CN103059984A - Heavy oil processing method adopting catalyst grading - Google Patents
Heavy oil processing method adopting catalyst grading Download PDFInfo
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Abstract
The invention discloses a heavy oil processing method adopting catalyst grading. The method comprises: mixing a heavy oil raw material blended with a homodisperse hydrogenation catalyst with hydrogen, then passing the mixture through an ebullated bed reactor loaded with two solid matters of different specifications in an upflow mode, and leaving them to react under a hydrotreating condition. The two solid matters include stainless steel cages for keeping a fixed bed and a particulate ebullated bed catalyst positioned in the space formed by the stainless steel cages. The solid matter loading mode adopted by the method provided in the invention provides greater porosity than the prior art, increases the dirt-holding capacity of the catalyst bed, and also can prevent the motion state of an ebullition catalyst from being obviously affected when the gas volume or oil volume in the reactor is instable, thus guaranteeing stable operation of the device. The disperse catalyst can be distributed in the voids among the stainless steel cages to achieve a complementary effect with the particulate ebullated bed catalyst.
Description
Technical field
The present invention relates to a kind of heavy oil upgrading method, particularly inert substance or the catalyzer with different states organically combines the method for producing light ends oil.
Background technology
Fast development along with global economy, the rapid growth of lightweight, clean fuel oil demand and former oil quality are worse and worse, restructuring minute content is more and more higher, how effectively to utilize non-renewable petroleum resources, realize to greatest extent lighting of residual oil, production high value petroleum products is the current important topic that faces.
In order to realize the deep processing of heavy oil, full-bodied inferior raw material is processed into high value added product, so that the heavy-oil hydrogenation technology is developed rapidly.At present the heavy-oil hydrogenation technology of comparative maturity is the fixed bed residual hydrogenation, and this technological operation is steady, but this technique is subject to the restriction of feedstock property, and is stricter to index requests such as the metal of raw material, carbon residues.And the boiling bed hydrogenation technique adaptability to raw material is wide; more and more receive people's concern; but this technique will keep the catalyzer in the reactor to be in boiling state; need to be grasped the viscosity of charging under the high-temperature high-voltage reaction state; the character such as density and surface tension; and gas-liquid flow velocity in the reactor there is strict restriction; the gas-liquid flow velocity is crossed the low catalyzer that can not guarantee and is seethed with excitement; the too high meeting of gas-liquid flow velocity goes out reactor with catalyst entrainment; clog downstream pipeline and equipment; this has increased the severity of operation virtually; especially when the device operation is not steady; if device is because accident stops charging; the granules of catalyst meeting deposition of boiling is on the distributing disc of reactor bottom; residual raw material is understood coking carbon deposit on catalyzer and is made catalyst agglomeration in the reactor under the pyroreaction condition; when device enabling again charging, catalyzer can not return to original good boiling state.Present boiling bed hydrogenation technology mainly is divided into two kinds of base types, the one, use with fixed bed hydrogenation substantially similar but require the strong catalyzer of antiwear property, such as H-OIL and LC-Fining technology, this utilization circulation cup and recycle pump with large quantitative response after liquid phase stream loop back reactor, recycle ratio is in the boiling shape up to 10～15 guarantee catalyzer; It is two for using the finely powdered catalyzer, such as the ebullated bed technology of Fushun Petrochemical Research Institute's use with triphase separator, this technical superiority is the recycle pump that does not use accident easily to send out and be difficult to safeguard, rely on reactor gas-liquid flow velocity to keep the catalyzer boiling state, but the physico-chemical property (such as indexs such as particle volume, tap density, skeletal densities) of logistics property and catalyzer is had strict demand.Face quality heavy oil feedstock worse and worse, how to develop a kind of novel process route existing technology is carried out the advantage restructuring, the effective processing that realizes inferior raw material is the technical scheme that is worth discussion.Existing process combination scheme is just according to logistics property, carry out in order flow arrangement, such as ebullated bed and fixed bed combination process, just simply with two kinds of technique series connection, adopt the ebullated bed technology that inferior raw material is carried out hydrogenation or cracking reaction, then hydrogenation distillate or hydrogenation tail oil or the full cut of hydrogenation are sent into fixed bed device and carry out further hydrogenation reaction, this combination process mode fails to give full play to the advantage of two kinds of technology.
