid flow velocity making progress, and maintains granules of catalyst in random boiling shape.Desirable ebullated bed reactor is full back-mixed reactors, in effective catalytic hydrocracking reaction zone, liquid stream, gas and solid catalyst are uniformly distributed, the logistics composition of reactor exit and the logistics in reactor form basic identical, so the unreacted raw material of part will be along with product after transforming together outflow reactor.Because the feed stock conversion of full back-mixed reactors is lower, so conventionally adopt the operating method of a plurality of reactors in series, the differential responses section of the same reactor that the catalyzer of identical or different function is seated in to different reactors successively or separates with dividing plate, to improve the transformation efficiency of raw material.This will increase cost of investment, cause the irrational utilization of resource, how under lower cost, carry out boiling bed hydrogenation operation, and can improve the quality of products to greatest extent and feed stock conversion is the major issue that is worth further investigation.
US Re 25,770 has described typical boiling bed process, and gas-liquid logistics enters ebullated bed reactor from reactor bottom, then along reactor, axially rises and keeps catalyzer in boiling shape, internal recycle cup is set in reactor and carries out gas-liquid separation.Whole reactor is in back-mixing state, and whole reactant flow transforms under identical operational condition, so the transformation efficiency of feed stream is lower, and quality product is poor.
Chinese patent CN01106024.7 has introduced a kind of method for modifying that adopts ebullated bed processing poor quality oil.In this invention, introduce with fluid distribution dish or sieve plate ebullated bed reactor is separated and forms different conversion zones, the catalyst loading of different hydrogenating functions is carried out to hydrogenation reaction at different conversion zones.Shortcoming of the present invention is: owing to using dividing plate that reactor is divided into differential responses section, need to carry out on differential responses section top the effectively separated of solid and gas-liquid mixture, otherwise catalyzer is by the duct of blocking on distributing disc, this need to increase separated space or set up separating device, thereby limited catalyzer ratio of expansion, reduced effective catalyzed reaction space, increased operation easier and wasted effective reaction volume.
Summary of the invention
The problem existing for prior art, the invention provides a kind of Multi-stage boiling bed hydrogenation process, form a plurality of different operatings interval in the ebullated bed reactor that is provided with internal recycle district, the reaction conditions between each operational zone is different, this operating method can improve feed stock conversion, improves the quality of products.
Multi-stage boiling bed hydrogenation process provided by the invention comprises:
Hydrocarbon feed mixes with hydrogen and from ebullated bed reactor bottom, enters reactor, under hydroprocessing condition, react, wherein said ebullated bed reactor comprises two or more internal recycle district, and different internal recycle districts adopt different operational conditions, form between different operational zones.
Described boiling bed hydrogenation reactor comprises the cylinder reactor housing perpendicular to ground, the triphase separator that is positioned at housing internal upper part, guide frame and Liang Ge internal recycle district at least.Internal recycle district described in each comprises cylinder, (without top) taper expansion section and guide frame.Described cylinder is positioned at taper expansion section top, and its lower end is connected with taper expansion section upper end.Described guide frame is the annular protrusion structure that is arranged at reactor wall, and its vertical section along reactor axis is trapezoidal, trilateral or arc.The concrete structure in ebullated bed reactor and internal recycle district can be referring to the record in the applicant's patent CN200910204287.9.According to the requirement of the aspect ratio of reactor and depth of conversion, 2～6 internal recycle districts can be set in reactor, 2～3 internal recycle districts are preferably set, wherein the barrel bore in different internal recycle districts can be identical or different.Can be set respectively adding and decaying catalyst discharge member of live catalyst in different internal recycle districts, also can only in reactor head, catalyzer be set and add parts, at reactor bottom, catalyzer discharge member is set.
Described hydrocarbon feed can comprise any petroleum, as crude oil, straight-run gas oil, wax tailings, solvent-deasphalted oils, long residuum and vacuum residuum etc.
