CN104560081B - Method for producing needle coke by kettle type coking - Google Patents
Method for producing needle coke by kettle type coking Download PDFInfo
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- CN104560081B CN104560081B CN201310496046.2A CN201310496046A CN104560081B CN 104560081 B CN104560081 B CN 104560081B CN 201310496046 A CN201310496046 A CN 201310496046A CN 104560081 B CN104560081 B CN 104560081B
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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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
- G01N11/10—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material
- G01N11/14—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material by using rotary bodies, e.g. vane
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Abstract
The invention discloses a method for producing needle coke by kettle type coking. The method comprises the following steps: (1) filling a coking still with raw material oil, sealing the coking still, filling the coking still with inert gas for pressurization, keeping the pressure constant, and heating to preheating temperature; (2) simultaneously slowly heating the system to reaction temperature from the preheating temperature and starting to measure the viscosity of the system, keeping the temperature constant when the system reaches the reaction temperature, and adding distillate oil into the coking still when the viscosity of the system reaches a viscosity threshold value in the temperature preservation process; (3) at the end of temperature preservation, heating the system to carbonizing temperature, performing carbonization under constant temperature, and performing cooling and pressure release to obtain the needle coke product. According to the method, the change of the viscosity of the reaction system can be effectively monitored, the generation process of an intermediate phase is optimized, and the quality of the needle coke product is improved.
Description
Technical field
The present invention relates to a kind of preparation method of needle coke, relates in particular to a kind of side of autoclave coking production needle coke
Method.
Background technology
Needle coke is a kind of novel carbon material, with thermal coefficient of expansion (CTE) it is relatively low, crystallization degree is high, resistivity is low
The advantages of, mainly for the production of high power（HP）, ultra high power (UHP) graphite electrode, extraordinary carbon materials etc., industry,
It is widely used in the fields such as national defence, medical treatment and space flight.
Compared with the production technology of ordinary coke, needle coke production has special requirement to raw material and technique.Which is crucial
It is " mesophase formation stages ", this theory is proposed in nineteen sixty-five first by Brooks and Taylor, this theory thinks needle coke
Formation can be divided into two stages：One is that aroma substance coal tar or black petroleum products Jing liquid carbonizeds generate mesophase ball,
Bead increases, and melts and into anisotropy height, the mesophase of good fluidity；Two is the further carbonization of this kind of mesophase, is produced
The effusion of Light ends cause the so-called acicular texture of the further arrangement form of fragrant hydrocarbon molecule arranged in parallel, while solidify obtaining
Obtain needle coke.
At present, in using the process of autoclave coking production needle coke, more using volume or pressure for generating gas etc.
Controlling production technology, such as CN101532937A discloses a kind of by gas production rate detection needle coke mesophase shape parameter
Into process, pressure gauge of the method by consersion unit, per ten minutes record reaction arrange in pressure, basis afterwards
The Ideal-Gas Equation is calculated the volume for generating gas, and then it is bent with the relation of time to obtain generating the speed of gas
Line, according to this variation tendency of curve reflect the generation progress of mesophase.
CN102965132A discloses a kind of method for preparing needle coke using magnetization reactor, and the method is by reaction
Kettle side is symmetrical arranged magnetizing assembly, in mesophase forming process makes polycyclic aromatic macromole orient row by external magnetic field
Row, so that form acicular texture.
CN1731189A discloses a kind of method for being formed in site detection of needle coke mesophase in real time, and the method is by one
Reference electrode and a measuring electrode are inserted in the middle part of reaction system, and an earth lead is inserted into reaction system bottom, then
Numerical value automatic production record is set to zero, start recording, and numerical value is amplified into conversion, supervised by numerical value automatic production record in real time
The reactive state changed to detect mesophase of control numerical value.
Existing technology cannot guarantee that reaction system is formed in suitable mesophase all the time during whole isothermal reaction
Environment, often reaction middle and late stage, due to the viscosity of reaction system it is excessive and hamper the growth of mesophasespherule with
Melt simultaneously, it is impossible to reach expected production effect.
