CN106635150A - Method for preparing needle-like coke through catalytic cracking-delayed coking combination process - Google Patents
Method for preparing needle-like coke through catalytic cracking-delayed coking combination process Download PDFInfo
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Abstract
The present invention discloses a method for preparing needle-like coke through a catalytic cracking-delayed coking combination process. The method comprises that catalytic cracking raw material oil enters a catalytic cracking apparatus and is subjected to a reaction, and the generated oil-gas is separated to obtain gas, light oil, middle distillate oil, and catalytic oil slurry; the middle distillate oil and the catalytic oil slurry enter a coking tower, and the oil-gas generated from the reaction is separated to obtain gas, light oil and circulation oil; and when a coking heating furnace is subjected to two-stage heating, the middle distillate oil and the circulation oil enter the coking tower in a mixed manner until the reaction period is ended. According to the present invention, with the method, the large area eurytopic intermediate phase is easily formed, and the coke drawing effect of the eurytopic intermediate phase is easily promoted.
Description
Technical field
The present invention relates to a kind of method for preparing needle coke, the method that more particularly to a kind of Integration of Resid Fcc And Delayed Coking prepares needle coke.
Background technology
The features such as needle coke has CTE low, easy graphitization, is the preferred material for producing high power and ultra high power graphite electrode.In the forming process of needle coke, feedstock oil needs to experience the generation of mesophasespherule, grows up, melts and wait course, develops for wide area mesophase, and line style texture structure is then formed in the presence of air-flow again, and final curing is obtained needle coke.At the coking initial stage, excessive disturbance is avoided the occurrence of inside system, to ensure that mesophasespherule is slow, smoothly develop, the development degree of mesophase directly affects the properties of product of needle coke；In " drawing burnt " stage, system domestic demand will constantly have air-flow at the uniform velocity to escape, wide area mesophase is pulled into into linear structure.
CN103045301 discloses a kind of method for preparing needle coke as raw material with catalytic cracked oil pulp, when delayed coking unit treating capacity reaches it processes the 60%～80% of total amount, oil will be generated separate out remaining cut after gasoline and fully enter delayed coking unit as drawing burnt gas, obtained needle coke that there is high microsteping structure.
CN103184057 discloses a kind of method for preparing homogeneous petroleum needle coke.In initial reaction stage, raw material enters coking tower and forms mesophase liquid crystal the method with lower temperature, and with the raising of furnace temp, raw material mixes successively heavy distillate and intermediate oil enters together coking tower, finally causes temperature in coking tower to reach 510 DEG C.
In needle coke preparation process, the formation for wide area mesophase is needed to provide mitigation, a stable environment, it is to avoid excessive disturbance occurs in reaction system.Conversely, in the pyrogenetic reaction middle and later periods, needing system inside constantly to have air-flow at the uniform velocity to escape again, wide area mesophase is pulled into into line style texture structure.Additionally, in " drawing burnt " stage, generally being fed than mode using systemic circulation, to ensure to have enough gas to escape from system, and the circulation oil mass that coking tower itself is generated tends not to meet the demand of systemic circulation ratio.
The content of the invention
For the deficiencies in the prior art, the present invention provides a kind of method for preparing needle coke.Coking tower by upper feeding mode by using upper feeding and lower feed combinations mode, in initial reaction stage, being effectively eliminated and feeding the disturbance brought to the formation of wide area mesophase in the method；In the reaction the later stage, La Jiao and heat supply can be played dual parts of by lower feeding manner.In order to make up the deficiency that delayed coking circulates oil mass, catalytic cracking unit recycle oil is passed through into delayed coking unit, it is ensured that there are enough air-flows " drawing burnt ".