According to hydrogenation technique provided by the invention, internal recycle districts different in reactor form different operational zones, and the reaction conditions of each operational zone is different.Each operational zone can be used identical or different catalyzer.
In a kind of embodiment of the inventive method, according to order from bottom to top, the service temperature in each internal recycle district improves gradually, and the temperature range in adjacent internal recycle district is 5～30 ℃.The temperature in each internal recycle district is adjusted by injecting hot hydrogen.Boiling bed hydrogenation reaction conditions is: reaction pressure 6～30MPa, and temperature of reaction is 350～500 ℃, air speed is 0.1～5h
-1, hydrogen to oil volume ratio is 400～3000.
According to hydrogenation technique provided by the invention, the active metal of catalyzer can be one or more in nickel, cobalt, molybdenum or tungsten.Carrier can be one or more in aluminum oxide, silicon oxide, aluminium oxide-silicon oxide or titanium oxide.The shape of catalyzer is extrudate or spherical.Catalyst reactor active metallic content (by weight percentage): wherein nickel or cobalt count 0.1%～10% with oxide compound, molybdenum or tungsten count 0.5%～25% with oxide compound, and bulk density is 0.5～0.9g/cm
3, particle size (spherical diameter or bar shaped diameter) is 0.08～1.0mm, specific surface area is 80～300m
2/ g.
Multi-stage boiling bed hydrogenation process of the present invention forms a plurality of internal recycle districts with different operating condition in ebullated bed reactor, by injecting hot hydrogen, adjusts the temperature of reaction between each operational zone.This operating method had both made the feature of itself and ebullated bed combine closely, and can overcome again the shortcoming that ebullated bed reactor exists.As everyone knows, compare with fixed-bed reactor, ebullated bed reactor catalyzer usage quantity is few, and catalyst particles intergranular voidage is large, can process various inferior raw materials, so have the advantages that adaptability to raw material is strong, simultaneously owing to will guaranteeing that catalyzer in reactor, in boiling shape, requires gas-liquid fluid to have certain linear velocity, so the liquid hourly space velocity of ebullated bed reactor is higher, logistics in ebullated bed reactor, in back-mixing state, realizes isothermal operation, can avoid local superheating phenomenon to occur.But because catalyzer is in boiling shape, gas-liquid contacts effect not as the fixed-bed reactor of dense phase loading with solid catalyst, its mass transfer effect is affected, the liquid product of reactor outlet is second-rate, simultaneously due to back-mixing operator scheme, the raw material that part does not have enough time to react, also along with hydrogenated products are got rid of reactor, has affected the transformation efficiency of raw material.Common ebullated bed reactor is all the operating method of single device single dose isothermal, in a reactor, use a kind of catalyzer, whole reactor is in uniform back-mixing state, reactor is realized isothermal operation, this operator scheme is unfavorable for effective utilization of catalyzer, limited the handiness of operation, be also unfavorable for that reactant flow is in deep hydrogenation and the conversion of reactor.Employing is with the ebullated bed reactor in a plurality of internal recycle district, different internal recycle districts adds the catalyzer of identical or different character, and determine rational operational condition according to logistics property and catalyst performance, be conducive to improve the quality of products and the effective rate of utilization of reactor, also greatly increased the handiness of operation.
Compared with prior art, the advantage of Multi-stage boiling bed hydrogenation process of the present invention is:
1, in the different internal recycle district of ebullated bed reactor, adopt different operational conditions to carry out hydrocarbon feed processing, logistics property and catalyst performance and operational condition can be carried out to rational Match, realize deep conversion and the hydro-upgrading of logistics, improve the quality of products and the utilization ratio of reaction compartment.
2, the internal recycle district in a plurality of different operatings interval is set in ebullated bed reactor, can in reactor, forms a plurality of isothermal operations district, make whole ebullated bed reactor operation more flexible.
3, the existence in ebullated bed internal recycle interval has extended the residence time of liquid ingredient in ebullated bed reactor in the rear logistics of reaction, is conducive to increase light oil yield.
