CN102816595B - Residuum hydrotreatment-catalytic cracking combination technology - Google Patents
Residuum hydrotreatment-catalytic cracking combination technology Download PDFInfo
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Abstract
A residuum hydrotreatment-catalytic cracking combination technology of catalytic cracking recycle oil is characterized in that a material inlet is arranged in front of a metal removal agent bed layer, a desulfurizer bed layer, and a residual carbon removal agent bed layer of a device respectively, residuum and hydrogen enter the device to react through a device raw material port, hydrogenated residuum enters a catalytic cracking device and continuously reacts, one part of the recovery oil of the catalytic cracking device enters a hydrogenation device to react through one or more of four material inlets of a hydrotreatment device, and the residual recovery oil of the catalytic cracking device is cycled to the catalytic cracking device and enters the catalytic cracking device together with the hydrogenated residuum. The technology enables the operations of the residuum hydrotreatment-catalytic cracking combination technology to be flexible and efficient, and has the advantages of prolongation of the operation period of the residuum hydrotreatment device, improvement of the impurity removal rates of residuum hydrogenation products, reduction of the application amount of cold hydrogen, and increase of the yield of light oil having high added values.
Description
Technical field
The present invention relates to a kind of residual hydrocracking and catalytic cracking combined technique.
Background technology
Current, the World Refining processing industry is being faced with the crude resources severe challenge of heaviness and in poor quality day by day.2008,3.42 hundred million tons of crude oil in China amount of finish, wherein heavy crude amount of finish reaches 1.37 hundred million tons, accounts for total amount more than 40%.As everyone knows, residual oil accounts for crude oil ratio conventionally 45～75%, and its character is significantly inferior to the gas wet goods cut that boiling range is lower, and therefore, the pressure that maximization production light-end products and industrial chemicals are made every effort in crude oil deep processing has just dropped on residual oil naturally.
In the optional technological line of residual oil deep processing, residual oil hydrogenation-catalytic cracking combined technological is a kind of well technique.Residual oil removes after the impurity such as metal, sulphur, nitrogen through hydrotreatment, has improved hydrogen richness, can be used as the Rfcc Feedstock of high-quality, and residual oil is transformed completely.This technique has obtained increasing application, but in this combination common process, catalytic cracking recycle oil is to be circulated to further processing in catalytic cracking.Owing to containing polycyclic aromatic hydrocarbons in heavy cycle oil, thereby light oil yield is low, and green coke amount is large, has increased revivifier load, has reduced unit capacity and economic benefit.
US4,713,221 disclose on conventional residual hydrogenation and catalytic cracking combined basis, the heavy cycle oil of catalytic cracking (comprising gas oil catalytic cracking and heavy oil fluid catalytic cracking) is circulated to residual hydrogenation equipment, after mixing with topped crude, carry out hydrogenation, hydrogenated residue enters catalytic cracking unit.The variation that this is little, can make the benefit of one barrel of crude oil of the every processing in refinery have a net increase of 0.29 dollar.
CN1119397C discloses a kind of residual hydrocracking---catalytic cracking combination process, is that residual oil enters residual hydrocracking device together with clarified oil, under hydrogen and hydrogenation catalyst existence, carries out hydrogenation reaction; The hydrogenated residue that obtains of reaction enters catalytic cracking unit, under cracking catalyst exists, carries out cracking reaction, and heavy cycle oil is in catalytic cracking unit internal recycling, react slurry oil be isolated to clarified oil, be back to hydrogenation unit.
CN101210200A discloses a kind of residual hydrocracking and catalytic cracking combination process, steaming together with thing of residual oil, the heavy catalytic cycle oil that removes solid impurity, optional distillate and optional catalytically cracked oil enters residual hydrocracking device, the hydrogenated residue of gained enters catalytic cracking unit together with optional vacuum gas oil, obtains various products; The catalytic cracking turning oil of imurity-removal is circulated to residual hydrocracking device; Catalytically cracked oil is carried out to fractionation by distillation, and be circulated to residual hydrocracking device.
In above combined method, recycle stock is all to enter residual hydrocracking device with raw material residual oil, and inconvenient running condition and oil property according to device adjusted.
