CN105733650B - Novel coke tower and needle coke production method - Google Patents
Novel coke tower and needle coke production method Download PDFInfo
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- CN105733650B CN105733650B CN201410732135.7A CN201410732135A CN105733650B CN 105733650 B CN105733650 B CN 105733650B CN 201410732135 A CN201410732135 A CN 201410732135A CN 105733650 B CN105733650 B CN 105733650B
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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 and its device for preparing needle coke, more particularly to one kind adopts delay coking process
The coking tower and technique of production needle coke.
Background technology
Needle coke is the main material for producing high power and ultra high power graphite electrode, current domestic production ultra high power stone
Needle coke used by electrode ink relies primarily on import.From the appearance, import needle coke has good silver gray metallic luster,
With excellent streamlined structure；In polarized light microscopy Microscopic observation, import needle coke is on the section parallel to streamlined direction
Nearly all it is in anisotropic threadiness.The physicochemical property of needle coke and its fibre structure have certain relation, with domestic needle-like
Jiao compares, import needle coke on parallel to streamlined direction have more preferable electrical and thermal conductivity performance, lower thermal coefficient of expansion,
It is easier to graphitization.
In needle coke preparation process, raw oil reacts through thermal cracking, thermal polycondensation, generate after mesophasespherule,
Grow up, melt simultaneously, ultimately form wide area mesophase, the now drawing of system burnt operation the pattern of product needle coke, structure are had to
Close important effect.CN1418931 discloses a kind of method that utilization pipe reaction stove prepares needle coke, in advance into reacting furnace
It is 0.2MPa～2MPa to be filled with noble gases to pressure, as the system pressure that carries out of reaction gradually rises, now release reaction
So that reaction pressure is maintained at certain limit, whole course of reaction depends merely on the gas of system release to draw Jiao for gas in stove.Should
Method exists clearly disadvantageous, and in the coking later stage, system thermal cracking, thermal polycondensation reaction are slow, and the light component of generation is significantly reduced,
The air-flow of generation e insufficient to for mesophase to pull into streamlined structure.
Compared with autoclave coking, delayed coking has clear superiority in terms of needle coke is prepared, and material constantly enters from bottom of towe
Enter, the air-flow of generation is continuously moved upwards, to System forming shearing force upwards, force mesophase to be arranged in order along airflow direction
Arrange and solidify, draw burnt effect is significant.The patents such as CN1297979A, CN1132895, CN101302434A are mentioned wax tailings
Loop back coking tower to continue to react, so as to greatly improve the yield of needle coke.Additionally, wax tailings are generally than needle-shape coke raw material oil
Thermal cracking, thermal polycondensation activity it is low, it loops back coke drum and is effectively reduced system viscosity, especially the coking later stage generate oil gas
Under conditions of amount deficiency, recycle oil plays remarkable effect as the burnt gas of drawing.However, generally delayed coking charging aperture is located at bottom of towe
Center, reaction mass sprayed into upwards in coking tower from charging aperture, and the drawing of coking tower center and periphery will certainly be caused burnt
Effect skewness.Central gas stream speed is too fast, causes burnt hole excessive, or even produces whirlpool；Central gas stream speed is excessively slow, coke
It is unobvious that tower periphery draws Jiaozhuo to use.
CN201381301Y discloses a kind of novel feeding port structure of coke drum in needle coke production, and the charging aperture is arranged and divided
Cloth device, material is entered from the bottom of distributor, is sprayed from side, i.e., the radial direction along coke drum sprays, and is uniformly distributed air-flow
In system cross section, be conducive to improving the quality of needle coke.But, if in the high viscosity environment in coking later stage, can not
Ensure that there is the material sprayed from distributor enough power to be evenly distributed in the cross section of system.
In needle coke preparation process, raw oil develops into wide area mesophase after mesophasespherule, with a constant current
The wide area mesophase of dynamic property is drawn into again threadiness in the presence of air-flow, and final solidification obtains the needle-like with streamlined structure
It is burnt.Airflow acting force it is uniform, gentle, be improve needle coke texture structure key factor.
