CN110066675A - A kind of method of the high-quality needle coke of continuous production - Google Patents
A kind of method of the high-quality needle coke of continuous production Download PDFInfo
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- CN110066675A CN110066675A CN201910336180.3A CN201910336180A CN110066675A CN 110066675 A CN110066675 A CN 110066675A CN 201910336180 A CN201910336180 A CN 201910336180A CN 110066675 A CN110066675 A CN 110066675A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B55/00—Coking mineral oils, bitumen, tar, and the like or mixtures thereof with solid carbonaceous material
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Abstract
A kind of method that the present invention discloses high-quality needle coke of continuous production, it mainly comprises the steps that and continuously enters in carbonization reaction device (high pressure coke drum) after the heated boiler tube of (1) reaction raw materials is pressurizeed by metering pump, maintaining temperature in carbonization reaction device is 400~500 DEG C, persistently charging 10~for 24 hours, then stops charging the reaction was continued 0~18h.During entire carbonization reaction, the pulse operation of high pressure-low pressure alternative expression is used in carbonization reaction device, reaction pressure variation is in the range of 1.0~6.0MPa；(2) green coke that carbonization reaction device bottom generates is discharged via hydraulic decoking from carbonization reaction device bottom；(3) green coke product is obtained into ripe coke after calcining 2~4h at 1450 DEG C.This method advantageously forms optical texture in the fine fibrous needle coke product of height uniaxial orientation, and in-between phase content reaches 95% or more, CTE≤1.3 × 10 that the graphite electrode of needle coke preparation measures at 25~600 DEG C‑6/℃.Meanwhile the technique has the characteristics that simple process flow, strong operability and can be continuously produced.
Description
Technical field
The present invention designs advanced carbon materials material manufacturing technique field, especially designs a kind of continuous work for producing high-quality needle coke
Skill.
Background technique
Needle coke is a kind of carbon material that purposes is more, and appearance has silver gray metallic luster, and green coke section has
The optical effects of fine-fibrous single shaft distribution, ripe coke have the characteristics of lesser thermal expansion coefficient, higher conductivity, make through it
At high power electrodes, ultra-high power graphite electrode have that resistivity is small, heat shock resistance power is strong, mechanical strength is higher, as a kind of excellent
Matter carbon materials are applied in electric-arc furnace steelmaking by wide hair, efficiency can be improved in metallurgy industry more than 3 times, with China
Steel industry flourishes, and also increases severely with day for the demand of needle coke, according to incompletely statistics, China needs needle-shaped every year
About 200,000 tons of burnt product, but due to the shortcoming in the deficiency and quality of domestic needle coke production capacity, significant portion also needs import,
It can be seen that needle coke has good market prospects, therefore cause numerous scientific research institutions and the concern of scientific research personnel.
Patent CN201110035564.5 discloses a kind of preparation method of acicular petroleum coke: feedstock oil is put into test tube
In, by test tube merging equipped in the tubular reaction vessel of reflux section, it is charged to 2.2~3.5MPa with inert gas, reaction kettle is first put into
It is preheated 5~10 minutes in 300~350 degree of heating equipment, then reaction kettle is heated to 430 degree of carbonization temperature in 5~10 seconds
It~480 degree, is deflated to initial pressure within 10~15 minutes, gas is released after every 10~15 minutes later to initial pressure and measurement is put
Gas volume to charing terminates out；Carbonize 12~18h, system at such a temperature again after gas volume is less than 10~20ml/10min
Obtain needle coke.Even if needle coke above-mentioned and using Gas-driven needle cokes technique preparation ordered structure, and discharging gas is with the time
Define, since needle coke generating process can undergo different phase, the gas flow of generation also can with the increase of char depth and
It is gradually reduced, Gas-driven needle cokes process is interphase system viscosity and the mutually matched process of light component tolerance, intermediate phase viscosity mistake
It is high and it is too low can all influence that Jiao Xiaoguo is drawn using the time as the point for defining deflation to have ignored the variation of intermediate phase viscosity, to intermediate
Mutually develop the later period, a large amount of body shape interphases generate, and increase along with the viscosity of system, at this time due to the deficiency of later period tolerance, most
It will affect eventually and draw Jiao Xiaoguo.
