CN102344827B - Hydrogenation method for catalytic cracking heavy cycle oil - Google Patents
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Abstract
A hydrogenation method for catalytic cracking heavy cycle oil. The invention includes a protective zone and a hydrogenation reaction zone, wherein the protective zone is filled with an adsorbent which is capable of absorbing catalyst fines of the catalytic cracking, and the hydrogenation reaction zone is filled with hydrogenation protective agent, hydrogenation asphaltene removing catalyst and hydrogenation refining agent; catalytic cracking heavy cycle oil enters into the protective zone first, absorbs most of the catalytic cracking catalyst fines, then is mixed with hydrogen to enter a heater, and is hydrogenated in the hydrogenation reaction zone after heating. According to the invention a protective zone is arranged before the hydrogenation reaction zone to filter most of the catalytic cracking catalyst fines laden in the catalytic cracking heavy cycle oil, so as to protect the main catalyst and realize long-time cycle running. In addition, a protective reactor connected in parallel in the protective zone conducts switch operation under low pressure, low temperature and non-hydro conditions, and is safe, reliable and convenient for application.
Description
Technical field
The present invention relates to a kind of method of refining hydrocarbon ils under the existence of hydrogen, more particularly, is a kind of hydroprocessing process of catalytic cracking heavy oil.
Background technology
Former oil quality along with the continuous increase of Oil extraction amount worse and worse, is mainly manifested in oil density and becomes large, and viscosity uprises, and heavy metal, sulphur, nitrogen, resin and asphalt equal size uprise.At present, the price difference of crude oil with poor quality and high-quality crude is along with the shortage of petroleum resources is also increasing, cause cheap crude oil with poor quality exploitation and working method more and more to receive publicity, that is to say, from crude oil with poor quality, improve as much as possible the yield of lightweight oil, this has brought huge challenge to the processing technology of traditional crude oil.
In the work flow of refinery, the technical way of realizing heavy oil conversion has the technology such as catalytic cracking, hydrocracking and coking.In China, catalytic cracking is because flexibility of operation is good, gasoline yield is high, the low broader applications that obtain of one-time investment.Existing catalytic cracking unit is in order to increase transformation efficiency and the yield of light oil of catalytic cracking, conventionally heavy oil catalytic unit being produced (heavy cycle oil) self circulates in catalytic cracking unit, but because the hydrogen richness of heavy catalytic cycle oil is low, aromaticity content is high, and its cracking effect is unsatisfactory.A big chunk of heavy catalytic cycle oil is converted into coke, has increased revivifier load, has reduced treatment capacity and the petrol and diesel oil product yield of catalytic cracking unit.
If catalytic cracking heavy oil is carried out to hydrotreatment, make the saturated generation naphthenic hydrocarbon of polycyclic aromatic hydrocarbons wherein, the cracking performance of catalytic cracking heavy oil be will greatly improve, thereby transformation efficiency and yield of light oil improved.After polycyclic aromatic hydrocarbons hydrogenation, also can some generate mononuclear aromatics, mononuclear aromatics is difficult for cracking in catalytic cracking unit, but can lose side chain, produces high-octane gasoline.Catalytic cracking heavy oil can also reduce sulphur, nitrogen content after hydrotreatment.The reduction of sulphur content can reduce the sulphur content of catalytically cracked gasoline, reduces the discharge of revivifier SOx.Because nitrogen compound can make the active centre of acidic catalyst cracking catalyst poisoning, activity decreased, transformation efficiency declines, so the reduction of nitrogen content can improve transformation efficiency and the product yield of catalytic cracking heavy oil.
But owing to inevitably can carrying the fine powder of catalytic cracking catalyst in catalytic cracking heavy oil secretly, these fine powders are easy to be deposited between hydrogenation unit granules of catalyst, cause bed pressure drop to rise, thereby force device frequent shutdowns catalyst changeout more, the utilization ratio ，Gei enterprise that greatly reduces device causes larger financial loss.Catalyst dust in catalytic cracking heavy oil is very tiny, generally only has 0.1～50 micron, and the overwhelming majority is 1～20 micron.Although existing hydrotreater has raw material strainer, but its strainer filters object and just removes inert solid particle, make it not stop up hydrogenation catalyst bed, general filtering accuracy is all very low, be 20 microns or 25 microns, and can be subject to holding quantitative limitation during the raw material that contains a large amount of powder in processing.Therefore, the strainer of existing hydrotreater itself is difficult to the effective filtering of these catalytic cracking catalyst dust.