The content of the invention
For the deficiencies in the prior art, it is an object of the present invention to provide a kind of novel coking tower and needle coke production method, adopt
There is flourishing needle-like texture structure with needle coke obtained in coking tower of the present invention and process.
The present invention provides a kind of novel coking tower, and the 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, baffle plate, the baffle plate is provided between coking section and packing section
It is the baffle plate with sieve aperture, baffle center is provided with charging aperture, and coking section is fixedly connected with packing section by flange, and low head is provided with
Enterprising material mouth and lower charging aperture, the enterprising material mouth is connected with the charging aperture of baffle plate by feed pipe and connected with coking section, under
Charging aperture is connected with packing section.
Coking tower of the present invention, packing section is highly 1/20～1/2, preferably the 1/20～1/5 of coking tower total height.
Coking tower of the present invention, the baffle plate is the baffle plate with sieve aperture, and charging aperture, the shape of the baffle plate sieve aperture are left in center
Shape is square, and rectangle, triangle, one kind in circle is preferably circular；Slot size is 0.1mm～10mm, preferably
1mm～5mm, along baffle plate radially in concentric circular distribution, total percent opening of baffle plate is 5%～50% to sieve aperture, can be uniform pore openings rate,
Can also be non-uniform perforation, preferred non-uniform perforation, when for non-uniform perforation when, from the center of circle along baffle plate radius side
Gradually increase to screen-aperture or sieve aperture quantity gradually increases.
Coking tower of the present invention, filling heatproof, pressure, corrosion resistant inert filler, described in described coking tower packing section
Filler can be one or more in rustless steel, ceramics, inertia silicon oxide, and its shape can be Raschig ring, Pall ring, also may be used
To be non-porous granulated filler, the Main Function of filler is to make recycle oil along tower radial dispersion, it is to avoid recycle oil is directly from gear
Hole in the middle part of plate enters coking section.
The present invention provides a kind of needle coke production method, and the needle coke production method adopts coking tower recited above,
Specifically include following content：
（1）After raw oil is heated to 400 DEG C～520 DEG C, carried out instead into the coking section of coking tower by enterprising material mouth
Should, react the oil gas for generating and enter fractionating system after filtering, it is isolated to gas, gasoline fraction, diesel oil distillate and heavy
Oil distillate；
（2）Recycle oil is heated to after 400 DEG C～520 DEG C the packing section that charging aperture under Jing enters coking tower；
（3）When coking tower reaches it processes total amount, stop logical raw oil, switch coking tower, into the burned stage, generate
Needle coke be deposited on coking section.
In needle coke production method of the present invention, step（2）The recycle oil can be in gasoline, diesel oil, wax tailings
One or more, preferably wax tailings.
In needle coke production method of the present invention, step（1）In the gasoline fraction, diesel oil distillate and the heavy oil fraction that obtain
One or more can partly or entirely as recycle oil, and recycle oil is entered after being heated to 400 DEG C～520 DEG C by lower charging aperture
Enter coking tower packing section.
In needle coke production method of the present invention, the step（1）Gasoline fraction, diesel oil distillate and the heavy oil fraction for obtaining
In the coking section that can also partly loop back coking tower for one or more, 400 DEG C～520 are preferably mixed and heated to raw oil
Coking section is entered by enterprising material mouth after DEG C, wherein the recycle oil for looping back coking section is the 10%～200% of raw material oil quality, it is excellent
Select 30%～150%.
In needle coke production method of the present invention, step（2）Described in recycle oil enter packing section from lower charging aperture, further
Coking section is entered after the peptizaiton of filler and baffle plate, the recycle oil entered by lower charging aperture is raw material oil quality
10%～200%, preferably 10%～150%.
In needle coke production method of the present invention, coking tower tower top pressure be 0.5～3.5MPa, preferably 0.5～2.0MPa,
The burnt time is filled for 16～48h, preferably 18～36h.