Summary of the invention
The object of the invention is to provide the freshening method of a kind of catalytic cracking recycle oil in For Combination Process of Residue Hydrotreating And Catalytic Cracking on existing basis.
Method provided by the invention is:
Before the metal remover bed of conventional residual hydrocracking device, before sweetening agent bed and increase respectively an opening for feed before de-carbon residue beds; catalyst loading still adopts catalyzer grating technology; the multiclass catalyzer of filling including protective material, metal remover, sweetening agent and de-carbon residue agent, different catalysts is seated in different beds.Under hydrogen existence and hydrotreatment reaction conditions, residual oil contacts with residual oil hydrocatalyst and carries out hydrotreatment reaction, and product separation obtains gas, hydrotreated naphtha, hydrogenated diesel oil and hydrogenated residue.
Hydrogenated residue directly or and optional other conventional catalytically cracked stock together with enter catalytic cracking unit and further react, reaction product separation obtains dry gas, liquefied gas, catalytic gasoline, catalytic diesel oil, heavy catalytic cycle oil and slurry oil.Using one or both in heavy catalytic cycle oil and slurry oil as catalytic cracking recycle oil.
Part catalytic cracking recycle oil enters residual hydrogenation equipment processing through removing after solid impurity is processed by one or more in four opening for feeds on residual hydrocracking device, and another part catalytic cracking recycle oil direct cycles to catalytic cracking unit.
Method provided by the invention is described as follows:
(1) residual hydrogenation part
Residual hydrogenation part of the present invention is the same with traditional residual hydrogenation equipment, and different is before metal remover bed, before sweetening agent bed and increase respectively an opening for feed before de-carbon residue beds.The residual oil that uses of device is one or more the mixture in long residuum and vacuum residuum.The catalyzer grating of residual hydrogenation equipment and filling need not change, the multiple catalysts of filling simultaneously including protective material, metal remover, sweetening agent, de-carbon residue catalyzer.Different catalysts is divided bed filling, can load in a reactor, also can be contained in multiple reactors.Catalyzer be generally taking porous inorganic oxide if aluminum oxide is as carrier, group vib and VIII family metal oxide, if W, Mo, Co are or/and the oxide compound of Ni is carrier, optionally add the catalyzer of P, Si or F auxiliary agent.Protective material bed can adopt fixed-bed reactor, also can adopt up-flow reactor, and other beds adopts fixed-bed reactor.
The normal operating condition of residual hydrocracking device is:: hydrogen partial pressure 10～22MPa, temperature of reaction is 310～435 DEG C, volume space velocity 0.1～2.5hr
-1, the volume ratio of hydrogen and residual oil is 500～2000, by weight, catalytic cracking recycle oil is 0.1～45% of raw material residual oil.
Residual oil and hydrogen carry out hydrotreatment reaction from residual hydrogenation equipment opening for feed access to plant, and reaction product can be separated into dry gas, hydrotreated naphtha, hydrogenated diesel oil and hydrogenated residue.
(2) catalytic cracking part
The hydrogenated residue of step (1) gained separately or and optional other conventional catalytically cracked stock together with enter catalytic cracking unit and further react, reaction product separation obtains dry gas, liquefied gas, catalytic gasoline, catalytic diesel oil, heavy catalytic cycle oil and slurry oil.Described catalytic cracking can be catalytic cracking family, as a set of or several covering devices in heavy oil fluid catalytic cracking, catalytic pyrolysis, maximizing iso-paraffins catalytic cracking etc.
The condition of catalytic cracking is: 470～650 DEG C of temperature of reaction, 0.5～5 second reaction times, the weight ratio 3～10 of catalyzer and stock oil, 650～800 DEG C of regeneration temperatures.
