CN105733650A - Novel coke tower and needle coke production method - Google Patents
Novel coke tower and needle coke production method Download PDFInfo
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- CN105733650A CN105733650A CN201410732135.7A CN201410732135A CN105733650A CN 105733650 A CN105733650 A CN 105733650A CN 201410732135 A CN201410732135 A CN 201410732135A CN 105733650 A CN105733650 A CN 105733650A
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Abstract
The present invention relates to a novel coke tower and a needle coke production method. The coke tower includes a cylinder, an upper end socket and a lower end socket. The upper end socket is provided with a decoking port; the cylinder is provided with a coking segment and a filler segment; a baffle plate is between the coking segment and the filler segment; a feed inlet is arranged in the center of the baffle plate; the lower end socket is provided with an upper feed port and a lower feed port; the upper feed port communicates with the feed inlet of the baffle plate through a feed tube; and the lower feed port communicates with the filler segment. The invention also provides a needle coke production method, which employs the coke tower for production of needle coke. The needle coke prepared by the coke tower and process has strong needle texture structure.
Description
Technical field
The present invention relates to a kind of method preparing needle coke and device thereof, particularly relate to a kind of coking tower adopting delay coking process to produce needle coke and technique.
Background technology
Needle coke is the main material producing high power and ultra high power graphite electrode, and the needle coke used by current domestic production ultra high power graphite electrode relies primarily on import.From the appearance, import needle coke has good silver gray metallic luster, has the streamlined structure of excellence；At polarized light microscopy Microscopic observation, import needle coke is nearly all anisotropic threadiness on the cross section being parallel to streamlined direction.The physicochemical property of needle coke and its fibre structure have certain relation, and compared with domestic needle coke, import needle coke is being parallel on streamlined direction to have better electrical and thermal conductivity performance, less thermal coefficient of expansion, is being easier to graphitization.
In needle coke preparation process, raw oil is through thermal cracking, thermal polycondensation reaction, going through mesophasespherule to generate, grow up, melt also, ultimately form wide area mesophase spherule, the pattern of product needle coke, structure are had vital effect by the now burnt operation of drawing of system.CN1418931 discloses a kind of method utilizing pipe reaction stove to prepare needle coke, being filled with noble gas to pressure in advance in reacting furnace is 0.2MPa～2MPa, along with the system pressure that carries out of reaction gradually rises, now the gas in release reaction stove is so that reaction pressure is maintained at certain limit, and whole course of reaction depends merely on the gas of system release to draw Jiao.The method exists clearly disadvantageous, and in the coking later stage, system thermal cracking, thermal polycondensation sluggish, the light component of generation significantly reduces, and the air-flow of generation is not sufficient to mesophase spherule is pulled into streamlined structure.
Compared with autoclave coking, delayed coking has clear superiority in preparing needle coke, and material constantly enters from the bottom of tower, the air-flow produced moves upward continuously, to System forming shearing force upwards, force mesophase spherule along airflow direction ordered arrangement and to solidify, draw burnt effect notable.The patents such as CN1297979A, CN1132895, CN101302434A are all mentioned and wax tailings are looped back coking tower continuation reaction, thus being greatly improved the yield of needle coke.Additionally, wax tailings is generally low than the thermal cracking of needle-shape coke raw material oil, thermal polycondensation activity, it loops back coke drum and is effectively reduced system viscosity, especially the coking later stage generate oil and gas content not enough when, recycle oil plays remarkable effect as drawing burnt gas.But, usual delayed coking charging aperture is positioned at the center at the bottom of tower, and reaction mass upwards sprays in coking tower from charging aperture, and coking tower center will certainly be caused to draw burnt effect skewness with peripheral.Central gas stream speed is too fast, causes burnt hole excessive, even produces whirlpool；Central gas stream speed is excessively slow, and coke drum periphery draws Jiaozhuo with inconspicuous.
CN201381301Y discloses a kind of coke drum in needle coke productionNovelFeeding inlet structure, this charging aperture arranges distributor, and material enters from the bottom of distributor, sprays from the side, namely sprays along the radial direction of coke drum, makes air-flow be evenly distributed on system cross section, is conducive to improving the quality of needle coke.But, if in the high viscosity environment in coking later stage, do not ensure that the material from distributor ejection has enough power and is evenly distributed in the cross section of system.