In needle coke production method of the present invention, when switch coking tower and devoke terminate after, from enterprising material mouth, lower charging aperture to
Coking tower is passed through hot-air or hot oxygen, and the coke remained in two sections of the coking section of coking tower and packing section is burnt, and clears up
Prepare for experiment next time after clean, it may be necessary to draw off hypomere filler, dryouied only with the coke that will be attached on filler.
In needle coke production method of the present invention, described raw oil can be coal tar, the coal tar for removing quinoline insolubles
Oil asphalt, or in desulfurization, ethylene bottom oil, catalytic cracking clarified oil, the ardent slugging oil etc. of de-ash process
One or several mixture.
In needle coke production method of the present invention, step（1）Described raw oil heating adopts alternating temperature programmed heating mode, plus
Hot outlet of still initial temperature is 420～460 DEG C, 1～8h of constant temperature, then with 0.1～10 DEG C/h, the preferred speed liter of 2～5 DEG C/h
To 460～480 DEG C, 1～5h of constant temperature is finally rapidly heated to 500～520 DEG C in 0.5h, 2～4h of constant temperature.
In needle coke production method of the present invention, described recycle ratio is the recycle oil and fresh feed into delayed coking drums
Mass ratio, i.e., the mass ratio of the recycle oil total amount and the fresh feed that enter from upper and lower charging aperture, recycle ratio is 0.1～2.
In needle coke production method of the present invention, step（1）Described in filtering requirement through filtration oil gas in coke powder matter
Amount content 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 arranges packing section by being improved to existing coking tower structure below the coking section of coking tower, makes
Obtain recycle oil and packing section is entered by lower charging aperture, oil gas is evenly distributed through the packing section that is dispersed in of filler, then passes through again
Sieve aperture on baffle plate enters coking section, and because baffle plate adopts non-uniform perforation, from baffle center, radially percent opening gradually increases
Greatly, it is directly proportional to percent opening by the oil and gas content of local sieve aperture, i.e., centre is compared in periphery by the recycle oil that tower wall region is passed through
It is many, so as to do certain compensation to the inhomogeneities that enterprising material mouth feeds, it is to avoid system viscosity is along tower diameter to skewness.Solution
Recycle oil enters the coking section of coking tower together with fresh feed oil from enterprising material mouth in prior art of having determined, in causing coking tower
The viscosity of center portion position is relatively small, and with the carrying out of reaction, the viscosity near coking tower tower wall region increases, and peripheral viscosity is got over
Greatly, the light component in centre spreads to the periphery slower, causes the mobility of peripheral system worse, vicious cycle occurs, causes
Gas draws burnt unobvious by the action effect in tower wall region to periphery.Additionally, the addition of hypomere recycle oil is especially leaned on to system
The region of nearly tower wall, plays good visbreaking and lubrication, then in the presence of the air-flow of center, whole system is along shearing
The direction arrangement of power, the needle coke of generation has good needle-like texture structure, and especially the sample near tower wall region also has
There is good needle-like texture structure.The filler of packing section filling not only plays scattered effect to circulating oil gas, and can be effective
The speed that circulation oil gas sprays upwards is reduced, so as to avoid the direct impact baffle plate of oil gas, is conducive to extending the service life of baffle plate.
Description of the drawings
Fig. 1 is coking tower structural representation of the present invention.
Fig. 2 is coking tower baffle arrangement schematic diagram of the present invention.
Fig. 3 is shone near the polarizing microscope of tower center sample using the method provided by the present invention and delayed coking unit
Piece.
Fig. 4 is using the petrographic microscope photo of the method provided by the present invention and delayed coking unit sample at tower wall.
Fig. 5 is using the stereoscan photograph of the method provided by the present invention and delayed coking unit sample at tower wall.
Fig. 6 is the petrographic microscope photo using Conventional delayed coking device near tower center sample.
Fig. 7 is using the petrographic microscope photo of Conventional delayed coking device sample at tower wall.