The content of the invention
For the deficiencies in the prior art, the invention provides a kind of method of autoclave coking production needle coke, the method can
Effectively to monitor the change of reaction system viscosity, the generating process of mesophase is optimized, improve needle coke product quality.
The method of the autoclave coking production needle coke of the present invention, including herein below：
（1）Load raw oil in coking still, after sealing, be filled with noble gases supercharging, and keep pressure constant, be warming up to
Preheating temperature；
（2）System is to slowly warm up to reaction temperature by preheating temperature, and intensification starts simultaneously at the viscosity of measurement system, works as system
Reaction temperature is reached, constant temperature, in thermostatic process when system viscosity reaches viscosity threshold values, adds distillate into coking still；
（3）After constant temperature terminates, system temperature is risen to into carbonization temperature, constant temperature carbonization, cooling, blood pressure lowering obtain needle coke product
Product.
In the inventive method, described raw oil include straight-run gas oil, wax tailings, heavy distillate, catalytic cracked oil pulp,
One or more mixture in catalytic cracking clarified oil or thermal cracking residue.
In the inventive method, step（1）Described coking still preheating temperature is 350～400 DEG C, and pressure is 1～1.5MPa；
Step（1）Described programming rate is 3～5 DEG C/min.
In the inventive method, step（2）420～480 DEG C of the reaction temperature, heating rate are 5～15 DEG C/h, permanent
The warm response time is 4～8 hours.
In the inventive method, step（2）The time interval of described measurement system viscosity be 10～60 minutes, preferably 10 ~
30 minutes.
In the inventive method, step（2）Described viscosity threshold determined by the characteristic of raw material, generally 60～100Pa s.
In the inventive method, step（2）Described distillate be raw oil distillation obtained by distillate, boiling range be 300 ~
450 DEG C, preferably 350～400 DEG C.
In the inventive method, step（2）Described distillate should be preheated to reaction temperature, distillate before injection reactor
Addition for raw material weight of oil 10%～25%.
In the inventive method, step（4）Described carbonization temperature be 510～570 DEG C, heating rate be 10～30 DEG C/it is little
When, constant temperature carbonization time is 2～4 hours.
In the inventive method, using rotor viscosity meter system viscosity, the wherein pivot design of rotor viscometer is for can
It is telescopic.Measuring process is as follows：（1）Rotor is slowly stretched into below liquid level at 2 ~ 5cm；（2）Viscometer switch is opened, reading is treated
Record data after steady, closes viscometer；（3）Rotor is lifted and is fixed to ullage, measurement terminates.
In the inventive method, sealed bearings are used in coking still with the seam of rotor viscometer rotating shaft.
In the inventive method, the rotor of rotor viscometer is detachable.
Existing process has been not able to accurately the real conditions inside solution reaction kettle, and whole reaction system is not
It is constantly in the optimum condition formed most useful for mesophase.During common autoclave coking production needle coke, system is glued
The change of degree typically follows following rule：（1）In the temperature rise period, system viscosity can be reduced because of the rising of temperature, viscosity with temperature
Degree change follows a kind of simple linear relationship, and this viscosity downward trend produced because of temperature rise can be with the end for heating up
And stop；（2）In later stage temperature rise period and constant temperature stage, in system, there is hot dehydrogenation polycondensation reaction, the continuous polycondensation of small molecule
For bigger molecule, mesophase is gradually formed, and during this, the mean molecule quantity of whole system rapidly increases, viscosity also with
Significant rising；（3）After constant temperature terminates, temperature rises to carbonization temperature, and pyrogenetic reaction occurs in system, and viscosity is risen rapidly
Height, until be fully cured.
In above-mentioned process（2）In, mainly there is hot dehydrogenation polycondensation reaction in system, less hydrocarbon molecules polycondensation be compared with
Big toluene insolubles（TI）, and then to continue polycondensation be pyridine insoluble (PI) and quinoline insolubles (QI), and polycondensation is put down
Face macromole is gathered into spherula in the presence of Van der Waals force, and spherula constantly grows, and melts with other spherulas and be
Bigger multiple ball, this process are the committed steps of needle coke production, need long-time, low viscosity, metastable reaction environment.