(3) catalytic cracking recycle oil
Catalytic cracking recycle oil is one or both in heavy catalytic cycle oil and slurry oil, catalytic cracking recycle oil is 0.1%～45% of raw material residual oil, a part of catalytic cracking recycle oil after removing solid impurity pre-treatment by the one or more access to plant processing in four opening for feeds on residual hydrocracking device; Another part catalytic cracking recycle oil direct cycles to catalytic cracking unit.Recycle stock solid impurity content after pre-treatment need be less than 5ppm, and pretreatment process can be one or more in filtration, distillation, rotating separation etc.The ratio that enters each several part recycle stock determines according to the running condition of oil property and device.For example, in the time that in recycle stock, metal content is higher, can from feed(raw material)inlet and metal remover bed, enter more; When sweetening agent bed and the higher and carbon deposit of de-carbon residue agent bed temperature are when more, can select introducing portion recycle stock from these two beds, reduce temperature of reaction, reduce carbon deposit.
Compared with existing method, method advantage provided by the invention mainly contains:
(1) combined method is more flexible, can adjust neatly according to oil property, device running condition the ratio of various piece recycle stock, increases the treatment capacity of device.
(2) because recycle stock kinematic viscosity is lower, on residual hydrogenation equipment, introduce recycle stock, can improve liquid-flow, distribution in reactor, reduce stock oil viscosity, improve residual oil molecule in catalyzer duct internal diffusion speed, and then improve the impurity removal percentage of device.
(3) because recycle stock aromaticity is higher, on residual hydrogenation equipment, introduce recycle stock, particularly introduce recycle stock by the sweetening agent entrance before entrance and de-carbon residue agent that advances, can improve the aromaticity of oil plant, promote the bitum dissolving of separating out gradually because of hydrogenation in residual oil, reduce the deposition of bituminous matter on catalyzer, and then reduce the coke content on catalyzer.
(4) operation is more flexible, on industrial reactor, can adjust reaction bed temperature by the feeding temperature that regulates each entrance recycle stock, reduces cold hydrogen usage quantity.
Brief description of the drawings
Fig. 1 freshening method flow provided by the invention schematic diagram
Embodiment
Accompanying drawing is freshening method flow schematic diagram provided by the invention; residual hydrocracking device adopts catalyzer grating technology; every kind of catalyzer is contained in different reactors; be respectively protective material reactor, metal remover reactor, reactive desulfurizing agent device and de-residual hydrogen-catalyst reactor, in de-carbon residue hydrogen-catalyst reactor, can also load in the catalyzer such as denitrfying agent except filling takes off carbon residue agent.Respectively before metal remover bed, before sweetening agent bed, before de-carbon residue beds increase a feed entrance.In schematic diagram, different catalysts has been contained in four reactors, also can be contained in practice in one or two or three or five reactors.
After mixing from the residual oil of pipeline 01 with from the hydrogen of pipeline 02, enter residual hydrogenation equipment through preheating, contact with hydrogenation catalyst and carry out hydrotreatment reaction; The product of residual hydrogenation enters tripping device through pipeline 06, obtain dry gas, hydrotreated naphtha, hydrogenated diesel oil, hydrogenated residue, dry gas, hydrotreated naphtha, hydrogenated diesel oil pass through respectively pipeline 07,08,09 caterpillar, and hydrogenated residue enters catalytic cracking unit through pipeline 10.Hydrogenated residue contacts with catalytic cracking catalyst and reacts in catalytic cracking unit, obtain dry gas, liquefied gas, catalytic gasoline, catalytic diesel oil, heavy catalytic cycle oil and slurry oil, dry gas, liquefied gas, catalytically cracked gasoline, catalytic cracking diesel oil are respectively by pipeline 11,12,13,14 caterpillars, and heavy catalytic cycle oil and slurry oil are respectively through 15,16 caterpillars.Using one or both in heavy cycle oil and slurry oil as recycle stock, a part of recycle stock is entered to catalytic cracking unit through pipeline 10 through pipeline 19 together with hydrogenated residue, by the one or more residual hydrogenation equipments that enter in another part recycle stock process pipeline 17, pre-treatment, pipeline 18 process pipelines 03,04,05,20.Can regulate by the feeding temperature of recycle stock the temperature of reaction of each bed.
One liter of four anti-pilot plant of fixed bed residual hydrogenation that the residual hydrogenation equipment using in embodiment and comparative example is produced for Xytel company of the U.S., device totally four reactors, load respectively protective material, metal remover, sweetening agent and de-carbon residue agent.Comparative example is the same with the catalyzer in embodiment, and grating ratio is 5: 40: 30: 25, and catalyzer is that independently develop in laboratory.In order to carry out experiment, before the reactor of filling metal remover, before the reactor of filling sweetening agent and before the reactor of the de-carbon residue agent of filling, increase each opening for feed.Comparative example is the same with the operational condition in embodiment, in table 1.