4, because ebullated bed reactor is the reactor that back-mixing degree is very high, so conventionally contain the unconverted raw material of part in reactor effluent, a plurality of little internal recycle districts are set, can the conversion so that raw material repeatedly circulates, be conducive to improve transformation efficiency.
5, the internal recycle district of ebullated bed reactor is through reducing and increases the little logistics internal recycle region that guide frame forms, the different zones of not strictly separating, the high activated catalyst on reactor top is along with the increase of metal refining and amount of coke increases its weight, can not meet the active requirement in this region simultaneously, but it can be slipped to the internal recycle district that is positioned at bottom, is conducive to making full use of of catalyst activity.
Accompanying drawing explanation
Fig. 1 is the structure of reactor schematic diagram (Liang Ge internal recycle district is only set) of a kind of embodiment of Multi-stage boiling bed hydrogenation process of the present invention.
Wherein: 1-material inlet pipe, 2-distributing disc, 3-reactor shell, 4-guide frame, 5-triphase separator inner core, 6-triphase separator urceolus, 7-beds, 8-targeting port, 9-live catalyst adds pipe, 10-gas outlet pipe, 11-triphase separator, 12-liquid outlet, 13-triphase separator catalyzer feed opening, 14-cylinder, 15-is without addendum cone shape expansion section, 16-decaying catalyst delivery pipe, 17-internal recycle district I, 18-internal recycle district II.
Embodiment
For further setting forth specific features of the present invention, in connection with accompanying drawing, be illustrated.
In conjunction with Fig. 1, multi-segment fluidized bed reaction process of the present invention is as follows:
After mixing with hot hydrogen, hot hydrocarbon feed enters reactor by opening for feed 1, after gas-liquid distributor 2, enter the effective reaction space of ebullated bed reactor, enter thereupon near distributing disc by guide frame 4, cylinder 14 and the internal recycle district 17 forming without addendum cone shape expansion section 15, being pooled in cylinder 14 fluid channels without addendum cone shape expansion section 15 of the targeting port 8 that logistics forms through guide frame 4 and cylinder, because the cross-sectional area of fluid channel now reduces, so gas-liquid flow velocity is accelerated, fluid is by behind cylinder top, fluid channel moment expansion, gas-liquid flow rate of flow of fluid moment reduces, its ability of carrying solid catalyst reduces, the passage that causes liquid after partial reaction and unconverted raw material and solid catalyst to form with reactor wall along cylinder outer wall flows to downwards into targeting port and mixes with the logistics from reactor lower part to upper reaches, thereby form little internal recycle district 17.The gaseous stream being risen by internal recycle district 17 and Partial Liquid Phase logistics and the catalyzer carrying on a small quantity enter the internal recycle district 18 of next-door neighbour's triphase separator, in internal recycle district 18, also there is above-mentioned heavy constituent and solid catalyst circulation and gaseous stream and Partial Liquid Phase logistics rise phenomenon, the targeting port 8 that the logistics wherein rising surrounds through guide frame 4 enters triphase separator 11, be separated: first gas separated, by gas discharge outlet 10, discharge reactor, the catalyzer separating returns to reaction zone through feed opening 13, and substantially containing the clarified liq logistics of granules of catalyst, by liquid outlet 12, do not discharge reactor.In order in time decaying catalyst to be discharged to reactor and fresh makeup catalyst, can add by the catalyzer on reactor top pipe 9 toward fresh makeup catalyst in reactive system, and by the delivery pipe 16 of reactor lower part, part decaying catalyst be discharged to reactive system.
The different internal recycle district of ebullated bed reactor of the present invention is used different operational conditions to carry out hydrogenation reaction, wherein the operational condition of main regulation and control is temperature of reaction, temperature of reaction between adjacent operational zone is poor is controlled at 5～30 ℃, by controlling to different operating is interval, injects hot hydrogen amount and adjusts.