However, in process of production, due to the continuous polycondensation of small molecule, the viscosity of system is caused rapidly to rise, often in thermostatic process
Middle and late stage, due to system viscosity excessive growth so as to hinder mesophasespherule and melt simultaneously, cause product property to decline.
The inventive method compared with prior art, with advantages below：
（1）By the real-time monitoring to viscosity inside coking reactor, when viscosity is too high, by adding low viscosity component
To reduce the viscosity of the system reacted, whole reaction system is made to maintain one always beneficial to mesophasespherule in the constant temperature stage
Generation, melt and low viscosity environment, enable spherula sufficiently to grow up, melt simultaneously, form continuous mesophase structure, improve
The anisotropic properties of product.
（2）The control parameters such as the pressure that generally adopted, tolerance, are a kind of modes of the situation in indirect reflection kettle, must
Certain error and time delay are there is so；And viscosity is a Macroscopic physical for directly embodying system mesophase reaction process
Amount, compared with above-mentioned parameter, more directly, accurately and in time.
（3）As raw material is presented non-Newtonian fluid properties at reaction conditions, after the long-time by rotor is sheared,
Raw material near measurement point will be unable to really reflect overall viscosity B coefficent trend, and the rotor viscosity in the present invention is calculated as can
It is telescopic so that in the intermittent time of each measurement, in that context it may be convenient to insert rotor or leave raw material liquid level, to eliminate raw material
" memory effect "；Rotor can be removed from rotating shaft for detachable, the cleaning after terminating in order to burning process with more
Change.
Description of the drawings
Fig. 1 is the rotor viscometer structural representation in the inventive method；Wherein, 1 is rotor viscometer, and 2,4 are transmission
Bar, 3 is connector, and 5 is coking still top flange, and 6 is sealed bearings, and 7 is rotor.
Fig. 2 is the curve of the viscosity with the time of the embodiment of the present invention 1.
Fig. 3 is the scanning electron microscope of the needle coke of the embodiment of the present invention 1（SEM）Photo.
Specific embodiment
Explanation and embodiment are described in detail to this technology scheme of the invention below in conjunction with the accompanying drawings, but the present invention is not by following
The restriction of embodiment.
Embodiment 1
The present embodiment is the autoclave coking test device using capacity for 15L, with Nanjing Effect of Catalysis In Petrochemistry cracking slurry oil as original
Material, loads 4kg raw oils first in the coking still, sealing, and being filled with nitrogen makes in kettle Stress control in 1.5MPa, with 3 DEG C/min
Speed temperature is risen very rapidly up to into 400 DEG C, start simultaneously at measurement viscosity（Measurement interval 30 minutes）, and draw viscosity-time
Curve（As shown in Figure 2）；
When system temperature reaches 400 DEG C, keep pressure constant, adjustment heating rate is 10 DEG C/h, and temperature is risen to
460℃；
When system temperature reaches 460 DEG C, this temperature and pressure is maintained 6 hours, viscosity measurement interval is changed to 15 minutes, when viscous
After degree is more than 80Pa s, from feeding line to kettle in inject and be preheated to 460 DEG C of distillate（Nanjing catalytic cracked oil pulp 350～
450 DEG C of fractions）, injection weight is 0.5kg；
After constant temperature terminates, system temperature is risen to into 520 DEG C with 10 DEG C/h of speed, continue 4 hours, start carbonization
Process；Carbonization terminates rear Temperature fall, blood pressure lowering, and experiment terminates.
After resulting coke is calcined at 1350 DEG C, test property result is as shown in table 1.
1 as shown by data of table, the needle coke density produced by example 1 are big（2.185 g/cm3）, ash it is low（0.06w%）, heat
The coefficient of expansion is low（1.26×10-6/℃）, the standard of high-quality needle coke has been reached, can be used to produce ultra-high power graphite electrode.Such as Fig. 3
Shown, the needle coke product of example 1 presents layer structure under a scanning electron microscope, with anisotropic characteristic.