The present invention provides a kind of method that Integration of Resid Fcc And Delayed Coking prepares needle coke, and methods described includes herein below：
（1）Catalytically cracked stock reacts into catalytic cracking unit, and the oil gas of generation is discharged into catalytic cracking fractionating system from tower top, and gas, light oil, intermediate oil and catalytic slurry are obtained after separation；
（2）Step（1）The intermediate oil and catalytic slurry of generation enters coking tower after coking heater is heated to 430～490 DEG C by the enterprising material mouth of coking tower, the oil gas that reaction is generated is discharged into coker fractionation system from tower top, gas, light oil and recycle oil are obtained after separation, described coking heater adopts the temperature programmed work mode of one section of constant temperature-three sections of constant temperature of-two sections of intensifications, wherein, one section of constant temperature is 430～490 DEG C of 10～25h of constant temperature, and two sections of intensifications rise to 490 DEG C～510 DEG C with the speed of 1～5 DEG C/h；Three sections of constant temperature are 490～510 DEG C of 1～5h of constant temperature；
（3）When coking heater terminates one section of constant temperature starts two sections of intensifications, stopping is fed by enterprising material mouth, step（1）The intermediate oil and step of generation（2）The recycle oil mixing of generation, coking tower is entered Jing after coking heater heating from the lower charging aperture of coking tower, until reaction time terminates, the needle coke of generation is deposited on coking section bottom.
In the inventive method, described coking heater adopts the temperature programmed work mode of one section of constant temperature-three sections of constant temperature of-two sections of intensifications, wherein, one section of constant temperature is 430～490 DEG C of 10～25h of constant temperature, and two sections of intensifications rise to 490～510 DEG C with the speed of 1～5 DEG C/h；Three sections of constant temperature are 490～510 DEG C of 1～5h of constant temperature；When heating furnace is in one section of constant temperature, intermediate oil and catalytic slurry enter coking tower by the enterprising material mouth of coking tower；When heating furnace terminates one section of constant temperature starts two sections of intensifications, stopping is passed through catalytic slurry, and intermediate oil and recycle oil enter coking tower by lower charging aperture, until filling burnt end cycle.
In the inventive method, the coking tower includes cylinder, upper cover and low head, the cylinder from top to bottom sets gradually coking section and packing section, baffle plate is provided between coking section and packing section, the baffle plate is the baffle plate with sieve aperture, and coking section, baffle plate are fixedly connected with packing section by flange, and on the cylinder of the coking section enterprising material mouth is arranged, the low head arranges lower charging aperture, and lower charging aperture is connected with packing section.
In the coking tower, described filler section is highly 1/20～1/2, preferably the 1/20～1/5 of coking tower total height.
In the coking tower, the enterprising material mouth is located at the middle and upper part of the coking section of coking tower, and the bottom of towe apart from coking tower is highly the 3/5～4/5 of total tower height.
In the coking tower, the baffle plate is the baffle plate with sieve aperture, and the baffle plate sieve aperture is shaped as square, and rectangle, triangle, one kind in circle is preferably circular；Slot size is 0.1mm～10mm, it is preferred that 1mm～5mm, sieve aperture is along baffle plate radially in concentric circles distribution, total percent opening of baffle plate is 5%～50%, can be uniform pore openings rate, or non-uniform perforation, preferred non-uniform perforation, when for non-uniform perforation when, gradually increase along baffle plate radial direction screen-aperture from the center of circle or sieve aperture quantity gradually increase.
In the coking tower, filling heatproof, pressure, corrosion resistant inert filler in described filler section, described filler can be one or more in stainless steel, ceramics, inertia silica, its shape can be Raschig ring, Pall ring, it can also be non-porous granulated filler, the Main Function of filler is to make to be difficult coking material along tower radial dispersion, it is to avoid is difficult coking material and concentrates on tower central shaft area.