Patent ZL01140582.1 provides a kind of method that needle coke is prepared by Gas-driven needle cokes.In pipe reaction furnace
It is inside put into the copolymerization raw material of coal measures raw material, petroleum raw material or coal measures Yu petroleum raw material, is filled with the inertia of 0.1~2,0MPa
Gas is heated to 480 degree~550 degree of coking temperature after sealing in 2~30s, be more than the 0.2 of original pressure to system pressure
After~1.0MPa, that is, gas is released to 0.2 original~2.0MPa, is then sealed, until the pressure in reacting furnace is no longer super
Until the 0.2~1.0MPa for crossing crude oil pressure.When reaction furnace pressure is constant, continues 4~8h of coking and needle coke is made.Above-mentioned skill
Art is to prepare needle coke using Gas-driven needle cokes technique, and the gas of release is defined with pressure that feedstock oil automatic gas-producing generates, still
Due to interphase nucleation, grow, melt simultaneously, draw the gas production of burnt several different phases different, such as after interphase development
The tolerance of phase is relative to initial reaction stage since the tolerance that the violent cracking of feedstock oil generates will reduce very much, in most cases
The shearing force that light component evolution generates in development later stage system is too small, and the burnt effect of ideal drawing is not achieved to the body interphase in system
Fruit causes needle coke microstructure to cannot achieve uniaxial orientation.In addition, above 2 kinds of similar patents are all batch process methods,
Lack a kind of continuous processing of high-quality needle coke of production (that is, interphase content height and mesophase structure height uniaxial orientation) at present
Method.
Summary of the invention
For the deficiency in terms of acicular coke preparation process, the present invention provides one kind to be suitable for industrial continuous production
Needle coke preparation method, which can produce optical texture in fine-fibrous, the preferably high-quality needle coke of uniaxial orientation degree.
Specific step is as follows for a kind of continuous processing producing high-quality needle coke:
(1) the heated boiler tube of reaction raw materials continuously enters in carbonization reaction device after being pressurizeed by metering pump, maintains carbonization reaction
Temperature is 400~500 DEG C in device, persistently feed 10~for 24 hours, then stop charging the reaction was continued 0~18h.It is anti-in entire charing
During answering, the pulse operation of high pressure-low pressure alternative expression is used in carbonization reaction device, reaction pressure variation is in 1.0~6.0MPa
In the range of；(2) light petroleum gas generated during pyrogenetic reaction obtains liquid by-product through high-pressure separator and low pressure separator
Object and gaseous by-product；(3) green coke that carbonization reaction device bottom generates is arranged via hydraulic decoking process from carbonization reaction device bottom
Out.Green coke obtains high-quality needle coke by 1450 DEG C of 2~4h of calcining.
Raw material used in production needle coke is middle coalite tar, high temperature coal-tar and its fraction, stone in above-mentioned steps (1)
Oily heavy oil fraction, decompression residuum, FCC slurry and above-mentioned raw materials oil solvent-extracted oil.
It is operated in carbonization reaction device using pulsed transformation in above-mentioned steps (1), specifically: when reaction pressure passes through from liter
When pressing through journey and reaching predetermined high pressure state, reaction after a certain period of time, reduces reaction pressure to predetermined low pressure state, then pass through reaction
Enter high pressure conditions from boosting, such circulation form carries out, until reaction terminates.In the whole process reaction raw materials continuously into
Material was in initial reaction stage into the fresh feed of reactor later, and the sufficient tolerance of generation is in generated body in reactor
Between mutually provide it is sufficient draw burnt shearing force, thus transformation operation by a larger margin may be implemented, and then can regulate and control to a greater extent
Air stream shear forces.
The continuous processing that above-mentioned steps (2) are protected is suitable for significantly transformation using high-pressure oil gas separation system
With pulse transforming reaction process, can meet high pressure charring process can also be used for low pressure charing Oil-gas Separation, to ensure that arteries and veins
Rush the product separation under transformation reaction process.
Obtained needle coke ash content≤0.4, real density >=2.13g/cm in above-mentioned steps (3)3, at 25~600 DEG C
CTE≤1.1 × 10 of measurement-6/℃.The needle coke is that optical texture is in the fine fibrous needle coke of height uniaxial orientation,
Interphase content is up to 95%~100%.