US6447671 discloses a kind of combination process process for heavily residuum hydroconversion.Detailed process is: heavy residual oil raw material and hydrogen are mixed into boiling bed hydrogenation cracking reaction district, logistics obtains lighting end and last running through tripping device behind the hydrocracking reaction, and lighting end enters distillate fixed bed hydrogenation processing section or directly enters water distilling apparatus carries out the narrow fraction cutting; After removing the catalyst solid residue, restructuring lease making filtering system enters the heavy oil fixed bed hydrogenating reaction zone; The whole logistics that perhaps flow out from boiling bed hydrogenation cracking reaction district directly enter filtering system, enter heavy oil fixed bed hydrogenating processing reaction district after isolating the catalyst solid material; Reacted all or part of logistics enters water distilling apparatus, cuts out each lighting end and divides with restructuring, and the restructuring that wherein obtains divides to enter catalytic cracking unit or loop back heavy-oil hydrogenation to be processed or the hydrocracking reaction district.This combination process process just requires according to the charging of device and reacted logistics property carries out the coupling of processing means, the characteristics of each Technology is not organically combined to form the process program of an integral body.
US5868923 has introduced and will weigh, residual oil raw material and oil-soluble catalyst and heavy hydrocarbon feeds mixture enter the boiling bed hydrogenation reactor that loaded catalyst is housed through separately pipeline respectively, carries out hydrogenation reaction under the hydrocracking condition of regulation.The adding of this technology introduction catalyzer can be conducive to the ebullated bed smooth operation, reduce energy consumption, but the oil-soluble catalyst add-on can only for 1 ~ 60 μ g/g, add the operational stability that the oil-soluble catalyst compound will affect ebullated bed reactor too much.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of heavy oil upgrading method that adopts the catalyzer grating is provided, the method has merged the operating method of ebullated bed and fixed bed, and introducing Uniform Dispersion catalyzer, can widen the work range of raw material, improve stationarity and the hydrogenation activity of operation, reduced operating severity.
The heavy oil upgrading method of a kind of catalyzer grating provided by the invention comprises the steps:
The heavy oil feedstock that is mixed with Uniform Dispersion type hydrogenation catalyst by the ebullated bed reactor of solid matter is housed, carries out hydrogenation reaction with upflowing with after hydrogen mixes under hydroprocessing condition, remove the metal, sulphur and the nitrogen impurity that contain in the heavy oil; Reaction effluent obtains light ends oil and hydrogenation tail oil through the tripping device separation; Wherein said solid matter comprises the solid matter of two kinds of different sizes, a kind of for keeping the large size solid cage shape thing of fixed bed, another kind is microgranular boiling-bed catalyst, and described microgranular boiling-bed catalyst is positioned in the space of large size cage shape thing formation.
Heavy oil feedstock described in the inventive method can be in viscous crude, long residuum, vacuum residuum, solvent-deasphalted oils, shale oil or the coal tar one or more.Described reactor can be the ebullated bed reactor with circulation cup or triphase separator.
Described decentralized hydrogenation catalyst can be the normally used suspension bed disperse type catalyzer in this area.As being Water-soluble Dispersed catalyzer or oil soluble disperse type catalyzer, the active ingredient of catalyzer is in the metallic elements such as Mo, Ni, Co, W, Cr and Fe one or more, wherein the Water-soluble Dispersed catalyzer is preferably the heteropolyacid salt of above-mentioned metal, and the oil soluble disperse type catalyzer is preferably the naphthenate of above-mentioned metal.The add-on of dispersed catalyst in heavy oil feedstock counted 20～1000 μ g/g with metal.That can use that mixing tank realizes dispersed catalyst and heavy oil feedstock mixes available mixing tank such as multistage shearing pump, colloidal mill, static mixer or ultrasonic oscillator etc.