Fig. 8 is using the stereoscan photograph of Conventional delayed coking device sample at tower wall.
Specific embodiment
Novel coking tower of the present invention includes cylinder 1, upper cover 2 and low head 3；Upper cover is provided with decoking mouth 4, and cylinder is by upper
Coking section 5 and packing section 6 are set gradually under, baffle plate 7 is provided between coking section and packing section, the baffle plate is with sieve aperture 22
Baffle plate, baffle center is provided with charging aperture 21, and coking section is fixedly connected with packing section by flange 8, and low head is provided with upper feeding
Mouthfuls 9 and lower charging aperture 10, the enterprising material mouth is connected with the charging aperture of baffle plate by feed pipe 11 and connected with coking section, under enter
Material mouth is connected with packing section.
The method and delayed coking unit provided using the present invention prepares needle coke, and the packing section of wherein delayed coking drums is accounted for
The 1/10 of total tower height, baffle plate is non-uniform perforation, and total percent opening is 28%；Using the treated cycle oil in certain refinery
Slurry reacts what is generated as fresh feed>350 DEG C of fractions are recycle oil.For convenience of description, fresh feed oil charging in embodiment
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
It is mixed with the fresh feed of recycle oil oil and enters delayed coking drums from enterprising material mouth 9 after coking heater heating
Coking section 5；Another road recycle oil also passes through the packing section for entering delayed coking drums after coking heater heating from lower charging aperture 10
6, recycle oil enters coking section 5 by the sieve aperture 21 on baffle plate 7 again.Coking heater adopts alternating temperature programme-control, initial temperature
430 DEG C of constant temperature 4h, then with the ramp of 4 DEG C/h to 470 DEG C, in period enterprising material mouth 9 quality of recycle oil be 30%, under
The quality of recycle oil is 20% in charging aperture 10, i.e., now recycle ratio is 0.5, delayed coking tower top pressure 1.5MPa；At 470 DEG C
At a temperature of constant temperature charging 4h, while 50% will be adjusted in the quality of recycle oil in lower charging aperture 10, i.e., now recycle ratio is 0.8；It is permanent
After temperature terminates, 80% will be adjusted in the quality of recycle oil in enterprising material mouth 9, i.e., now recycle ratio is 1.2, then again in 0.5h
2h is rapidly heated to 515 DEG C and is kept, system pressure is adjusted downward to into 0.6MPa in temperature-rise period.In whole coking, prolong
Late the actual total feed of coking tower keeps constant, and total fills the burnt time for 20.5h.Wherein, near the inclined of tower center sample
Light microscope photo is shown in Fig. 3, and the petrographic microscope photo near sample at tower wall is shown in Fig. 4, near the scanning electricity of sample at tower wall
Mirror photo is shown in accompanying drawing 5.
Comparative example 1
Conventional delayed coking device, compared with coking tower used in embodiment 1, institute in comparative example 1 are adopted in comparative example 1
Cancel packing section with coking tower, low head is provided only with a charging aperture.Raw oil used and recycle oil with embodiment 1, equally
Fresh feed oil inlet amount is set to into 1.
The fresh feed oil of contaminated product recycle oil enters delayed coking drums after coking heater heating from bottom.Coking adds
Hot stove using 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, follow by period
Chain rate is 0.5, and delayed coking tower top pressure is 1.5MPa；The constant temperature charging 4h at a temperature of 470 DEG C, while will be adjusted in recycle ratio
0.8；After constant temperature terminates, 1.2 will be adjusted in recycle ratio, be then rapidly heated to 515 DEG C in 0.5h and keep 2h again, heated up
During system pressure is adjusted downward to into 0.6MPa.In whole coking, the actual total feed of delayed coking drums keeps constant,
Total fills the burnt time for 20.5h.Petrographic microscope photo near tower center sample is shown in Fig. 6, and sample is inclined at close tower wall
Light microscope photo is shown in Fig. 7, and the stereoscan photograph near sample at tower wall is shown in Fig. 8.