Embodiment 2
The present embodiment uses coking plant same as Example 1, with Ba Ling Effect of Catalysis In Petrochemistry cracking clarified oils as raw material,
Load 4.5kg raw oils in coking still, sealing, being filled with nitrogen makes in kettle Stress control in 1.0MPa, with 5 DEG C/min of speed
Temperature is risen very rapidly up to into 350 DEG C, measurement viscosity is started simultaneously at（Measurement interval 30 minutes）, and draw viscosity profile over time；
When system temperature reaches 350 DEG C, keep pressure constant, adjustment heating rate is 15 DEG C/h, and temperature is risen to
480℃；
When system temperature reaches 480 DEG C, this temperature and pressure is maintained 4 hours, viscosity measurement interval is changed to 15 minutes, when viscous
After degree is more than 60Pa s, from feeding line to kettle in inject and be preheated to 480 DEG C of distillate（Ba Ling Effect of Catalysis In Petrochemistry cracking clarified oils
300～450 DEG C of fractions）, injection weight is 0.5kg；
After constant temperature terminates, system temperature is risen to into 560 DEG C with 30 DEG C/h of speed, continue 2 hours, start carbonization
Process；Carbonization terminates rear Temperature fall, blood pressure lowering, and experiment terminates.
After resulting coke is calcined at 1350 DEG C, test property result is as shown in table 1.
1 as shown by data of table, the needle coke density produced by example 2 are big（2.216 g/cm3）, ash it is low（0.04w%）, heat
The coefficient of expansion is low（1.28×10-6/℃）, the standard of high-quality needle coke has been reached, can be used to produce ultra-high power graphite electrode.
Embodiment 3
The present embodiment uses coking plant same as Example 1, with Kelamayi windy city super-viscous oil as raw material, in coking
Load 4.0kg raw oils in kettle, sealing, being filled with nitrogen makes in kettle Stress control in 1.3MPa, with 5 DEG C/min of speed by temperature
Degree rises very rapidly up to 380 DEG C, starts simultaneously at measurement viscosity（Measurement interval 30 minutes）, and draw viscosity profile over time；
When system temperature reaches 380 DEG C, keep pressure constant, adjustment heating rate is 10 DEG C/h, and temperature is risen to
420℃；
When system temperature reaches 420 DEG C, this temperature and pressure is maintained 8 hours, viscosity measurement interval is changed to 15 minutes, when viscous
After degree is more than 100Pa s, from feeding line to kettle in inject and be preheated to 420 DEG C of distillate（The 300 of catalytic cracking clarified oil～
400 DEG C of fractions）, injection weight is 0.8kg；
After constant temperature terminates, system temperature is risen to into 520 DEG C with 30 DEG C/h of speed, continue 3 hours, start carbonization
Process；Carbonization terminates rear Temperature fall, blood pressure lowering, and experiment terminates.
After resulting coke is calcined at 1350 DEG C, test property result is as shown in table 1.
1 as shown by data of table, the needle coke density produced by example 3 are big（2.197 g/cm3）, ash it is relatively low（0.07w%）、
Thermal coefficient of expansion is low（1.29×10-6/℃）, the standard of high-quality needle coke has been reached, can be used to produce ultra-high power graphite electrode.
Embodiment 4
The present embodiment uses coking plant same as Example 1, with wax tailings as raw material, loads in coking still
4.0kg raw oils, sealing, being filled with nitrogen makes in kettle Stress control in 1.2MPa, with 3 DEG C/min of speed will be temperature rapid on
360 DEG C are risen to, measurement viscosity is started simultaneously at（Measurement interval 30 minutes）, and draw viscosity profile over time；
When system temperature reaches 360 DEG C, keep pressure constant, adjustment heating rate is 5 DEG C/h, and temperature is risen to 430
℃；
When system temperature reaches 430 DEG C, this temperature and pressure is maintained 4 hours, viscosity measurement interval is changed to 15 minutes, when viscous
After degree is more than 80Pa s, from feeding line to kettle in inject and be preheated to 430 DEG C of distillate（350～400 DEG C of raw oil evaporate
Point）, injection weight is 1kg；
After constant temperature terminates, system temperature is risen to into 510 DEG C with 20 DEG C/h of speed, continue 3 hours, start carbonization
Process；Carbonization terminates rear Temperature fall, blood pressure lowering, and experiment terminates.