The solid matter that loads in the ebullated bed reactor comprises the solid matter of two kinds of different sizes, and a kind of for keeping the large size inertia cage of fixed bed, the material of cage shape thing is generally stainless steel.Described Rotating Stainless Steel Cage is preferably the multiaspect cage of the face with 4 above homalographics or unequal-area, each face of cage all has aperture, pitch of holes is 0.5～2 mm, wherein account for the aperture in hole of total hole number 60%～99% less than the diameter of microgranular boiling-bed catalyst, the aperture in 1%～40% hole is more than or equal to the diameter of boiling-bed catalyst.Described microgranular boiling-bed catalyst is wrapped in the Rotating Stainless Steel Cage, and its particle diameter (spherical diameter or bar shaped diameter) is 0.2～1.2mm, and specific surface area is 100～300m
2/ g.Wherein Rotating Stainless Steel Cage is 10～1000 with the equivalent diameter ratio of particle catalyst.Rotating Stainless Steel Cage in the ebullated bed reactor mainly plays and supports and buffer action, is used for the dispersion of particle catalyst, the distribution of gas-liquid logistics, and the reaction heat transmission is for active catalyst forms a plurality of boiling spaces little and that be interconnected.For each fixing reactor, the structure of Rotating Stainless Steel Cage and size are fixing and uniform.
Microgranular boiling-bed catalyst recited above, its carrier can be in aluminum oxide, silicon oxide, aluminium oxide-silicon oxide or the titanium oxide one or more, reactive metal can be in nickel, cobalt, molybdenum or the tungsten one or more.Can comprise by weight percentage such as the catalyzer composition: nickel or cobalt count 1%～20% with oxide compound, and molybdenum or tungsten count 1%～30% with oxide compound.The shape of catalyzer is extrudate or sphere, and bulk density is 0.4～0.9g/cm
3, particle diameter (spherical diameter or bar shaped diameter) is 0.2～1.2mm, specific surface area is 100～300m
2/ g.Wherein the large size Rotating Stainless Steel Cage is 10～1000 with the equivalent diameter ratio of granules of catalyst.The large size Rotating Stainless Steel Cage mainly plays and supports and buffer action, is used for the dispersion of tiny catalyzer, the distribution of gas-liquid logistics, and the reaction heat transmission is for catalyzer forms a plurality of boiling spaces little and that be interconnected.
The described method of hydrotreating of the inventive method, before reactor that Rotating Stainless Steel Cage and particle catalyst are packed into, at first microgranular boiling-bed catalyst not being sealed the cage face from a reservation of Rotating Stainless Steel Cage joins the cage, the loadings of catalyzer is 40%～90% of cage volume in each Rotating Stainless Steel Cage, then this cage face of mechanical close seals such as the method that can adopt welding.The Rotating Stainless Steel Cage that the particulate boiling-bed catalyst will be housed is again packed into the dilute phase type of feed in the reactor.
Hydroprocessing condition described in the present invention is generally: reaction pressure 6～30MPa, 350～480 ℃ of temperature of reaction, volume space velocity 0.1～5.0h during liquid
-1, hydrogen to oil volume ratio (under the standard conditions) 200～2000.Be preferably reaction pressure 12～26MPa, 370～450 ℃ of temperature of reaction, volume space velocity 0.3～3.0 h during liquid
-1Hydrogen to oil volume ratio (under the standard conditions) 300～1000.
Described reaction product tripping device generally comprises the devices such as high-pressure separator, light pressure separator, flashing tower, atmospheric distillation tower and vacuum still.Doing of described light ends oil is generally 330 ℃～385 ℃.Light ends oil can be used as gasoline or diesel oil blending component usually, and hydrogenation tail oil can be used as the charging of catalytic cracking unit or fixed bed residual hydrogenation.
Compared with prior art, the advantage of the inventive method is:
1, adopt the cage shape upholder that keeps fixed bed to hold the array mode of microgranular boiling-bed catalyst, can guarantee that catalyzer is in random motion at relative narrow space under response behaviour, and its kinestate is little to the support of logistics speed and logistics property, flexible operation can require flexible adjusting operation condition according to feedstock property and target product.