In needle coke preparation process, raw oil is gone through mesophasespherule and is developed into wide area mesophase spherule, and the wide area mesophase spherule with certain fluidity is drawn into threadiness again under the effect of air-flow, and final solidification obtains the needle coke with streamlined structure.Airflow acting force uniform, mild, is the key factor improving needle coke texture structure.
Summary of the invention
For the deficiencies in the prior art, it is an object of the present invention to provide oneNovelCoking tower and needle coke production method, adopt the needle coke that coking tower of the present invention and process prepare to have the needle-like texture structure of prosperity.
The present invention provides a kind ofNovelCoking tower, described coking tower includes cylinder, upper cover and low head；Upper cover is provided with decoking mouth, cylinder from top to bottom sets gradually coking section and packing section, it is provided with baffle plate between coking section and packing section, described baffle plate is the baffle plate with sieve aperture, baffle center is provided with charging aperture, coking section and packing section and connects by flange is fixing, and low head is provided with upper feeding mouth and lower charging aperture, described upper feeding mouth is connected with the charging aperture of baffle plate by feed pipe and is connected with coking section, and lower charging aperture connects with packing section.
Coking tower of the present invention, packing section height is the 1/20～1/2 of coking tower total height, it is preferred to 1/20～1/5.
Coking tower of the present invention, described baffle plate is the baffle plate with sieve aperture, and charging aperture is left at center, described baffle plate sieve aperture be shaped as square, rectangle, triangle, the one in circle, it is preferred to circular；Slot size is 0.1mm～10mm, preferred 1mm～5mm, sieve aperture is the radially distribution in concentric circular along baffle plate, total percent opening of baffle plate is 5%～50%, can be uniform pore openings rate, it is also possible to be non-uniform perforation, it is preferable that non-uniform perforation, when for non-uniform perforation, it is gradually increased from the center of circle along baffle plate radial direction screen-aperture or sieve aperture quantity increases gradually.
Coking tower of the present invention, heatproof, inert filler pressure, corrosion resistant is filled in described coking tower packing section, described filler can be one or more in rustless steel, pottery, inertia silicon oxide, its shape can be Raschig ring, Pall ring, it can also be the granulated filler of atresia, the Main Function of filler is to make recycle oil along tower radial dispersion, it is to avoid recycle oil directly enters coking section from the hole in the middle part of baffle plate.
The present invention provides a kind of needle coke production method, and described needle coke production method adopts coking tower recited above, specifically includes following content:
(1) after raw oil is heated to 400 DEG C～520 DEG C, the coking section being entered coking tower by upper feeding mouth is reacted, and the oil gas that reaction generates enters fractionating system after filtering, is isolated to gas, gasoline fraction, diesel oil distillate and heavy oil fraction；
(2) recycle oil is heated to enter after 400 DEG C～520 DEG C the packing section of coking tower through lower charging aperture；
(3) when coking tower reaches its process total amount, stopping logical raw oil, switch coking tower, enter the burned stage, the needle coke of generation is deposited on coking section.
In needle coke production method of the present invention, step (2) described recycle oil can be one or more in gasoline, diesel oil, wax tailings, it is preferred to wax tailings.
In needle coke production method of the present invention, one or more in gasoline fraction, diesel oil distillate and heavy oil fraction that step (1) obtains can partly or entirely as recycle oil, and recycle oil enters coking tower packing section by lower charging aperture after being heated to 400 DEG C～520 DEG C.
In needle coke production method of the present invention, one or more in gasoline fraction, diesel oil distillate and heavy oil fraction that described step (1) obtains can also partly loop back the coking section of coking tower, coking section is entered by upper feeding mouth after being preferably mixed and heated to 400 DEG C～520 DEG C with raw oil, wherein loop back recycle oil is raw oil quality the 10%～200% of coking section, it is preferable that 30%～150%.
In needle coke production method of the present invention, recycle oil described in step (2) enters packing section from lower charging aperture, further across entering coking section, recycle oil is raw oil quality 10%～200% entered by lower charging aperture, it is preferred to 10%～150% after the peptizaiton of filler and baffle plate.
In needle coke production method of the present invention, coking tower tower top pressure is 0.5～3.5MPa, it is preferred to 0.5～2.0MPa, and filling the burnt time is 16～48h, it is preferred to 18～36h.