Using having the characteristics that the charing continuous processing of pulse transforming in the present invention, which has integration type anti-
Answer feature.Specifically, occur into the raw material of carbonization reaction device in the alkyl side chain of carbonization reaction initial stage aromatic compound disconnected
It splits and generates a large amount of light components, in the presence of reacting high pressure, a large amount of light components, which are dissolved in response matrix, can reduce the viscous of response matrix
Degree, and then facilitate the generation of mesophase ball, growth and subsequent melt and form body interphase；Then due to pressure reduction is light
Group branch largely escapes, and then realizes that air-flow draws Jiaozhuo to use to the body interphase of generation, is transformed into edge by sheet mesophase structure
The fine-fibrous mesophase structure of autoclave body longitudinal axis uniaxial orientation；Since fresh feed constantly enters carbonization reaction device, in pulse
The raw material of subsequent entrance will also occur to generate under high pressure similar to above-mentioned body interphase uniaxial under low pressure in turn under transformation operation
The evolutionary process of orientation, thus this technique also shows the reaction characteristics of integration type.
The present invention distinguishes compared with existing preparation method to be: the present invention is grasped during continuously carbonizing using pulse transforming
Make, show integration type reaction characteristics, can ensure can realize large scale interphase knot in reaction process most stages
The generation of structure and subsequent transformation are the coupling of the two processes of uniaxial orientation acicular texture.
Detailed description of the invention
Fig. 1 is needle coke production technological process.
1: heating furnace 2: carbonization reaction device
3: high pressure hot separator 4: cold high pressure separator
5: cold low separator 6: thermal low-pressure separators
7: condenser 8: gas-phase product outlet
9: liquid product outlet 10: green coke discharge port
Specific embodiment
Below in conjunction with the drawings and the specific embodiments, the present invention is described in further detail.
Specific step is as follows for a kind of continuous processing producing high-quality needle coke, as shown in the picture:
(1) feedstock oil is entered into carbonization reaction device 2 by heating furnace 1, keeping temperature in carbonization reaction device is 400~500
DEG C, persistently feed 10~for 24 hours, then stop charging the reaction was continued 0~18h；Arteries and veins is carried out in the range of 1~6MPa of reaction pressure
Rush transformation operation；(2) high-temperature oil gas generated during pyrogenetic reaction enters high pressure hot separator 3 at the top of carbonization reaction device 2,
The obtained liquid phase component of 3 lower part of separator enters thermal low-pressure separators 6 by bottom, and the oil-gas component on 3 top of separator by
Top, which enters cold high pressure separator 4 and is further cooled to high pressure liquid product, enters cold low separator 5 from bottom, by heat low
Liquid product in separator 6 and cold low separator 5 is collected into tank 9；4 top oil gas of cold high pressure separator passes through condenser 7
Further after cooling, remaining gaseous product is by 8 discharge of gas-phase product outlet；(3) the green coke warp that 2 bottom of carbonization reaction device generates
It by hydraulic decoking process, is discharged from the green coke discharge port 10 of 1 bottom of carbonization reaction device, needle coke production is then obtained by calcining
Product.
Embodiment 1
Using high temperature coal-tar as the charging of the continuous processing, raw material enters in carbonization reaction device 2, under nitrogen protection,
Reaction raw materials total residence time is 18h, and reaction temperature is 420 DEG C, and pulse reaction process control is carried out in reaction time,
I.e. reaction starts after controlling high pressure 1MPa reaction 3h, and after pressure drops to 0.1MPa reaction 3h, then it is anti-to rise to 1MPa for pressure
3h is answered, then pressure drops to 0.1MPa reaction 3h, next constantly carries out the pulse reaction technique as circulation, reacted
Continuous feed in journey, until terminating reaction time；After reaction, green coke is transferred out of carbonization reaction device, green coke yield rapidly
It is 55.9%, liquid by-product yield is 35.3%, and gaseous by-product yield is 8.8%.Obtained green coke interphase content is
100%, in the uniaxial fine-fibrous of orientation；For green coke after 1450 DEG C of calcining 2h, obtained needle coke product ash content is 0.3, is waved
Hair is divided into 0.4, real density 2.13g/cm3, the CTE measured at 25-600 DEG C is 1.3 × 10-6/℃。
Embodiment 2
Using coalite tar as the charging of the continuous processing, raw material enters in carbonization reaction device 2, under nitrogen protection,
Reaction raw materials total residence time is 20h, and reaction temperature is 430 DEG C, and pulse reaction process control is carried out in reaction time,