Claims (23)
1. a kind of coking tower, the coking tower includes cylinder, upper cover and low head；The upper cover is provided with decoking mouth, cylinder
Coking section and packing section are from top to bottom set gradually, baffle plate is provided between coking section and packing section, the baffle plate is with sieve aperture
Baffle plate, baffle center is provided with charging aperture, and coking section is fixedly connected with packing section by flange, low head be provided with enterprising material mouth and
Lower charging aperture, the enterprising material mouth is connected with the charging aperture of baffle plate by feed pipe and connected with coking section, lower charging aperture with fill out
Material section connection.
2. coking tower according to claim 1, it is characterised in that：Described filler section is highly the 1/20 of coking tower total height
～1/2.
3. coking tower according to claim 2, it is characterised in that：Described filler section is highly the 1/20 of coking tower total height
～1/5.
4. coking tower according to claim 1, it is characterised in that：The sieve aperture of the baffle plate is shaped as square, rectangular
Shape, triangle, the one kind in circle.
5. coking tower according to claim 4, it is characterised in that：The sieve aperture of the baffle plate it is generally circular in shape.
6. coking tower according to claim 1, it is characterised in that：The sieve aperture is along baffle plate radially in concentric circular distribution, gear
Total percent opening of plate is 5%～50%, and slot size is 0.1mm～10mm.
7. coking tower according to claim 6, it is characterised in that：The slot size is 1mm～5mm.
8. according to the coking tower described in claim 1, it is characterised in that：The baffle plate is using uniform pore openings rate or non-homogeneous perforate
Rate, when using non-uniform perforation, gradually increase along baffle plate radial direction screen-aperture from the center of circle or sieve aperture quantity by
It is cumulative many.
9. a kind of needle coke production method, the needle coke production method is using described in any claim in claim 1 to 8
Coking tower, comprise the steps：
（1）After raw oil is heated to 400 DEG C～520 DEG C, reacted into the coking section of coking tower by enterprising material mouth, instead
The oil gas that should be generated enters after filtering fractionating system, is isolated to gas, gasoline fraction, diesel oil distillate and mink cell focus and evaporates
Point；
（2）Recycle oil is heated to after 400 DEG C～520 DEG C the packing section that charging aperture under Jing enters coking tower；
（3）When coking tower reaches it processes total amount, stop logical raw oil, switch coking tower, into burned stage, the pin of generation
Shape coke deposits is in coking section.
10. according to the needle coke production method described in claim 9, it is characterised in that：Step（2）The recycle oil be gasoline,
One or more in diesel oil, wax tailings.
11. according to the needle coke production method described in claim 10, it is characterised in that：Step（2）The recycle oil is coking
Wax oil.
12. according to the needle coke production method described in claim 9, it is characterised in that：Step（1）Gasoline fraction, the bavin for obtaining
Partly or entirely as recycle oil, recycle oil is heated to 400 DEG C～520 for one or more in oil distillate and heavy oil fraction
Coking tower packing section is entered by lower charging aperture after DEG C.
13. according to the needle coke production method described in claim 9, it is characterised in that：The step（1）The gasoline for obtaining evaporates
Point, one or more part in diesel oil distillate and heavy oil fraction loop back the coking section of coking tower.
14. according to the needle coke production method described in claim 13, it is characterised in that：The step（1）The gasoline for obtaining evaporates
Point, one or more part in diesel oil distillate and heavy oil fraction and raw oil passes through after being mixed and heated to 400 DEG C～520 DEG C
Enterprising material mouth enters coking section, wherein the recycle oil for looping back coking section is the 10～200% of raw material oil quality.
15. according to the needle coke production method described in claim 14, it is characterised in that：The recycle oil for looping back coking section
For the 30～150% of raw material oil quality.
16. according to the needle coke production method described in claim 9, it is characterised in that：Step（2）Described in recycle oil enter from down
Material mouth enters packing section, further across coking section is entered after the peptizaiton of filler and baffle plate, is entered by lower charging aperture
Recycle oil is the 10～200% of raw material oil quality.