In needle coke production method of the present invention, after switching coking tower decoking terminate, hot-air or hot oxygen is passed into from upper feeding mouth, lower charging aperture to coking tower, the coke of residual in the coking section of coking tower and packing section two sections is burnt, prepare for experiment next time after cleaning out, hypomere filler can be drawn off if desired, dryout only will be attached to the coke on filler.
In needle coke production method of the present invention, described raw oil can be remove the coal tar of quinoline insolubles, coal tar asphalt, it is also possible to is one or several mixture in desulfurization, the ethylene bottom oil of de-ash process, catalytic cracking clarified oil, ardentization residual oil etc..
In needle coke production method of the present invention, raw oil heating described in step (1) adopts alternating temperature programmed heating mode, furnace outlet initial temperature is 420～460 DEG C, constant temperature 1～8h, then with 0.1～10 DEG C/h, it is preferable that the speed of 2～5 DEG C/h rises to 460～480 DEG C, constant temperature 1～5h, finally it is rapidly heated in 0.5h to 500～520 DEG C, constant temperature 2～4h.
In needle coke production method of the present invention, described recycle ratio is the mass ratio of the recycle oil and the fresh feed that enter delayed coking drums, and the mass ratio of the recycle oil total amount namely entered from upper and lower charging aperture and fresh feed, recycle ratio is 0.1～2.
In needle coke production method of the present invention, the coke powder mass content in the oil gas filtered of the filtering requirement described in step (1) is down to less than 0.1%.
Compared with prior art, coking tower of the present invention and needle coke production method have the advantage that
The present invention is by improving existing coking tower structure, coking section at coking tower is arranged below packing section, recycle oil is made to enter packing section by lower charging aperture, oil gas is evenly distributed through the packing section that is dispersed in of filler, then coking section is entered then through the sieve aperture on baffle plate, owing to baffle plate adopts non-uniform perforation, it is gradually increased from baffle center radially percent opening, it is directly proportional to percent opening by the oil and gas content of local sieve aperture, namely the peripheral recycle oil leaning on Ta Bi region to pass into is more than centre, thus the inhomogeneities of upper feeding mouth charging has been done certain compensation, avoid system viscosity along tower diameter to skewness.Solve recycle oil in prior art and enter the coking section of coking tower together with fresh feed oil from upper feeding mouth, the viscosity causing coking tower centre is relatively small, and along with the carrying out of reaction, viscosity near coking tower Ta Bi region increases, peripheral viscosity is more big, and the light component in centre spreads more slow to the periphery, causes that the mobility of peripheral system is worse, vicious cycle occurs, causes that gas draws burnt that periphery is inconspicuous by the action effect in Ta Bi region.In addition, the addition of hypomere recycle oil is to system, especially near the region of tower wall, play good visbreaking and lubrication, again under the effect of center air-flow, whole system arranges along the direction of shearing force, and the needle coke of generation has good needle-like texture structure, especially also has good needle-like texture structure near the sample in Ta Bi region.Circulation oil gas is not only played scattered effect by the filler of packing section filling, and can effectively reduce circulation oil gas and spray up the speed penetrated, thus avoiding the direct impact baffle plate of oil gas, is conducive to extending the service life of baffle plate.
Accompanying drawing explanation
Fig. 1It it is coking tower structural representation of the present inventionFigure。
Fig. 2It it is coking tower baffle arrangement of the present invention signalFigure。
Fig. 3It is adopt the present invention to provide method and delayed coking unit near the polarizing microscope photo of tower center sample.
Fig. 4It is adopt the present invention to provide method and delayed coking unit near the polarizing microscope photo of tower wall place sample.
Fig. 5It is adopt the present invention to provide method and delayed coking unit near the stereoscan photograph of tower wall place sample.
Fig. 6It is adopt Conventional delayed coking device near the polarizing microscope photo of tower center sample.
Fig. 7It is adopt Conventional delayed coking device near the polarizing microscope photo of tower wall place sample.
Fig. 8It is adopt Conventional delayed coking device near the stereoscan photograph of tower wall place sample.
Detailed description of the invention
The present inventionNovelCoking tower includes cylinder 1, upper cover 2 and low head 3；Upper cover is provided with decoking mouth 4, cylinder from top to bottom sets gradually coking section 5 and packing section 6, baffle plate 7 it is provided with between coking section and packing section, described baffle plate is the baffle plate with sieve aperture 22, baffle center is provided with charging aperture 21, coking section and packing section and connects by flange 8 is fixing, and low head is provided with upper feeding mouth 9 and lower charging aperture 10, described upper feeding mouth is connected with the charging aperture of baffle plate by feed pipe 11 and is connected with coking section, and lower charging aperture connects with packing section.