In embodiment and comparative example, catalytic cracking experiment is carried out on the small riser reactor pilot plant of laboratory designed, designed, the catalyzer that uses for developing voluntarily in laboratory.Comparative example is the same with the operational condition in embodiment, in table 1.
The residual oil using in embodiment and comparative example is Kuwait's long residuum, and catalytic cracking recycle oil is circulated to residual hydrogenation equipment part and carries out fine filtering, and solid impurity content is less than 5ppm.
The main operational condition of table 1
Table 2 test raw material oil (Kuwait's long residuum) main character
| Density (20 DEG C), kg/m 3 | 0.977 |
| S，m％ | 4.43 |
| N，m％ | 0.37 |
| Carbon residue (MCR), m% | 13.2 |
| Metal (Ni+V), ppm | 78.5 |
| Bituminous matter, m% | 4.1 |
| Aromatic hydrocarbon, m% | 40.7 |
Comparative example 1
Kuwait's residual oil enters residual hydrogenation pilot plant together with hydrogen, through residual hydrocracking, reacts according to the condition in table 1, and reaction product is separated into gas, hydrotreated naphtha, hydrogenated diesel oil, hydrogenated residue; Hydrogenated residue enters catalytic cracking unit, react according to the condition in table 1, catalytic cracking production is divided into dry gas, liquefied gas, catalytic gasoline, catalytic diesel oil, heavy catalytic cycle oil and slurry oil, recycle stock adopts heavy cycle oil, recycle stock is all circulated to catalytic cracking unit and enters catalytic cracking unit react together with hydrogenated residue, and product distributes in table 3.
Comparative example 2
Kuwait's residual oil enters residual hydrogenation pilot plant together with hydrogen, through residual hydrocracking, reacts according to the condition in table 1, and reaction product is separated into gas, hydrotreated naphtha, hydrogenated diesel oil, hydrogenated residue; Hydrogenated residue enters catalytic cracking unit, react according to the condition in table 1, catalytic cracking production is divided into dry gas, liquefied gas, catalytic gasoline, catalytic diesel oil, heavy catalytic cycle oil and slurry oil, recycle stock adopts heavy cycle oil, recycle stock is all circulated to residual hydrogenation equipment, enter residual hydrocracking device and react together with residual oil, product distributes in table 3.
Embodiment 1
Kuwait's residual oil enters residual hydrogenation pilot plant together with hydrogen, through residual hydrocracking, reacts according to the condition in table 1, and reaction product is separated into gas, hydrotreated naphtha, hydrogenated diesel oil, hydrogenated residue, hydrogenated residue enters catalytic cracking unit, react according to the condition in table 1, catalytic cracking production is divided into dry gas, liquefied gas, catalytic gasoline, catalytic diesel oil and, heavy catalytic cycle oil and slurry oil, recycle stock adopts heavy cycle oil, 40% recycle stock is circulated to catalytic cracking unit and enters catalytic cracking unit react together with hydrogenated residue, 60% recycle stock is through fine filtering, be equally divided into four parts and hydrogen respectively through residual hydrogenation equipment feed(raw material)inlet, entrance before metal remover bed, entrance before sweetening agent bed, entrance before de-carbon residue beds, enter residual hydrogenation equipment reaction, product distributes in table 3.
Embodiment 2
Kuwait's residual oil enters residual hydrogenation pilot plant together with hydrogen, through residual hydrocracking, reacts according to the condition in table 1, and reaction product is separated into gas, hydrotreated naphtha, hydrogenated diesel oil, hydrogenated residue, hydrogenated residue enters catalytic cracking unit, react according to the condition in table 1, catalytic cracking production is divided into dry gas, liquefied gas, catalytic gasoline, catalytic diesel oil, heavy catalytic cycle oil and slurry oil, recycle stock adopts heavy cycle oil, 40% recycle stock is circulated to catalytic cracking unit and enters catalytic cracking unit react together with hydrogenated residue, 60% recycle stock is through fine filtering, be equally divided into two portions and hydrogen respectively through residual hydrogenation equipment feed(raw material)inlet, entrance before sweetening agent bed, entrance before de-carbon residue beds, enter residual hydrogenation equipment reaction, product distributes in table 3.