2, dispersed catalyst is introduced the reactor that solid matter is housed, can so that the space between the Rotating Stainless Steel Cage also is full of active hydrofining catalyst, play complementary action with microgranular boiling-bed catalyst.
3, in reactor, use two kinds of multi-form solid fills, Rotating Stainless Steel Cage and the microgranular boiling-bed catalyst that is positioned at Rotating Stainless Steel Cage.Wherein a large amount of Rotating Stainless Steel Cages is isolated into some narrow spaces with the useful space of whole reactor, tiny active particles catalyzer keeps the random motion state in the space that basically is isolated and is interconnected, the Design Mode of this kind reactor charge thing can provide the voidage larger than prior art, increases the appearance dirt ability of beds.
4, adopt two kinds of different sizes and in reactor the solid operating method of different motion state, can consider that the physico-chemical property of logistics under high-temperature and high-pressure conditions is on the impact of tiny catalyzer boiling state, in the time of can preventing also simultaneously in the reactor that tolerance or oil mass are unstable, the kinestate of tiny catalyzer of boiling is subject to remarkably influenced, in addition since the excessive catalyzer of tolerance is taken out of or when stopping oil-feed catalyzer subside to form and stop up etc.
Embodiment
The below further specifies method provided by the present invention.
With dispersed catalyst and heavy oil feedstock through mixing tank (such as multistage shearing pump, colloidal mill, static mixer, ultrasonic oscillator) etc. evenly mix, dispersed catalyst can be the normally used suspension bed disperse type catalyzer in this area, can be Water-soluble Dispersed catalyzer or oil soluble disperse type catalyzer, the active ingredient of catalyzer is one or more material in the metallic elements such as Mo, Ni, Co, W, Cr and Fe, wherein water-soluble dispersed catalyst is preferably the heteropolyacid salt of above-mentioned metal, and the oil soluble disperse type catalyzer is preferably the naphthenate of above-mentioned metal.The catalyzer add-on is counted 20～1000 μ g/g with metal.This mixture is after heat exchange or process furnace are preheating to 340～370 ℃, mix with hot hydrogen and to enter the ebullated bed reactor that is filled with solid matter with upflowing and react, this solid matter is the solid matter of two kinds of different size specifications, one is large-sized inert solids, cage shape thing such as stainless steel, be preferably the multiaspect cage shape thing of the face with 4 above homalographics or unequal-area, each face of cage shape thing is provided with some apertures, pitch of holes is 0.5～2mm, wherein account for the aperture in total hole number 60%～99% hole less than the diameter of boiling-bed catalyst, 1%～40% aperture is more than or equal to the diameter of boiling-bed catalyst.Another kind of material is the boiling-bed catalyst of fine particle.The large size solid matter is 10～1000 with the equivalent diameter ratio of granules of catalyst.Before the catalyst loading reactor, the cage face that at first tiny boiling-bed catalyst is not welded from a reservation joins the cage, and the loadings of catalyzer is 40%～90% of cage volume in each cage.Then be welded this cage face.Large size solid that boiling-bed catalyst is housed is packed in the reactor with the dilute phase type of feed.The large size inert solids mainly play and support and buffer action, are used for the dispersion of tiny catalyzer, the distribution of gas-liquid logistics, and the transmission of reaction heat is for catalyzer forms a plurality of boiling spaces little and that be interconnected.The ebullating bed reactor condition is generally: reaction pressure 6～30MPa, and 350～480 ℃ of temperature of reaction, volume space velocity is 0.1～5.0h during liquid
-1, hydrogen to oil volume ratio (under the standard conditions) 200～2000.Be preferably reaction pressure 12～26MPa, 370～450 ℃ of temperature of reaction, volume space velocity 0.3～3.0 h during liquid
-1Hydrogen to oil volume ratio (under the standard conditions) 300～1000.Reaction product obtains light ends oil and hydrogenation tail oil through tripping device, wherein the reaction product tripping device can be the devices such as high-pressure separator, light pressure separator, flashing tower, atmospheric distillation tower and vacuum still, and doing of light ends oil is generally 330 ℃～385 ℃.Wherein light ends can be used as the petrol and diesel oil blend component, and hydrogenation tail oil can be used as the charging of catalytic cracking unit or fixed bed residual hydrogenation.