After resulting coke is calcined at 1350 DEG C, test property result is as shown in table 1.
1 as shown by data of table, the needle coke density produced by example 3 are big（2.207 g/cm3）, ash it is relatively low（0.05w%）、
Thermal coefficient of expansion is low（1.28×10-6/℃）, the standard of high-quality needle coke has been reached, can be used to produce ultra-high power graphite electrode.
Comparative example 1
Comparative example 1 adopts raw material same as Example 1 and initial condition, and after system temperature reaches 400 DEG C, adjustment rises
Warm speed is 5 DEG C/h, starts simultaneously at record cracking gas velocity, when gas flow rate is less than 0.05L/ hours, is considered as mesophase
It is completely formed, now system temperature is 475 DEG C, maintains this temperature and pressure 6 hours, and carbonization process condition is with embodiment 1.
After resulting coke is calcined at 1350 DEG C, test property result is as shown in table 1.As shown by data, is using phase
Under same raw material, compared with example 1, true density is less for the product of comparative example 1（2.164 g/cm3）, thermal coefficient of expansion it is higher
（1.31×10-6/℃）, product quality is slightly poor.
Comparative example 2
Compared with Example 1, identical raw material used in comparative example 2, but viscosity test is not carried out, also it is not added with fraction
Oily viscosity reduction, actual conditions are as follows：Load 4kg Nanjing Effect of Catalysis In Petrochemistry cracking slurry oil in kettle, being filled with nitrogen after sealing makes pressure control
Temperature is risen to 400 DEG C with 3 DEG C/min of speed, after reaching 400 DEG C, with 10 DEG C/h of ramp in 1.5MPa by system
To 460 DEG C, system temperature is risen to 520 DEG C with 10 DEG C/h of speed by constant temperature 6 hours, continues 2 hours, natural after terminating
Cooling, blood pressure lowering, experiment terminate.
1 embodiment of table and comparative example product test property.
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 | Comparative example 2 |
| Volatile matters, wt% | 0.52 | 0.32 | 0.25 | 0.27 | 0.41 | 0.47 |
| Ash, wt% | 0.06 | 0.04 | 0.07 | 0.05 | 0.07 | 0.06 |
| Sulphur content, wt% | 0.28 | 0.31 | 0.29 | 0.35 | 0.25 | 0.27 |
| True density, g/cm3 | 2.185 | 2.216 | 2.197 | 2.207 | 2.164 | 2.124 |
| Thermal coefficient of expansion, × 10-6/℃(100-600℃) | 1.26 | 1.28 | 1.29 | 1.28 | 1.31 | 1.35 |
After resulting coke is calcined at 1350 DEG C, test property result is as shown in table 1.As shown by data, in identical
Under raw material and Elevated Temperature Conditions, compared with example 1, true density is less for the product of comparative example 2（2.124 g/cm3）, thermal coefficient of expansion
It is higher（1.35×10-6/℃）, product quality is poor, and the method used in embodiment can effective improve product quality.
Claims (9)
1. a kind of method of autoclave coking production needle coke, including herein below：（1）Load raw oil in coking still, seal
Afterwards, noble gases supercharging is filled with, and keeps pressure constant, be warming up to preheating temperature；（2）System is to slowly warm up to by preheating temperature
Reaction temperature, intensification start simultaneously at the viscosity of measurement system, and when system reaches reaction temperature, constant temperature works as system in thermostatic process
When viscosity reaches viscosity threshold values, distillate is added into coking still；（3）After constant temperature terminates, system temperature is risen to into carbonization temperature,
Constant temperature carbonization, cooling, blood pressure lowering, obtains needle coke product；
Wherein, using rotor viscosity meter system viscosity, wherein the pivot design of rotor viscometer is extension type.