I.e. reaction starts after controlling high pressure 2MPa reaction 3h, and after pressure drops to 1MPa reaction 3h, then pressure rises to 2MPa reaction
3h, then pressure drops to 1MPa reaction 3h, next the continuous pulse reaction technique carried out as circulation, in reaction process
Continuous feed, until terminating reaction time；After reaction, green coke is transferred out of carbonization reaction device rapidly, green coke yield is
58.7%, liquid by-product yield is 33.0%, and gaseous by-product yield is 8.3%.Obtained green coke interphase content is
95%, it is in directional profile single shaft crude fibre shape；After 1450 DEG C of calcining 2h, obtained needle coke product ash content is green coke
0.25, volatilization is divided into 0.3, real density 2.15g/cm3, the CTE measured at 25-600 DEG C is 1.3 × 10-6/℃。
Embodiment 3
Using decompression residuum as the charging of the continuous processing, raw material enters in carbonization reaction device 2, under nitrogen protection, instead
Answering raw material total residence time is 19h, and reaction temperature is 435 DEG C, pulse reaction process control is carried out in reaction time, i.e.,
Reaction starts after controlling high pressure 2MPa reaction 2.5h, and after pressure drops to 1.5MPa reaction 2.5h, then pressure rises to 2MPa
2.5h is reacted, then pressure drops to 1.5MPa reaction 2.5h, the pulse reaction technique as circulation is next constantly carried out,
Continuous feed in reaction process, until terminating reaction time；After reaction, green coke is transferred out of carbonization reaction device rapidly, it is raw
Yield of coke is 60.5%, and liquid by-product yield is 33.2%, and gaseous by-product yield is 6.3%.Obtained green coke interphase
Content is 100%, in the uniaxial fine-fibrous of orientation；After 1450 DEG C of calcining 2h, obtained needle coke product ash content is green coke
0.25, volatilization is divided into 0.35, real density 2.17g/cm3, the CTE measured at 25-600 DEG C is 1.08 × 10-6/℃。
Embodiment 4
Using FCC slurry as the charging of the continuous processing, raw material enters in carbonization reaction device 2, under nitrogen protection, reaction
Raw material total residence time is 20h, and reaction temperature is 460 DEG C, pulse reaction process control is carried out in reaction time, i.e., instead
It should start after controlling high pressure 4MPa reaction 2h, after pressure drops to 3MPa reaction 2h, then pressure rises to 4MPa reaction 2h, connects
Pressure drop to 3MPa reaction 2h, next constantly carry out the pulse reaction technique as circulation, it is continuous in reaction process
Charging, until terminating reaction time；After reaction, green coke being transferred out of carbonization reaction device rapidly, green coke yield is 65.9%,
Liquid by-product yield is 27.3%, and gaseous by-product yield is 6.8%.Obtained green coke interphase content is 100%, optics
Structure is in the uniaxial crude fibre shape of orientation；Green coke is after 1450 DEG C of calcining 2h, and obtained needle coke product ash content is 0.2, volatilization
It is divided into 0.33, real density 2.17g/cm3, the CTE measured at 25-600 DEG C is 1.15 × 10-6/℃。
Embodiment 5
FCC solvent-extracted oil is starched into the charging as the continuous processing, raw material enters in carbonization reaction device 2, protects in nitrogen
Under shield, reaction raw materials total residence time is that for 24 hours, reaction temperature is 470 DEG C, and pulse reaction technique is carried out in reaction time
Regulation, i.e. reaction start after controlling high pressure 5MPa reaction 3h, and after pressure drops to 4MPa reaction 3h, then pressure rises to 5MPa
3h is reacted, then pressure drops to 4MPa reaction 3h, next constantly carries out the pulse reaction technique as circulation, reacted
Continuous feed in journey, until terminating reaction time；After reaction, green coke is transferred out of carbonization reaction device, green coke yield rapidly
It is 68.1%, liquid by-product yield is 25.6%, and gaseous by-product yield is 6.3%.Obtained green coke interphase content is
95%, optical texture is in directional profile single shaft fine-fibrous；For green coke after 1450 DEG C of calcining 2h, obtained needle coke product is grey
It is divided into 0.2, volatilization is divided into 0.28, real density 2.14g/cm3, the CTE measured at 25-600 DEG C is 1.1 × 10-6/℃。
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (4)
1. a kind of continuous processing for producing needle coke, it is characterised in that: (1) the heated boiler tube of reaction raw materials enters carbonization reaction device
In, maintaining temperature in carbonization reaction device is 400~500 DEG C, persistently feeds 10~for 24 hours, then stop charging the reaction was continued 0~
18h；During entire carbonization reaction, the pulse operation of high pressure-low pressure alternative expression, reaction pressure variation are used in carbonization reaction device
In the range of 1.0~6.0MPa；(2) green coke that carbonization reaction device bottom generates is anti-from charing via hydraulic decoking process
Device bottom is answered to be discharged to obtain green coke product；(3) green coke obtains needle coke product through calcining 2~4h at 1450 DEG C.