CN1148404A discloses a kind of method that improves hydro carbons quality, this method is the organic solid particle that electrophoresis removes suspension from stock oil, allow stock oil flow through successively one or more containing electrode containers, DC electric field effect by electrode attracts to remove at least 10% inorganic solid particles, is mainly Armco magnetic iron.This method can not remove non magnetic iron class and easy green coke material, therefore the problem that can't avoid hydrogenation unit beds to stop up.
CN1484684A discloses a kind of method of the hydrotreatment heavy hydrocarbon with switchable type guard reactor; the method arranges the guard reactor system that can switch before main reactor; remove beavy metal impurity in raw material and the easy foulant of green coke, reach the object of protection Primary Catalysts.Guard reactor in the method need to be at high temperature, high pressure, face blocked operation under the condition of hydrogen.
Summary of the invention
The object of the invention is to propose on the basis of existing technology a kind of hydrogenation method for catalytic cracking heavy cycle oil with guard reactor system; adopt the method can solve cost-effectively the problem that catalytic cracking heavy oil hydrogenation unit beds stops up, guarantee the steady running of hydrogenation unit long period.
Hydrogenation method for catalytic cracking heavy cycle oil provided by the invention:
Protective belt and hydroconversion reaction zone are set, and the sorbent material that wherein in protective belt, filling can adsorption catalysis cracking catalyst powder, loads hydrogenation protecting agent, hydrogenation diasphaltene catalyzer and hydrofining agent successively according to the flow direction of reactant flow in hydroconversion reaction zone; Catalytic cracking heavy oil is introduced into protective belt, and most catalytic cracking catalyst powder are fallen in absorption, are then mixed into process furnace with hydrogen, enter hydroconversion reaction zone and carry out hydrotreatment reaction after heating.
Catalytic cracking heavy oil of the present invention refers in catalytic cracking charging and in catalytic cracking unit, is converted into unconverted part outside gas, light-end products and coke.The boiling range of described catalytic cracking heavy oil is 260 ℃～550 ℃.
Described protective belt arranges at least two guard reactors in parallel, and each guard reactor can be used separately, or can cut out separately system.
In a preferred embodiment, protective belt arranges two guard reactors in parallel, first uses guard reactor A, and guard reactor B is cut out outside system.Catalytic cracking heavy oil is introduced into guard reactor A, and most catalytic cracking catalyst powder are fallen in absorption, then after feedstock pump supercharging, are mixed into process furnace with hydrogen, enter hydroconversion reaction zone and carry out hydrotreatment reaction after heating.When the guard reactor A adsorptive capacity that reaches capacity, stop up, while causing guard reactor A pressure reduction to rise, by guard reactor B incision system, guard reactor A is cut out to system simultaneously, and change sorbent material wherein.When the guard reactor B adsorptive capacity that reaches capacity, stop up, while causing pressure reduction to rise, cut out guard reactor B, the guard reactor A of sorbent material has been changed in incision simultaneously.So circulation, until the hydrogenation catalyst of hydroconversion reaction zone reaches life cycle.
The shape of described sorbent material is Raschig ring shape, porous spherical or cellular, and sorbent material one or more inert materials in being selected from aluminum oxide, silicon oxide, aluminium oxide-silicon oxide form, and aperture is 80 order～400 orders.The shape of preferred adsorbent is cellular.
The sorbent material loading in guard reactor can be a kind of, can be also multiple grading loading.Preferably adopt kinds of protect agent grading loading; described protective belt adopts the sorbent material grading loading of multiple different pore size; according to the flow direction of catalytic cracking heavy oil; successively decrease successively in the aperture of described sorbent material; when guaranteeing adsorption effect, make catalytic cracking catalyst powder can be in guard reactor uniform deposition.
The operational condition of described protective belt is pressure 0.2MPa～3.0MPa, and temperature 50 C～200 ℃ are to carry out under the condition of low temperature, low pressure and non-hydrogen.