The operational condition of boiling bed hydrogenation is: reaction pressure is 6～30MPa, is preferably 10～18MPa; Temperature of reaction is 350～500 ℃, is preferably 400～450 ℃; Air speed is 0.1～5h
-1, be preferably 0.5～3h
-1; Hydrogen to oil volume ratio is 400～2000, is preferably 600～1500.
Two different internal recycle districts of ebullated bed reactor can be used the catalyzer of identical or different activity, if use the catalyzer of different activities, internal recycle district from reactor bottom to top is used the activity of catalyzer to increase successively, and the specific surface area of catalyzer increases, and granularity reduces.The active metal of catalyzer can be one or more in nickel, cobalt, molybdenum or tungsten.Carrier can be one or more in aluminum oxide, silicon oxide, aluminium oxide-silicon oxide or titanium oxide.The shape of catalyzer is extrudate or spherical.Catalyst reactor active metallic content (by weight percentage): wherein nickel or cobalt count 0.1%～10% with oxide compound, molybdenum or tungsten count 0.5%～25% with oxide compound, and bulk density is 0.5～0.9g/cm
3, particle size (spherical diameter or bar shaped diameter) is 0.08～1.0mm, specific surface area is 80～300m
2/ g.According to hydrogenation technique provided by the invention, along the engagement sequence of hydrocarbon feed and catalyzer, in internal recycle district, the particle size of catalyzer reduces 0.01～1mm, preferably reduces 0.05～0.5mm; It is 10wt%～500wt% that active metallic content in catalyzer increases progressively ratio, preferably 50wt%～300wt%.
Below in conjunction with embodiment, further the reaction effect of Multi-stage boiling bed hydrogenation process of the present invention is described.
Embodiment 1
The embodiment that the present embodiment carries out poor quality oil processing for the boiling bed hydrogenation reactor using with Liang Ge internal recycle district.Wherein Liang Ge internal recycle district is used respectively the catalyzer of different hydrogenation activities, the catalyst property using near the internal recycle district 17 of reactor lower part and consisting of: nickel 1% (calculating by its oxide compound), tungsten is 4% (calculating by its oxide compound), and bulk density is 0.7g/cm
3, particle diameter is 0.6mm, specific surface area is 90m
2/ g; The catalyst property using near reactor top internal recycle district 18 with consist of: nickel 3% (calculating by its oxide compound), molybdenum 10% (calculating by its oxide compound), bulk density is 0.54g/cm
3, particle diameter is 0.3mm, specific surface area is 220m
2/ g.Wherein internal recycle district 17Yu internal recycle district 18 catalyst filling ratios are 3: 1.
The feedstock property that test is used is carbon residue 18.3wt%, metal content 160 μ g.g
-1, bituminous matter 3wt%, S content 2.5wt%, N content 0.6wt%, is with the unmanageable inferior raw material of ordinary method.
Liang Ge internal recycle district adopts different operational conditions, injects hot hydrogen and adjusts temperature of reaction, its test conditions and the results are shown in Table 1 by inside race way 18.
Embodiment 2
This embodiment 2 is substantially the same manner as Example 1, and difference is that the Liang Ge internal recycle district in reactor is used identical catalyzer, uses catalyzer identical with the catalyzer in internal recycle district 17 in embodiment 1.Reaction conditions and the results are shown in Table 1.
Comparative example 1
This comparative example 1 is substantially the same manner as Example 2, and difference is that Liang Ge internal recycle district is used identical operational condition, its reaction conditions and the results are shown in Table 1.