In the inventive method, step（1）Described catalytically cracked stock is one or more mixing in Conventional catalytic cracking feedstock oil, including atmospheric hydrogenation residual oil, decompression hydrogenated residue, low-sulfur straight-run gas oil, low-sulfur wax tailings etc..Catalytic cracking unit can more than a set of or a set of, reactor, a regenerator at least be included per covering device.Catalytic cracking unit is operated according to this area normal condition：Reaction temperature is 480 DEG C～530 DEG C, and regeneration temperature is 650 DEG C～750 DEG C, and oil ratio is 2～10（Mass ratio）, pressure 0.1MPa～0.5 MPa.Catalyst used by catalytic cracking unit is conventional catalyst, including silica-alumina catalyst, silica-magneia cataslyst, or X-type, Y types, ZSM-5 equimolecular sieve catalysts.
In the inventive method, step（1）The intermediate oil boiling range that described catalytic cracking fractionating system is isolated is 350 DEG C～500 DEG C, and preferably 375 DEG C～490 DEG C, be catalytic slurry than the cut of intermediate oil weight, it is desirable to S ≯ 0.5% of intermediate oil and catalytic slurry（Quality meter）.
In the inventive method, step（2）Described in intermediate oil and catalytic slurry entering coking heater after filtering off except the ash content for wherein containing, ash content ≯ 0.1% contained in the intermediate oil and catalytic slurry after filtration（Quality meter）.
In the inventive method, described coking heater adopts the temperature programmed work mode of one section of constant temperature-three sections of constant temperature of-two sections of intensifications, wherein, one section of constant temperature is 440～480 DEG C of 12～18h of constant temperature；Two sections of intensifications rise to 490～510 DEG C with the speed of 1～5 DEG C/h；Three sections of constant temperature are 495 DEG C～505 DEG C constant temperature 2h～4h.
In the inventive method, the operation temperature of the coking tower is 410 DEG C～505 DEG C, and operating pressure is 0.5 MPa～2MPa, can be constant voltage operation, or change press operation.
In the inventive method, the lower gating location at described coking tower bottom is the position of Conventional delayed coking charging aperture.
In the inventive method, step（2）The recycle oil that described coker fractionation system is isolated is>200 DEG C of distillates, preferably>350 DEG C of distillates.
In the inventive method, step（3）Described recycle oil inlet amount is the 0.1～2 of intermediate oil inlet amount（Mass ratio）.
Compared with prior art, coking tower of the present invention and prepare the method for needle coke and have the advantage that：
1st, at the pyrogenetic reaction initial stage, intermediate oil and catalytic slurry enter coking tower using upper feeding mode, avoid and cause system disturbance excessive due to the entrance of fresh feed, for the generation of mesophasespherule, grow up and melt and there is provided one relax, stable developing environment, be conducive to the formation of large area wide area mesophase；In the pyrogenetic reaction middle and later periods, intermediate oil and recycle oil are passed through from lower charging aperture, due to being both difficult coking, while system viscosity is reduced, as the raising of temperature is escaped in gaseous form, the system internal gas flow of considerably increasing linear velocity in axial direction, may advantageously facilitate " drawing burnt " effect of wide area mesophase.
2nd, the intermediate oil of catalytic cracking unit is without the return mechanism in the form of recycle oil, using one way by by the way of, greatly reduce the burning load of catalytic cracking regenerator, for maintenance system heat balance, the mode of catalytically cracked stock residue can be taken, is conducive to improving the economic benefit of catalytic cracking unit.
3rd, coking tower packing section and baffle plate play good peptizaiton to bottom feed, and to dispersion of the air-flow along tower in the radial direction facilitation is played, and being uniformly distributed for system temperature is improved, and greatly improve the texture structure and performance of coke.In the decoking stage, the flange of coking section, baffle plate and packing section junction is dismantled, remove baffle plate and packing section, then carry out normal de-coking operations.For the coke adhered on filler, can burn in air atmosphere, not interfere with the recycling of filler.
Description of the drawings
Fig. 1 is the schematic flow sheet that Integration of Resid Fcc And Delayed Coking of the present invention prepares needle coke.