Adopting method provided by the invention and delayed coking unit to prepare needle coke, wherein the packing section of delayed coking drums accounts for the 1/10 of total tower height, and baffle plate is non-uniform perforation, and total percent opening is 28%；Adopting the treated catalytic cracked oil pulp in certain refinery as fresh feed, reaction generates > 350 DEG C of fractions are recycle oil.For convenience of description, in embodiment, fresh feed oil inlet amount is set to 1, and the quality of described recycle oil refers to that recycle oil accounts for the percentage ratio of fresh feed oil quality.
Embodiment 1
The fresh feed oil being mixed with recycle oil enters the coking section 5 of delayed coking drums after coking heater heats from upper feeding mouth 9；Another road recycle oil also passes through the packing section 6 entering delayed coking drums after coking heater heats from lower charging aperture 10, and recycle oil enters coking section 5 again through the sieve aperture 21 on baffle plate 7.Coking heater adopts alternating temperature programme-control, 430 DEG C of constant temperature 4h of initial temperature, then with the ramp of 4 DEG C/h to 470 DEG C, in period upper feeding mouth 9, the quality of recycle oil is 30%, the quality of recycle oil is 20% in lower charging aperture 10, namely now recycle ratio is 0.5, delayed coking tower top pressure 1.5MPa；Constant temperature charging 4h at 470 DEG C of temperature, will be adjusted to 50% in the quality of recycle oil in lower charging aperture 10 simultaneously, and namely now recycle ratio is 0.8；After constant temperature terminates, being adjusted to 80% in upper feeding mouth 9 in the quality of recycle oil, namely now recycle ratio is 1.2, is then rapidly heated in 0.5h to 515 DEG C again and keeps 2h, in temperature-rise period, system pressure being adjusted downward to 0.6MPa.In whole coking, the actual total feed of delayed coking drums remains unchanged, and amounts to that to fill the burnt time be 20.5h.Wherein, see near the polarizing microscope photo of tower center sampleFig. 3, the polarizing microscope photo near tower wall place sample is shown inFig. 4, the stereoscan photograph near tower wall place sample is shown inAccompanying drawing 5。
Comparative example 1
Adopting Conventional delayed coking device in comparative example 1, compared with coking tower used in embodiment 1, in comparative example 1, packing section cancelled by coking tower used, and low head is provided only with a charging aperture.Fresh feed oil inlet amount, with embodiment 1, is set to 1 by raw oil used and recycle oil equally.
The fresh feed oil of contaminated product recycle oil enters delayed coking drums after coking heater heats from bottom.Coking heater adopts alternating temperature programme-control, and 430 DEG C of constant temperature 4h of initial temperature, then with the ramp of 4 DEG C/h to 470 DEG C, period recycle ratio is 0.5, and delayed coking tower top pressure is 1.5MPa；Constant temperature charging 4h at 470 DEG C of temperature, will be adjusted to 0.8 simultaneously in recycle ratio；After constant temperature terminates, recycle ratio will be adjusted to 1.2, be then rapidly heated in 0.5h to 515 DEG C again and keep 2h, in temperature-rise period, system pressure being adjusted downward to 0.6MPa.In whole coking, the actual total feed of delayed coking drums remains unchanged, and amounts to that to fill the burnt time be 20.5h.Polarizing microscope photo near tower center sample is shown inFig. 6, the polarizing microscope photo near tower wall place sample is shown inFig. 7, the stereoscan photograph near tower wall place sample is shown inFig. 8。
Claims (15)
1. a coking tower, described coking tower includes cylinder, upper cover and low head；Described upper cover is provided with decoking mouth, cylinder from top to bottom sets gradually coking section and packing section, it is provided with baffle plate between coking section and packing section, described baffle plate is the baffle plate with sieve aperture, baffle center is provided with charging aperture, coking section and packing section and connects by flange is fixing, and low head is provided with upper feeding mouth and lower charging aperture, described upper feeding mouth is connected with the charging aperture of baffle plate by feed pipe and is connected with coking section, and lower charging aperture connects with packing section.
2. coking tower according to claim 1, it is characterised in that: described packing section height is the 1/20～1/2 of coking tower total height, it is preferred to 1/20～1/5.