The reaction conditions of described hydroconversion reaction zone is: hydrogen dividing potential drop 4.0MPa～20.0MPa, preferred 6.0MPa～18.0MPa, 330 ℃～420 ℃ of temperature of reaction, preferably 340 ℃～400 ℃, hydrogen to oil volume ratio 100Nm
3/ m
3～1200Nm
3/ m
3, preferred 200Nm
3/ m
3～1000Nm
3/ m
3, volume space velocity 0.1h
-1～2.0h
-1, preferred 0.2h
-1～1.8h
-1.
The hydroconversion reaction zone integer catalyzer volume of take is benchmark, and the admission space percentage ratio of described hydrogenation protecting agent, the agent of hydrogenation diasphaltene and hydrofining agent is respectively 2%～30%, 5%～50% and 5%～93%.
Described hydrogenation protecting agent is Raschig ring shape; contain a kind of alumina supporter and load on molybdenum and/or the tungsten on this alumina supporter; and nickel and/or cobalt; the gross weight of hydrogenation protecting agent of take is benchmark; and in oxide compound; the content of molybdenum and/or tungsten is 1～10 % by weight, and the content of nickel and/or cobalt is 0.5～3 % by weight.Described aluminum oxide is gama-alumina, and the pore volume of described hydrogenation protecting agent is not less than 0.50ml/g, is preferably not less than 0.60ml/g.This hydrogenation protecting agent has low coke content, low pore volume rate of descent, good activity stability and high intensity.The present invention is in the larger hydrogenation protecting agent of the top of reactor filling voidage; can further remove the tiny catalytic cracking catalyst powder of carrying secretly in raw material; the foulant of easy green coke in while energy effective elimination raw material; the object that reaches protection hydrogenation Primary Catalysts, guarantees hydrotreater long-time running.
Described hydrogenation diasphaltene agent is butterfly type, contain a kind of carrier and load on molybdenum and/or the tungsten on this carrier, and nickel and/or cobalt, the gross weight of hydrogenation diasphaltene agent of take is benchmark, and in oxide compound, the content of molybdenum and/or tungsten is 0.5～18 % by weight, the content of nickel and/or cobalt is 0.3～10 % by weight, carrier is aluminum oxide and optional silicon oxide, and described hydrogenation diasphaltene agent pore volume is not less than 0.60ml/g, is preferably not less than 0.70ml/g.The asphalt content of conventional wax oil hydrogenation refining plant design charging generally should be less than 500 μ g/g, and asphalt content in catalytic cracking heavy oil is in 3000 μ g/g left and right, far above the requirement of conventional Wax Oil Hydrogenation Unit design charging.And, bituminous matter is component the heaviest in catalytic cracking heavy oil, is green coke precursor main in catalytic cracking heavy oil, and molecular dimension often reaches tens more than nanometer, easily cause catalyzer coking and deactivation, affect the work-ing life of catalyst activity stability and shortening catalyzer.Therefore the hydrogenation diasphaltene agent that will load large pore volume after hydrogenation protecting agent, makes the bituminous matter in raw material can obtain partly removing, to reach the object of protection rear portion hydrofining agent.
Described hydrofining agent is butterfly type, contain a kind of carrier and load on molybdenum and/or the tungsten on this carrier, and nickel and/or cobalt, the gross weight of hydrofining agent of take is benchmark, and in oxide compound, the content of molybdenum and/or tungsten is 10～40 % by weight, the content of nickel and/or cobalt is 0.3～7 % by weight, carrier is aluminum oxide and optional silicon oxide, and hydrofining agent pore volume is not less than 0.25ml/g, is preferably not less than 0.30ml/g.After hydrogenation diasphaltene catalyzer, load Hydrobon catalyst, this catalyzer has much higher Polycyclic aromatic hydrocarbons saturated activity, has high desulfurization and denitrification activity simultaneously.
Advantage of the present invention:
1, the present invention arranges protective belt before hydroconversion reaction zone, and most catalytic cracking catalyst powder of carrying secretly in can filtering catalytic cracking heavy oil, reach protection hydrogenation Primary Catalysts, realize the object of long-term operation.