Fig. 2 is coking tower structural representation of the present invention.
Fig. 3～Fig. 5 is the optical texture photo that needle coke sample is prepared using the inventive method.
Specific embodiment
The process and effect of the present invention are further illustrated with reference to embodiment.Catalytically cracked stock 1 reacts through catalytic cracking unit 2, and the oil gas 3 of generation enters catalytic cracking fractionating system 4, isolates gas 5, light oil 6, intermediate oil 7 and catalytic slurry 8；Wherein, intermediate oil 7 and catalytic slurry 8 are filtered respectively through filter 11 and 9, miscella 10 is Jing after coking heater is heated to 430 DEG C～490 DEG C of one section of constant temperature stage after removal ash content, coking tower 14A/B is entered from enterprising material mouth, the oil gas 15 of generation is separated through coker fractionation system 16, obtains gas 17, light oil 18 and recycle oil 19；When coking heater enters two sections of temperature rise periods, intermediate oil switches to circuit 13 from 12, mixes with coking recycle oil 19, coking tower is entered from lower charging aperture Jing after coking heater heating, until filling burnt end cycle.
As shown in Figure 2, in the inventive method, the coking tower includes cylinder 1, upper cover 2 and low head 3, the cylinder 1 from top to bottom sets gradually coking section 4 and packing section 5, and baffle plate 9 is provided between coking section 4 and packing section 5, and the baffle plate 9 is the baffle plate with sieve aperture, coking section 4, baffle plate 9 are fixedly connected with packing section 5 by flange 10, enterprising material mouth 8 is set on the cylinder of the coking section 4, and the low head 3 arranges lower charging aperture 7, and lower charging aperture 7 is connected with packing section 5.
Embodiment 1
Using coking tower of the present invention and the combined technical method for preparing needle coke, the wherein enterprising material mouth of coking tower is highly the 4/5 of total tower height apart from bottom of towe, and the height of bottom of towe packing section is the 1/10 of total tower height.
The fundamental property of catalytically cracked stock is shown in Table 1, and the process conditions of catalytic cracking unit are shown in Table 2, and catalyst adopts the trade mark for the catalyst of RICC-1.Catalytic cracking production enters fractionating system, isolates gas, light oil, intermediate oil and catalytic slurry, wherein, through filtration treatment, content of ashes is down to less than 0.1% for intermediate oil and catalytic slurry.In addition, intermediate oil boiling range is 382 DEG C～459 DEG C；Delayed coking generate recycle oil be>355 DEG C of cuts.
The fundamental property of the catalytically cracked stock of table 1
The process conditions of the catalytic cracking unit of table 2
Coking heater is using alternating temperature control, 440 DEG C of holding 16h of initial temperature, then with the ramp of 4 DEG C/h to 505 DEG C of holding 3h.When furnace outlet temperature is 440 DEG C of constant temperature, the intermediate oil and catalytic slurry that catalytic cracking unit is generated enters coking tower from enterprising material mouth；When heating furnace is in the temperature programming stage, stopping is passed through catalytic slurry, and the recycle oil that intermediate oil is generated with coking plant enters coking tower from lower charging aperture, until 505 DEG C of constant temperature terminate, wherein, recycle oil inlet amount is 0.5 times of intermediate oil inlet amount.In whole course of reaction, temperature range is 425 DEG C～498 DEG C in coking tower, and pressure is constant for 0.8MPa.The optical texture of the needle coke sample prepared is as shown in Figure 3.
Embodiment 2
Embodiment prepares needle coke using the inventive method, is with the difference of embodiment 1, and delayed coker operation condition is different.