For further specifying all main points of the present invention, enumerate following examples, but not thereby limiting the invention.
The raw material that test is used is vacuum residuum inferior, and the content of metallic nickel and vanadium is 258 μ g/g, asphalt content 7.2wt%, carbon residue content is 19.5wt%, sulphur content is 3.56%, and nitrogen content is 0.53%, is that conventional fixed bed Residue Hydrotreating Technology is difficult to the directly inferior raw material of processing.
Embodiment
Residual oil raw material evenly mixes through colloidal mill with molybdenum naphthenate, formation contains the parallel feeding of molybdenum naphthenate (in metal) 700 μ g/g, this mixing raw material is after heat exchange or process furnace are preheating to 370 ℃, mix with upflowing with hot hydrogen and to enter reactor, stationary state bed in the reactor is that 6 cage shapes of stainless steel thing of 1.5 centimetres consists of by diameter, the tiny boiling-bed catalyst of 60v% is housed in the cage, it can be in random kinestate under reaction conditions, wherein each face of cage shape thing is provided with some apertures, pitch of holes is 1.2mm, wherein account for the aperture in quantity 99% hole, total aperture less than the diameter of boiling-bed catalyst, the aperture in 1% hole is more than or equal to the diameter of boiling-bed catalyst.Reaction product through high-pressure separation apparatus and atmospheric distillation plant obtain＜180 ℃ gasoline fraction and 180 ~ 350 ℃ diesel oil distillate and 350 ℃ hydrogenation tail oil.Wherein hydrogenation tail oil can be used as the charging of catalytic cracking unit or fixed bed residual hydrogenation.
The boiling bed hydrogenation catalyst that process of the test is used as microspheroidal with the molybdenum-nickel catalyzator of aluminum oxide as carrier, wherein contain MoO in the catalyzer
3Be 12wt%, containing NiO is 3wt%.The bulk density of catalyzer is 0.69g/cm
3, surface-area is 220m
2/ g, the granules of catalyst mean diameter is 0.8mm.Reaction conditions sees Table 1, and test-results sees Table 2.
Comparative example
The catalyzer that comparative example is used and operational process of craft and embodiment are basic identical, and difference is not add in the raw material suspended state disperse type catalyzer.
Test conditions sees Table 1, and experimental result sees Table 2.
Table 1 test conditions
| Project | Embodiment | Comparative example |
| The reaction stagnation pressure, MPa | 16 | 16 |
| Volume space velocity, h -1 | 1.0 | 1.0 |
| Temperature of reaction, ℃ | 420 | 420 |
| Hydrogen-oil ratio, v/v | 600 | 600 |
Table 2 test-results
| Project | Embodiment | Comparative example |
| ＜180 ℃ of gasoline fractions | ? | ? |
| Sulphur/μ g.g -1 | 78 | 142 |
| Nitrogen/μ g.g -1 | 16 | 35 |
| Yield, wt% | 3.2 | 3.5 |
| 180 ~ 350 ℃ of diesel oil distillates | ? | ? |
| Sulphur/μ g.g -1 | 289 | 478 |
| Nitrogen μ g.g -1 | 48 | 79 |
| Yield, wt% | 19.4 | 20.3 |
| 350 ℃ of hydrogenation tail oils | ? | ? |
| Sulphur, wt% | 0.31 | 0.52 |
| Nitrogen, wt% | 0.25 | 0.40 |
| Metal (Ni+V)/μ g.g -1 | 20 | 67 |
| Yield, wt% | 75.2 | 74.1 |
Claims (11)
1. the heavy oil upgrading method of a catalyzer grating comprises the steps:
The heavy oil feedstock that is mixed with Uniform Dispersion type hydrogenation catalyst by the ebullated bed reactor of solid matter is housed, carries out hydrogenation reaction with upflowing with after hydrogen mixes under hydroprocessing condition, remove the metal, sulphur and the nitrogen impurity that contain in the heavy oil; Reaction effluent obtains light ends oil and hydrogenation tail oil through the tripping device separation; Wherein said solid matter comprises the solid matter of two kinds of different sizes, and a kind of another kind is microgranular boiling-bed catalyst in order to keep the large size solid cage of fixed bed, and described microgranular boiling-bed catalyst is positioned in the space of large size cage formation.