2. in accordance with the method for claim 1, it is characterised in that：Described raw oil includes straight-run gas oil, wax tailings, weight
One or more mixture in distillate, catalytic cracked oil pulp, catalytic cracking clarified oil or thermal cracking residue.
3. in accordance with the method for claim 1, it is characterised in that：Step（1）Described coking still preheating temperature be 350～
400 DEG C, pressure is 1～1.5MPa, and programming rate is 3～5 DEG C/min.
4. in accordance with the method for claim 1, it is characterised in that：Step（2）420～480 DEG C of the reaction temperature, heat up speed
Rate is 5～15 DEG C/h, and the isothermal reaction time is 4～8 hours.
5. in accordance with the method for claim 1, it is characterised in that：Step（2）The time interval of described measurement system viscosity
For 10～60 minutes.
6. in accordance with the method for claim 1, it is characterised in that：Step（2）Described viscosity threshold is 60～100Pa s.
7. in accordance with the method for claim 1, it is characterised in that：Step（2）Described distillate is raw oil distillation gained
The boiling range for arriving is 300 ~ 450 DEG C of distillate, and the addition of distillate is the 10%～25% of raw material weight of oil.
8. in accordance with the method for claim 1, it is characterised in that：Step（3）Described carbonization temperature is 510～570 DEG C, is risen
Warm speed is 10～30 DEG C/h, and constant temperature carbonization time is 2～4 hours.
9. in accordance with the method for claim 1, it is characterised in that：Measuring process is as follows：（1）Rotor is slowly stretched under liquid level
At 2 ~ 5cm of side；（2）Viscometer switch is opened, the record data after reading is steady closes viscometer；（3）Rotor is lifted into liquid
Fixed above face, measurement terminates.
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| CN105372280B (en) * | 2016-01-18 | 2018-07-20 | 中国科学院山西煤炭化学研究所 | A kind of method of determining needle coke preparation process liquid-phase polymerization time |
| CN106403579B (en) * | 2016-10-21 | 2018-10-30 | 中国石油大学(华东) | A kind of method that mesophase pitch prepares high-quality needle coke electrode material |
| CN108795462B (en) * | 2018-06-11 | 2021-09-21 | 中国石油大学(华东) | Preparation method of high-order needle petroleum coke |
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| US4436615A (en) * | 1983-05-09 | 1984-03-13 | United States Steel Corporation | Process for removing solids from coal tar |
| CN101532937A (en) * | 2009-04-08 | 2009-09-16 | 太原理工大学 | Method for detecting needle coke mesophase formation |
| CN102634361A (en) * | 2011-02-10 | 2012-08-15 | 中国石油天然气股份有限公司 | Preparation method of acicular petroleum coke |
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| CN103205271A (en) * | 2012-01-12 | 2013-07-17 | 易高环保能源研究院有限公司 | Method for hydrogenation of high temperature coal tar to produce mesophase pitch |
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| JPH086092B2 (en) * | 1987-04-20 | 1996-01-24 | 興亜石油株式会社 | Highly oriented needle coke manufacturing method |
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|---|---|---|---|---|
| US4436615A (en) * | 1983-05-09 | 1984-03-13 | United States Steel Corporation | Process for removing solids from coal tar |
| CN101532937A (en) * | 2009-04-08 | 2009-09-16 | 太原理工大学 | Method for detecting needle coke mesophase formation |
| CN102634361A (en) * | 2011-02-10 | 2012-08-15 | 中国石油天然气股份有限公司 | Preparation method of acicular petroleum coke |
| CN103045278A (en) * | 2011-10-17 | 2013-04-17 | 中国石油化工股份有限公司 | Kettle-type method for preparing needle coke |
| CN103205271A (en) * | 2012-01-12 | 2013-07-17 | 易高环保能源研究院有限公司 | Method for hydrogenation of high temperature coal tar to produce mesophase pitch |
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