17. according to the needle coke production method described in claim 16, it is characterised in that：The recycle oil entered by lower charging aperture
For the 10～150% of raw material oil quality.
18. according to the needle coke production method described in claim 9, it is characterised in that：The coking tower tower top pressure be 0.5～
3.5MPa, fills the burnt time for 16～48h.
19. according to the needle coke production method described in claim 18, it is characterised in that：The coking tower tower top pressure is 0.5
～2.0MPa, fills the burnt time for 18～36h.
20. according to the needle coke production method described in claim 9, it is characterised in that：The raw oil is to remove quinoline non-soluble
The coal tar of thing, coal tar asphalt, through desulfurization, the ethylene bottom oil of de-ash process, catalytic cracking clarified oil, ardent slugging oil
In one or several.
21. according to the needle coke production method described in claim 9, it is characterised in that：Step（1）Described raw oil adds thermal recovery
With alternating temperature programmed heating mode, furnace outlet initial temperature is 420～460 DEG C, 1～8h of constant temperature, then with 0.1～10 DEG C/h
Speed rise to 460～480 DEG C, 1～5h of constant temperature is finally rapidly heated to 500～520 DEG C in 0.5h, 2～4h of constant temperature.
22. according to the needle coke production method described in claim 21, it is characterised in that：Step（1）Described raw oil heating
Using alternating temperature programmed heating mode, furnace outlet initial temperature is 420～460 DEG C, 1～8h of constant temperature, then with 2～5 DEG C/h
Speed rise to 460～480 DEG C, 1～5h of constant temperature is finally rapidly heated to 500～520 DEG C in 0.5h, 2～4h of constant temperature.
23. according to the needle coke production method described in claim 9, it is characterised in that：Step（1）Described in filtering requirement Jing
Coke powder mass content is down to less than 0.1% in the oil gas for filtering.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410732135.7A CN105733650B (en) | 2014-12-06 | 2014-12-06 | Novel coke tower and needle coke production method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410732135.7A CN105733650B (en) | 2014-12-06 | 2014-12-06 | Novel coke tower and needle coke production method |
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| Publication Number | Publication Date |
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| CN105733650A CN105733650A (en) | 2016-07-06 |
| CN105733650B true CN105733650B (en) | 2017-04-12 |
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| CN201410732135.7A Active CN105733650B (en) | 2014-12-06 | 2014-12-06 | Novel coke tower and needle coke production method |
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| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2868078A1 (en) * | 2004-03-25 | 2005-09-30 | Petroleo Brasileiro Sa | INJECTION CHARGE SYSTEM IN DELAYED COKEFACTION DRUMS |
| CN102585880A (en) * | 2011-12-31 | 2012-07-18 | 太原重工股份有限公司 | High-temperature medium-pressure coking drum |
| CN102732297A (en) * | 2011-04-12 | 2012-10-17 | 中国石油化工股份有限公司 | Method for delaying coking |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8419931B2 (en) * | 2009-01-07 | 2013-04-16 | The University Of Tulsa | Silicone free anti-foaming process and controlled foaming process for petroleum coking |
-
2014
- 2014-12-06 CN CN201410732135.7A patent/CN105733650B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2868078A1 (en) * | 2004-03-25 | 2005-09-30 | Petroleo Brasileiro Sa | INJECTION CHARGE SYSTEM IN DELAYED COKEFACTION DRUMS |
| CN102732297A (en) * | 2011-04-12 | 2012-10-17 | 中国石油化工股份有限公司 | Method for delaying coking |
| CN102585880A (en) * | 2011-12-31 | 2012-07-18 | 太原重工股份有限公司 | High-temperature medium-pressure coking drum |
Non-Patent Citations (1)
| Title |
|---|
| 杨惠谷 等.亚洲第一塔-140万t/a延迟焦化焦炭塔.《化工装备技术》.2005,第26卷(第2期), * |
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