2, guard reactor blocked operation under the condition of low pressure, low temperature, non-hydrogen of parallel connection in protective belt of the present invention, safe and reliable, convenient enforcement.
3, the present invention, by catalytic cracking heavy oil hydrofining, makes the polycyclic aromatic hydrocarbons major part in catalytic cracking heavy oil saturated, has improved the cracking performance of catalytic cracking heavy oil, has significantly improved catalytic cracking liquid yield, realizes the efficient utilization of petroleum resources.In addition, by catalytic cracking heavy oil hydrofining, make sulphur, nitrogen in catalytic cracking heavy oil obtain most removing, can reduce the discharge of For Fcc Regenerator SOx, improve transformation efficiency and the product yield of catalytic cracking heavy oil.
Accompanying drawing explanation
Accompanying drawing is a kind of hydrogenation method for catalytic cracking heavy cycle oil schematic flow sheet provided by the invention.
Embodiment
Below by accompanying drawing, method of the present invention is further described, but not thereby limiting the invention.As shown in the figure: open valve 2 and valve 6, from the catalytic cracking heavy oil of pipeline 1 through valve 2 and valve 6 by guard reactor 4.Now, valve 3 and valve 7 are in closing condition, and guard reactor 5 is outside system.Catalytic cracking heavy oil contacts filtering overwhelming majority catalytic cracking catalyst powder with the sorbent material in guard reactor 4, after raw oil pump 8 superchargings, mixes with the hydrogen from pipeline 9.Then enter process furnace 10, heating enters hydrogenator 12 by pipeline 11, contacts and reacts successively with hydrogenation protecting agent, the agent of hydrogenation diasphaltene with hydrofining agent.Gained hydrogenated oil enters high-pressure separator 14 through pipeline 13 and carries out gas-liquid separation, and liquid product goes out device through pipeline 15, and gas mixes by pipeline 9 and mixes with catalytic cracking heavy oil with new hydrogen from pipeline 18 after compressor 17 compression.When guard reactor 4 adsorptive capacity that reaches capacity, stop up, while causing guard reactor 4 pressure reduction to rise, open valve 3 and valve 7, by guard reactor 5 incision systems.Shut-off valve 2 and valve 6, cut out system by guard reactor 4 simultaneously, changes sorbent material wherein.
The following examples will be further described the present invention, but therefore not limit the present invention.
Raw material used in embodiment is catalytic cracking heavy oil, and main character is in Table 1.From table 1, the polycyclic aromatic hydrocarbon content of catalytic cracking heavy oil A and catalytic cracking heavy oil B is all higher, has reached respectively 29.6% and 37.5%, and bitum content is respectively 2920 μ g/g and 3260 μ g/g, and solid content is respectively 140 μ g/g and 110 μ g/g.
The sorbent material that in embodiment, protective belt adopts is produced by Jiangxi Ying Taokangshun Industrial Co., Ltd., and trade names are BN-01A.This sorbent material is cellular aluminium oxide-silicon oxide, and the present embodiment adopts three kinds of specification combination grading loadings, is respectively 80 orders, 300 orders and 400 orders.
The trade names of the hydrogenation protecting agent adopting in embodiment are respectively RG-10B, by Sinopec catalyzer branch office Chang Ling catalyst plant, are produced.The agent of hydrogenation diasphaltene and hydrofining agent are prepared by laboratory, and physico-chemical property is in Table 2.
Embodiment 1
First catalytic cracking heavy oil A passes through guard reactor A; contact filtering overwhelming majority catalytic cracking catalyst powder with sorbent material; through raw oil pump supercharging, mix laggard process furnace with hydrogen; after heating, enter hydrogenator, contact with hydrofining agent with hydrogenation protecting agent, the agent of hydrogenation diasphaltene successively.Hydrogenated oil carries out gas-liquid separation through high-pressure separator, and liquid product goes out device, and gas mixes with stock oil after mixing with new hydrogen after compressor compression.When the guard reactor A adsorptive capacity that reaches capacity, stop up, while causing pressure reduction to rise, by guard reactor B incision system, guard reactor A is cut out to system simultaneously, and change sorbent material wherein.