2. in accordance with the method for claim 1, it is characterized in that, described decentralized hydrogenation catalyst is the suspension bed disperse type catalyzer, and the add-on of this catalyzer in heavy oil feedstock counted 20～1000 mg/g with metal.
3. in accordance with the method for claim 2, it is characterized in that, described suspension bed catalyzer is Water-soluble Dispersed catalyzer or oil soluble disperse type catalyzer, and the active ingredient of catalyzer is in the metallic elements such as Mo, Ni, Co, W, Cr and Fe one or more.
4. in accordance with the method for claim 1, it is characterized in that, described heavy oil feedstock is one or more in viscous crude, long residuum, vacuum residuum, solvent-deasphalted oils, shale oil or the coal tar.
5. in accordance with the method for claim 1, it is characterized in that, described solid cage is Rotating Stainless Steel Cage, and it has the face of 4 above homalographics or unequal-area, and each face has aperture.
6. in accordance with the method for claim 1, it is characterized in that, the pitch of holes of described aperture is 0.5～2 mm, wherein accounts for the aperture in hole of total hole number 60%～99% less than the diameter of microgranular boiling-bed catalyst, and the aperture in 1%～40% hole is more than or equal to the diameter of boiling-bed catalyst.
7. according to claim 1 or 6 described methods, it is characterized in that, the particle diameter of described microgranular boiling-bed catalyst is 0.2～1.2mm, and the solid cage is 10～1000 with the equivalent diameter ratio of particle catalyst.
8. in accordance with the method for claim 1, it is characterized in that, the carrier of described boiling-bed catalyst is one or more in aluminum oxide, silicon oxide, aluminium oxide-silicon oxide or the titanium oxide, reactive metal is one or more in nickel, cobalt, molybdenum or the tungsten, catalyzer forms and comprises by weight percentage: nickel or cobalt count 1%～20% with oxide compound, and molybdenum or tungsten count 1%～30% with oxide compound.
9. in accordance with the method for claim 1, it is characterized in that, the loadings of boiling-bed catalyst is 40%～90% of solid cage volume in the described solid cage.
10. in accordance with the method for claim 1, it is characterized in that, before reactor that Rotating Stainless Steel Cage and particle catalyst are packed into, at first microgranular boiling-bed catalyst not being sealed the cage face from a reservation of Rotating Stainless Steel Cage joins the cage, then this cage face of mechanical close, the Rotating Stainless Steel Cage that the particulate boiling-bed catalyst will be housed are again packed into the dilute phase type of feed in the reactor.
11. in accordance with the method for claim 1, it is characterized in that, described hydroprocessing condition is: reaction pressure 6～30MPa, and 350～480 ℃ of temperature of reaction, volume space velocity is 0.1～5.0h during liquid
-1, hydrogen to oil volume ratio 200～2000.
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| CN104560158A (en) * | 2013-10-22 | 2015-04-29 | 中国石油化工股份有限公司 | Residual oil hydrogenation method |
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| CN106867573A (en) * | 2015-12-10 | 2017-06-20 | 辽宁石油化工大学 | A kind of method of suspension bed hydrogenation catalyst high efficiency dispersion |
| CN110791311A (en) * | 2018-08-01 | 2020-02-14 | 中国石油化工股份有限公司 | Heavy oil hydrotreating method |
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| CN110791311A (en) * | 2018-08-01 | 2020-02-14 | 中国石油化工股份有限公司 | Heavy oil hydrotreating method |
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| CN103059984B (en) | 2014-10-22 |
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