Coking heater is using alternating temperature control, 450 DEG C of holding 13h of initial temperature, then with the ramp of 3 DEG C/h to 505 DEG C of holding 2h.When furnace outlet temperature is 450 DEG C of constant temperature, the intermediate oil and catalytic slurry that catalytic cracking unit is generated enters coking tower from enterprising material mouth；When heating furnace is in the temperature programming stage, stopping is passed through catalytic slurry, and the recycle oil that intermediate oil is generated with coking plant enters coking tower from lower charging aperture, until 505 DEG C of constant temperature terminate, wherein, recycle oil inlet amount is 1 times of intermediate oil inlet amount.In whole course of reaction, temperature range is 433 DEG C～497 DEG C in coking tower, and pressure is constant for 1.1MPa.The optical texture of the needle coke sample prepared is as shown in Figure 4.
Embodiment 3
Embodiment prepares needle coke using the inventive method, is with the difference of embodiment 1, and delayed coker operation condition is different.
Coking heater is using alternating temperature control, 440 DEG C of holding 16h of initial temperature, then with the ramp of 4 DEG C/h to 500 DEG C of holding 2h.When furnace outlet temperature is 440 DEG C of constant temperature, the intermediate oil and catalytic slurry that catalytic cracking unit is generated enters coking tower from enterprising material mouth；When heating furnace is in the temperature programming stage, stopping is passed through catalytic slurry, and the recycle oil that intermediate oil is generated with coking plant enters coking tower from lower charging aperture, until 500 DEG C of constant temperature terminate, wherein, recycle oil inlet amount is 1 times of intermediate oil inlet amount.In whole course of reaction, temperature range is 433 DEG C～497 DEG C in coking tower, and initial pressure is 1.1MPa, and when furnace outlet temperature rises to 500 DEG C of constant temperature, pressure is down to 0.5MPa in 1h.The optical texture of the needle coke sample prepared is as shown in Figure 5.
Claims (18)
1. a kind of method that Integration of Resid Fcc And Delayed Coking prepares needle coke, methods described includes herein below：
（1）Catalytically cracked stock reacts into catalytic cracking unit, and the oil gas of generation is discharged into catalytic cracking fractionating system from tower top, and gas, light oil, intermediate oil and catalytic slurry are obtained after separation；
（2）Step（1）The intermediate oil and catalytic slurry of generation enters coking tower after coking heater is heated to 430～490 DEG C by the enterprising material mouth of coking tower, the oil gas that reaction is generated is discharged into coker fractionation system from tower top, gas, light oil and recycle oil are obtained after separation, described coking heater adopts the temperature programmed work mode of one section of constant temperature-three sections of constant temperature of-two sections of intensifications, wherein, one section of constant temperature is 430～490 DEG C of 10～25h of constant temperature, and two sections of intensifications rise to 490 DEG C～510 DEG C with the speed of 1～5 DEG C/h；Three sections of constant temperature are 490～510 DEG C of 1～5h of constant temperature；
（3）When coking heater terminates one section of constant temperature starts two sections of intensifications, stopping is fed by enterprising material mouth, step（1）The intermediate oil and step of generation（2）The recycle oil mixing of generation, coking tower is entered Jing after coking heater heating from the lower charging aperture of coking tower, until reaction time terminates, the needle coke of generation is deposited on coking section bottom.
2. in accordance with the method for claim 1, it is characterised in that：The coking tower includes cylinder, upper cover and low head, the cylinder from top to bottom sets gradually coking section and packing section, baffle plate is provided between coking section and packing section, the baffle plate is the baffle plate with sieve aperture, coking section, baffle plate are fixedly connected with packing section by flange, enterprising material mouth is set on the cylinder of the coking section, and the low head arranges lower charging aperture, and lower charging aperture is connected with packing section.
3. in accordance with the method for claim 2, it is characterised in that：Described filler section is highly 1/20～1/2, preferably the 1/20～1/5 of coking tower total height.
4. in accordance with the method for claim 2, it is characterised in that：The enterprising material mouth is located at the middle and upper part of the coking section of coking tower, and the bottom of towe apart from coking tower is highly the 3/5～4/5 of total tower height.