In guard reactor in the filling ratio of sorbent material, hydrogenator the character of filling ratio, hydrogenation conditions and the hydrogenated oil of hydrogenation catalyst in Table 3.
From table 3, catalytic cracking heavy oil A is after hydrotreatment, and the polycyclic aromatic hydrocarbons in hydrogenated oil has obtained major part and removed, and has improved the cracking performance of catalytic cracking heavy oil, has significantly improved catalytic cracking liquid yield, realizes the efficient utilization of petroleum resources.Sulphur in hydrogenated oil, nitrogen obtain most removing, and can reduce the discharge of For Fcc Regenerator SOx, improve transformation efficiency and the product yield of catalytic cracking heavy oil.
First catalytic cracking heavy oil B passes through guard reactor A; contact filtering overwhelming majority catalytic cracking catalyst powder with sorbent material; through raw oil pump supercharging, mix laggard process furnace with hydrogen; after heating, enter hydrogenator, contact with hydrofining agent with hydrogenation protecting agent, the agent of hydrogenation diasphaltene successively.Hydrogenated oil carries out gas-liquid separation through high-pressure separator, and liquid product goes out device, and gas mixes with stock oil after mixing with new hydrogen after compressor compression.When the guard reactor A adsorptive capacity that reaches capacity, stop up, while causing pressure reduction to rise, by guard reactor B incision system, guard reactor A is cut out to system simultaneously, and change sorbent material wherein.
In guard reactor in the filling ratio of sorbent material, hydrogenator the character of filling ratio, hydrogenation conditions and the hydrogenated oil of hydrogenation catalyst in Table 3.
From table 3, catalytic cracking heavy oil B is after hydrotreatment, and the polycyclic aromatic hydrocarbons in hydrogenated oil has obtained major part and removed, and has improved the cracking performance of catalytic cracking heavy oil, has significantly improved catalytic cracking liquid yield, realizes the efficient utilization of petroleum resources.Sulphur in hydrogenated oil, nitrogen obtain most removing, and can reduce the discharge of For Fcc Regenerator SOx, improve transformation efficiency and the product yield of catalytic cracking heavy oil.
Table 1
| Stock oil character | Catalytic cracking heavy oil A | Catalytic cracking heavy oil B |
| Density (20 ℃), g/cm 3 | 0.9444 | 0.9398 |
| Sulphur, heavy % | 0.45 | 0.71 |
| Nitrogen, heavy % | 0.32 | 0.16 |
| Carbon, heavy % | 88.11 | 88.37 |
| Hydrogen, heavy % | 11.12 | 10.84 |
| Bituminous matter, μ g/g | 2920 | 3260 |
| Catalyst fines content, μ g/g | 140 | 100 |
| Mass spectrum quality forms, heavy % | ||
| Paraffinic hydrocarbons | 14.6 | 17.6 |
| Total naphthenic hydrocarbon | 33.9 | 27.2 |
| Total aromatic hydrocarbons | 45.5 | 50.6 |
| Wherein: mononuclear aromatics | 15.9 | 13.1 |
| Polycyclic aromatic hydrocarbons | 29.6 | 37.5 |
| Colloid | 6.0 | 4.6 |
Table 2
| Catalyzer | The agent of hydrogenation diasphaltene | Hydrofining agent |
| Chemical constitution, % by weight | ||
| Nickel oxide | 1.1 | 2.8 |
| Molybdenum oxide | 6.2 | / |
| Tungsten oxide 99.999 | / | 26.2 |
| Physical properties: | ||
| Specific surface area, m 2/g | 120 | 170 |
| Pore volume, ml/g | 0.71 | 0.33 |
| Crushing strength, N/ |
11 | 18 |
| Shape | Butterfly type | Butterfly type |
Table 3
Claims (9)
1. a hydrogenation method for catalytic cracking heavy cycle oil, it is characterized in that, protective belt and hydroconversion reaction zone are set, the sorbent material that wherein in protective belt, filling can adsorption catalysis cracking catalyst powder, loads hydrogenation protecting agent, hydrogenation diasphaltene catalyzer and hydrofining agent successively according to the flow direction of reactant flow in hydroconversion reaction zone; Catalytic cracking heavy oil is introduced into protective belt; most catalytic cracking catalyst powder are fallen in absorption; then be mixed into process furnace with hydrogen; after heating, enter hydroconversion reaction zone and carry out hydrotreatment reaction; described protective belt adopts the sorbent material grading loading of multiple different pore size; according to the flow direction of catalytic cracking heavy oil, successively decrease successively in the aperture of described sorbent material.