By table 3 contrast, we can know, move after 4000 hours, hydrogenated residue character in embodiment 1,2 is obviously better than comparative example 1,2, and the carbon deposit on sweetening agent HDS1, HDS2 and denitrfying agent HDN is starkly lower than comparative example, estimates that runtime is higher 4 months and 2 months than comparative example 1,2 respectively; In catalytic cracking product, embodiment 1,2 every yields approach, and diesel yield is higher 1.7 and 0.4 percentage points respectively than comparative example 1,2, high 1.4 percentage points in steam oil ratio (SOR) comparative example.
Table 3 moves 4000 hours residual hydrogenation product data and catalyst carbon deposit situation
Claims (2)
1. residual hydrocracking and a catalytic cracking combined technique, is characterized in that: step comprises:
(1) residual hydrogenation part
The catalyst grade of residual hydrogenation equipment is joined constant rate, filling protective material, metal remover, sweetening agent and de-carbon residue catalyzer, different catalysts is divided bed filling, load in a reactor or be contained in multiple reactors, catalyzer is taking porous alumina as carrier, and load W, Mo, Co are or/and the oxide compound of Ni, optionally add the catalyzer of P, Si or F auxiliary agent, protective material bed adopts fixed-bed reactor, or adopts up-flow reactor, and other beds adopts fixed-bed reactor;
The operational condition of residual hydrocracking device is: hydrogen partial pressure 10～22MPa, and temperature of reaction is 310～435 DEG C, volume space velocity 0.1～2.5hr-1, the volume ratio of hydrogen and residual oil is 500～2000;
Residual oil and hydrogen carry out hydrotreatment reaction from residual hydrogenation equipment opening for feed access to plant, and reaction product is separated into dry gas, hydrotreated naphtha, hydrogenated diesel oil and hydrogenated residue;
(2) catalytic cracking part
The hydrogenated residue of step (1) gained separately or and optional other conventional catalytically cracked stock together with enter catalytic cracking unit and further react, reaction product separation obtains dry gas, liquefied gas, catalytic gasoline, catalytic diesel oil, heavy catalytic cycle oil and slurry oil; The condition of catalytic cracking is: 470～650 DEG C of temperature of reaction, 0.5～5 second reaction times, the weight ratio 3～10 of catalyzer and stock oil, 650～800 DEG C of regeneration temperatures; Catalyzer is conventional catalytic cracking catalyst;
(3) catalytic cracking recycle oil
Catalytic cracking recycle oil is one or both in heavy catalytic cycle oil and slurry oil, catalytic cracking recycle oil is 0.1～45% of raw material residual oil weight, and a part of catalytic cracking recycle oil enters residual hydrogenation equipment processing by four opening for feeds that are separately positioned on protective material, metal remover, sweetening agent and de-carbon residue beds place on residual hydrocracking device after removing solid impurity pre-treatment; Another part catalytic cracking recycle oil direct cycles to catalytic cracking unit;
Described pretreatment process is one or more in filtration, distillation, rotating separation.
2. according to a kind of residual hydrocracking claimed in claim 1 and catalytic cracking combined technique, it is characterized in that: described residual oil is one or the mixture in long residuum and vacuum residuum.
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2011
- 2011-06-10 CN CN201110156347.1A patent/CN102816595B/en active Active
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| US4713221A (en) * | 1984-05-25 | 1987-12-15 | Phillips Petroleum Company | Crude oil refining apparatus |
| JP2619706B2 (en) * | 1987-11-17 | 1997-06-11 | シエル・インターナショネイル・リサーチ・マーチヤツピイ・ベー・ウイ | Method for producing light hydrocarbon fraction by hydrocracking and catalytic cracking |
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| CN1119397C (en) * | 1999-01-28 | 2003-08-27 | 中国石油化工集团公司 | Hydrogenation and catalystic cracking combined process for residual oil |
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