3. coking tower according to claim 1, it is characterised in that: the sieve aperture of described baffle plate be shaped as square, rectangle, triangle, the one in circle, it is preferred to circular.
4. the coking tower according to claim 1 or 3, it is characterised in that: described sieve aperture is the radially distribution in concentric circular along baffle plate, and total percent opening of baffle plate is 5%～50%, and slot size is 0.1mm～10mm, it is preferable that 1mm～5mm.
5. the coking tower described in claim 4, it is characterised in that: described baffle plate adopts uniform pore openings rate or non-uniform perforation, when adopting non-uniform perforation, is gradually increased from the center of circle along baffle plate radial direction screen-aperture or sieve aperture quantity increases gradually.
6. a needle coke production method, described needle coke production method adopts the coking tower in claim 1 to 5 described in any claim, including following content:
(1) after raw oil is heated to 400 DEG C～520 DEG C, the coking section being entered coking tower by upper feeding mouth is reacted, and the oil gas that reaction generates enters fractionating system after filtering, is isolated to gas, gasoline fraction, diesel oil distillate and heavy oil fraction；
(2) recycle oil is heated to enter after 400 DEG C～520 DEG C the packing section of coking tower through lower charging aperture；
(3) when coking tower reaches its process total amount, stopping logical raw oil, switch coking tower, enter the burned stage, the needle coke of generation is deposited on coking section.
7. the needle coke production method described in claim 6, it is characterised in that: step (2) described recycle oil is one or more in gasoline, diesel oil, wax tailings, it is preferred to wax tailings.
8. the needle coke production method described in claim 6, it is characterized in that: one or more in gasoline fraction, diesel oil distillate and heavy oil fraction that step (1) obtains are partly or entirely as recycle oil, and recycle oil enters coking tower packing section by lower charging aperture after being heated to 400 DEG C～520 DEG C.
9. the needle coke production method described in claim 6, it is characterized in that: one or more parts in gasoline fraction, diesel oil distillate and heavy oil fraction that described step (1) obtains loop back the coking section of coking tower, coking section is entered by upper feeding mouth after being preferably mixed and heated to 400 DEG C～520 DEG C with raw oil, wherein loop back recycle oil is raw oil quality the 10～200% of coking section, it is preferable that 30～150%.
10. the needle coke production method described in claim 6, it is characterized in that: recycle oil described in step (2) enters packing section from lower charging aperture, further across entering coking section after the peptizaiton of filler and baffle plate, recycle oil is raw oil quality 10～200% entered by lower charging aperture, it is preferred to 10～150%.
11. the needle coke production method described in claim 6, it is characterised in that: described coking tower tower top pressure is 0.5～3.5MPa, it is preferred to 0.5～2.0MPa, and filling the burnt time is 16～48h, it is preferred to 18～36h.
12. the needle coke production method described in claim 6, it is characterised in that: described raw oil is one or several that remove in the coal tar of quinoline insolubles, coal tar asphalt, the ethylene bottom oil processed through desulfurization, de-ash, catalytic cracking clarified oil, ardentization residual oil etc..
13. the needle coke production method described in claim 6, it is characterized in that: the raw oil heating described in step (1) adopts alternating temperature programmed heating mode, furnace outlet initial temperature is 420～460 DEG C, constant temperature 1～8h, then with 0.1～10 DEG C/h, it is preferable that the speed of 2～5 DEG C/h rises to 460～480 DEG C, constant temperature 1～5h, finally it is rapidly heated in 0.5h to 500～520 DEG C, constant temperature 2～4h.
14. the needle coke production method described in claim 6, it is characterized in that: described recycle ratio is the mass ratio of recycle oil and the fresh feed entering delayed coking drums, the mass ratio of the recycle oil total amount namely entered from upper and lower charging aperture and fresh feed, recycle ratio is 0.1～2.
15. the needle coke production method described in claim 6, it is characterised in that: the coke powder mass content in the oil gas filtered of the filtering requirement described in step (1) is down to less than 0.1%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111321003A (en) * | 2018-12-13 | 2020-06-23 | 中国石油化工股份有限公司 | Process for producing needle coke |
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| CN111321003A (en) * | 2018-12-13 | 2020-06-23 | 中国石油化工股份有限公司 | Process for producing needle coke |
| CN111321003B (en) * | 2018-12-13 | 2021-08-31 | 中国石油化工股份有限公司 | Process for producing needle coke |
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