2. in accordance with the method for claim 1, it is characterized in that, described protective belt arranges at least two guard reactors in parallel, and each guard reactor can be used separately, or can cut out separately system.
3. in accordance with the method for claim 1, it is characterized in that, the shape of described sorbent material is Raschig ring shape, porous spherical or cellular, and sorbent material one or more inert materials in being selected from aluminum oxide, silicon oxide, aluminium oxide-silicon oxide form, and aperture is 80 order～400 orders.
4. in accordance with the method for claim 1, it is characterized in that, the shape of described sorbent material is cellular.
5. in accordance with the method for claim 1, it is characterized in that, the reaction conditions of hydroconversion reaction zone is: hydrogen dividing potential drop 4.0MPa～20.0MPa, 330 ℃～420 ℃ of temperature of reaction, hydrogen to oil volume ratio 100Nm
3/ m
3～1200Nm
3/ m
3, volume space velocity 0.1h
-12.0h
-1.
6. in accordance with the method for claim 1; it is characterized in that; the hydroconversion reaction zone integer catalyzer volume of take is benchmark, and the admission space percentage ratio of described hydrogenation protecting agent, the agent of hydrogenation diasphaltene and hydrofining agent is respectively 2%～30%, 5%～50% and 5%～93%.
7. in accordance with the method for claim 1; it is characterized in that; described hydrogenation protecting agent is Raschig ring shape, contains a kind of alumina supporter and loads on molybdenum and/or the tungsten on this alumina supporter, and nickel and/or cobalt; the gross weight of hydrogenation protecting agent of take is benchmark; and in oxide compound, the content of molybdenum and/or tungsten is 1～10 % by weight, the content of nickel and/or cobalt is 0.5～3 % by weight; described aluminum oxide is gama-alumina, and the pore volume of described hydrogenation protecting agent is not less than 0.50ml/g.
8. in accordance with the method for claim 1, it is characterized in that, described hydrogenation diasphaltene agent is butterfly type, contains a kind of carrier and loads on molybdenum and/or the tungsten on this carrier, and nickel and/or cobalt, the gross weight of hydrogenation diasphaltene agent of take is benchmark, and in oxide compound, the content of molybdenum and/or tungsten is 0.5～18 % by weight, the content of nickel and/or cobalt is 0.3～10 % by weight, carrier is aluminum oxide and optional silicon oxide, and described hydrogenation diasphaltene agent pore volume is not less than 0.60ml/g.
9. in accordance with the method for claim 1, it is characterized in that, described hydrofining agent is butterfly type, contains a kind of carrier and loads on molybdenum and/or the tungsten on this carrier, and nickel and/or cobalt, the gross weight of hydrofining agent of take is benchmark, and in oxide compound, the content of molybdenum and/or tungsten is 10～40 % by weight, the content of nickel and/or cobalt is 0.3～7 % by weight, carrier is aluminum oxide and optional silicon oxide, and hydrofining agent pore volume is not less than 0.25ml/g.
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|---|---|---|---|---|
| CN1313379A (en) * | 2000-03-10 | 2001-09-19 | 中国石油化工集团公司 | Process for hydrogenating poor-quality raw material for catalytic cracking |
| CN1335368A (en) * | 2000-07-24 | 2002-02-13 | 中国石油化工股份有限公司 | Heavy oil and residual oil hydrogenating process |
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| US5744025A (en) * | 1997-02-28 | 1998-04-28 | Shell Oil Company | Process for hydrotreating metal-contaminated hydrocarbonaceous feedstock |
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| CN1313379A (en) * | 2000-03-10 | 2001-09-19 | 中国石油化工集团公司 | Process for hydrogenating poor-quality raw material for catalytic cracking |
| CN1335368A (en) * | 2000-07-24 | 2002-02-13 | 中国石油化工股份有限公司 | Heavy oil and residual oil hydrogenating process |
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