2. a kind of continuous processing for producing needle coke according to claim 1, it is characterised in that: the feedstock oil packet
It includes: middle coalite tar, high temperature coal-tar and its fraction, petroleum heavy oil distillate, decompression residuum, FCC slurry and above-mentioned original
Expect the solvent-extracted oil of oil.
3. a kind of continuous processing for producing needle coke according to claim 1, it is characterised in that: entire carbonization reaction process
It is middle to be operated using pulsed transformation, i.e., in the carbonization reaction device pressure reach predetermined high pressure, reduced when reacting certain time anti-
Answer pressure to predetermined low pressure, the reaction was continued a period of time, is re-circulated into predetermined high pressure from boosting by reaction process, so high
Low pressure interconversion is reciprocal, until reaction terminates.
4. a kind of continuous processing for producing needle coke according to claim 1, it is characterised in that: what is obtained after calcining is needle-shaped
Charred ashes point≤0.3, volatile matter≤0.4 real density >=2.13g/cm3, CTE≤1.3 × 10 that are measured at 25~600 DEG C-6/℃。
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109516826A (en) * | 2018-11-28 | 2019-03-26 | 凤城市宝山炭素有限公司 | A method of 600 ultra high power connector of Φ is manufactured with domestic needle coke |
| CN110734779A (en) * | 2019-10-15 | 2020-01-31 | 湖南中科星城石墨有限公司 | isotropic cokes suitable for lithium ion battery cathode raw materials and preparation method thereof |
| CN113004924A (en) * | 2021-04-15 | 2021-06-22 | 山东京阳科技股份有限公司 | Production process of needle coke for ultrahigh-power graphite electrode connector |
| WO2021232560A1 (en) * | 2020-05-22 | 2021-11-25 | 中国石油大学(华东) | Method for preparing needle coke for ultra-high power electrode from heavy oil |
| CN113862033A (en) * | 2021-09-18 | 2021-12-31 | 中国石油大学(华东) | Method for preparing needle coke with low thermal expansion coefficient by combining fluid coking and delayed coking |
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| CN203079911U (en) * | 2013-01-30 | 2013-07-24 | 陕西煤业化工技术研究院有限责任公司 | Device for preparing coal based needle coke |
| CN106566570A (en) * | 2016-10-21 | 2017-04-19 | 中国石油大学(华东) | Method for preparing high-quality needle coke through heavy oil |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN203079911U (en) * | 2013-01-30 | 2013-07-24 | 陕西煤业化工技术研究院有限责任公司 | Device for preparing coal based needle coke |
| CN106566570A (en) * | 2016-10-21 | 2017-04-19 | 中国石油大学(华东) | Method for preparing high-quality needle coke through heavy oil |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109516826A (en) * | 2018-11-28 | 2019-03-26 | 凤城市宝山炭素有限公司 | A method of 600 ultra high power connector of Φ is manufactured with domestic needle coke |
| CN110734779A (en) * | 2019-10-15 | 2020-01-31 | 湖南中科星城石墨有限公司 | isotropic cokes suitable for lithium ion battery cathode raw materials and preparation method thereof |
| WO2021232560A1 (en) * | 2020-05-22 | 2021-11-25 | 中国石油大学(华东) | Method for preparing needle coke for ultra-high power electrode from heavy oil |
| US11286425B2 (en) | 2020-05-22 | 2022-03-29 | China University Of Petroleum | Method for preparing needle coke for ultra-high power (UHP) electrodes from heavy oil |
| CN113004924A (en) * | 2021-04-15 | 2021-06-22 | 山东京阳科技股份有限公司 | Production process of needle coke for ultrahigh-power graphite electrode connector |
| CN113862033A (en) * | 2021-09-18 | 2021-12-31 | 中国石油大学(华东) | Method for preparing needle coke with low thermal expansion coefficient by combining fluid coking and delayed coking |
| CN113862033B (en) * | 2021-09-18 | 2023-01-13 | 中国石油大学(华东) | Method for preparing needle coke with low thermal expansion coefficient by combining fluid coking and delayed coking |
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