Table 1 test conditions and test-results
Claims (10)
1. a Multi-stage boiling bed hydrogenation process, heavy hydrocarbon feeds mixes with hydrogen and from ebullated bed reactor bottom, enters reactor, under hydroprocessing condition, react, wherein said ebullated bed reactor comprises two or more internal recycle district, different internal recycle districts adopt different operational conditions, according to order from bottom to top, the service temperature in each internal recycle district improves gradually, and the temperature range in adjacent internal recycle district is 5～30 ℃;
Wherein said internal recycle district comprises cylinder, without addendum cone shape expansion section and guide frame, described cylinder is positioned at without addendum cone shape expansion section top, cylinder lower end is with being connected without addendum cone shape expansion section upper end; Described guide frame is the annular protrusion structure that is arranged at reactor wall, and its vertical section along reactor axis is trilateral, trapezoidal or arc.
2. according to hydrogenation technique claimed in claim 1, it is characterized in that, the temperature in each internal recycle district is adjusted by injecting hot hydrogen.
3. according to hydrogenation technique claimed in claim 1, it is characterized in that, described ebullated bed reactor comprises 2～6 internal recycle districts.
4. according to hydrogenation technique claimed in claim 1, it is characterized in that, what live catalyst was set respectively in different internal recycle districts adds parts and decaying catalyst discharge member.
5. according to hydrogenation technique claimed in claim 1, it is characterized in that, described boiling bed hydrogenation treatment condition are: reaction pressure 6～30MPa, and temperature of reaction is 350～500 ℃, air speed is 0.1～5h
-1, hydrogen to oil volume ratio is 400～3000.
6. according to hydrogenation technique claimed in claim 1, it is characterized in that, the barrel bore in different internal recycle district is identical or different.
7. according to hydrogenation technique claimed in claim 1, it is characterized in that, different internal recycle district is used the hydrogenation catalyst of identical activity or different activities.
8. according to hydrogenation technique claimed in claim 7, it is characterized in that, the internal recycle district from reactor bottom to top is used the activity of catalyzer to increase successively, and granularity reduces.
9. according to hydrogenation technique claimed in claim 8, it is characterized in that, along the engagement sequence of hydrocarbon feed and catalyzer, in internal recycle district, the particle size of catalyzer reduces 0.01～1mm, and it is 10wt%～500wt% that the active metallic content in catalyzer increases progressively ratio.
10. according to hydrogenation technique claimed in claim 9, it is characterized in that, along the engagement sequence of hydrocarbon feed and catalyzer, in internal recycle district, the particle size of catalyzer reduces 0.05～0.5mm, and it is 50wt%～300wt% that the active metallic content in catalyzer increases progressively ratio.
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Citations (4)
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|---|---|---|---|---|
| CN1362477A (en) * | 2001-01-05 | 2002-08-07 | 中国石油化工股份有限公司 | Hydrogenating modification method for heavy and inferior raw oil |
| CN101376092A (en) * | 2007-08-27 | 2009-03-04 | 中国石油化工股份有限公司 | Novel bubbling bed reactor |
| CN101721960A (en) * | 2008-10-29 | 2010-06-09 | 中国石油化工股份有限公司 | Fluidized bed reactor |
| CN102311763A (en) * | 2010-07-07 | 2012-01-11 | 中国石油化工股份有限公司 | Catalyst-graded fluidized bed hydrogenation process |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1172832A (en) * | 1979-09-06 | 1984-08-21 | Hydrocarbon Research, Inc. | Reactor having dual upflow catalyst beds |
| CN100362477C (en) * | 2006-03-10 | 2008-01-16 | 华为技术有限公司 | Method and device for co-ordinating executing sequence facing user function |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1362477A (en) * | 2001-01-05 | 2002-08-07 | 中国石油化工股份有限公司 | Hydrogenating modification method for heavy and inferior raw oil |
| CN101376092A (en) * | 2007-08-27 | 2009-03-04 | 中国石油化工股份有限公司 | Novel bubbling bed reactor |
| CN101721960A (en) * | 2008-10-29 | 2010-06-09 | 中国石油化工股份有限公司 | Fluidized bed reactor |
| CN102311763A (en) * | 2010-07-07 | 2012-01-11 | 中国石油化工股份有限公司 | Catalyst-graded fluidized bed hydrogenation process |
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