5. in accordance with the method for claim 2, it is characterised in that：The baffle plate is the baffle plate with sieve aperture, and the baffle plate sieve aperture is shaped as square, and rectangle, one kind in triangle or circle is preferably circular.
6. in accordance with the method for claim 5, it is characterised in that：The slot size is 0.1mm～10mm, preferred 1mm～5mm.
7. in accordance with the method for claim 5, it is characterised in that：Along baffle plate radially in concentric circles distribution, total percent opening of baffle plate is 5%～50% to the sieve aperture.
8. in accordance with the method for claim 7, it is characterised in that：The baffle plate using uniform pore openings rate or non-uniform perforation, when for non-uniform perforation when, gradually increase along baffle plate radial direction screen-aperture from the center of circle or sieve aperture quantity gradually increase.
9. in accordance with the method for claim 2, it is characterised in that：Filling heatproof, pressure, corrosion resistant inert filler in described filler section, described filler is one or more in stainless steel, ceramics, inertia silica, and its shape is Raschig ring, Pall ring.
10. in accordance with the method for claim 1, it is characterised in that：Step（1）Described catalytically cracked stock is one or more mixing in Conventional catalytic cracking feedstock oil, including atmospheric hydrogenation residual oil, decompression hydrogenated residue, low-sulfur straight-run gas oil, low-sulfur wax tailings etc..
11. in accordance with the method for claim 1, it is characterised in that：Step（1）Described catalytic cracking unit is more than a set of, reactor, a regenerator at least to be included per covering device.
12. in accordance with the method for claim 1, it is characterised in that：Step（1）Described catalytic cracking unit operating condition：Reaction temperature is 480 DEG C～530 DEG C, and regeneration temperature is 650 DEG C～750 DEG C, and oil ratio is 2～10（Mass ratio）, pressure 0.1MPa～0.5 MPa.
13. in accordance with the method for claim 1, it is characterised in that：Step（1）The intermediate oil boiling range that described catalytic cracking fractionating system is isolated is 350 DEG C～500 DEG C, is catalytic slurry than the cut of intermediate oil weight, it is desirable to S ≯ 0.5% of intermediate oil and catalytic slurry.
14. in accordance with the method for claim 1, it is characterised in that：Step（2）Described in intermediate oil and catalytic slurry entering coking heater after filtering off except the ash content for wherein containing, ash content ≯ 0.1% contained in the intermediate oil and catalytic slurry after filtration.
15. in accordance with the method for claim 1, it is characterised in that：Described coking heater adopts the temperature programmed work mode of one section of constant temperature-three sections of constant temperature of-two sections of intensifications, wherein, one section of constant temperature is 440～480 DEG C of 12～18h of constant temperature；Two sections of intensifications rise to 490～510 DEG C with the speed of 1～5 DEG C/h；Three sections of constant temperature are 495 DEG C～505 DEG C constant temperature 2h～4h.
16. in accordance with the method for claim 1, it is characterised in that：The operation temperature of the coking tower is 410 DEG C～505 DEG C, and operating pressure is 0.5 MPa～2MPa, constant voltage operation or change press operation.
17. in accordance with the method for claim 1, it is characterised in that：Step（2）The recycle oil that described coker fractionation system is isolated is>200 DEG C of distillates, preferably>350 DEG C of distillates.
18. in accordance with the method for claim 1, it is characterised in that：Step（3）Described recycle oil inlet amount is the 0.1～2 of intermediate oil inlet amount.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109777458A (en) * | 2017-11-14 | 2019-05-21 | 中国石油化工股份有限公司 | A kind of preparation method of high-quality needle coke |
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| US5286371A (en) * | 1992-07-14 | 1994-02-15 | Amoco Corporation | Process for producing needle coke |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109777458A (en) * | 2017-11-14 | 2019-05-21 | 中国石油化工股份有限公司 | A kind of preparation method of high-quality needle coke |
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