CN109135789A - A kind of method that middle coalite tar prepares needle coke - Google Patents
A kind of method that middle coalite tar prepares needle coke Download PDFInfo
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- CN109135789A CN109135789A CN201810932497.9A CN201810932497A CN109135789A CN 109135789 A CN109135789 A CN 109135789A CN 201810932497 A CN201810932497 A CN 201810932497A CN 109135789 A CN109135789 A CN 109135789A
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- coalite tar
- middle coalite
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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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- 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
- C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
- C10B57/08—Non-mechanical pretreatment of the charge, e.g. desulfurization
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- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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- General Chemical & Material Sciences (AREA)
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Abstract
A kind of method that middle coalite tar prepares needle coke, include the following steps: middle coalite tar obtaining heavy component through distillation, by polar solvent, nonpolar solvent, two kinds therein of the mixture of polar solvent and nonpolar solvent is uniformly mixed for 1:10~10:1 obtains mixed solvent in mass ratio, the heavy component of middle coalite tar is sent into reaction kettle, 60~200 DEG C are heated to stir evenly, mixed solvent is added into reaction kettle again, the mass ratio of mixed solvent and heavy component is 0.5:1~3:1, 1~20h is stood after 50~200 DEG C of 1~10h of stirring, high reaction activity substance is removed using the method for physical separation, the clarified solution obtained after high reaction activity substance will be removed to parse, parse the unreacted mixed solvent in clarified solution, obtain needle-shape coke raw material The needle-shape coke raw material pitch is obtained needle coke through coking and calcine technology by pitch.Present invention process method is simple, and reaction condition is mild, low for equipment requirements, is not necessarily to high temperature and pressure, and strong operability is at low cost.
Description
Technical field
The present invention relates to middle coalite tar field of deep more particularly to a kind of middle coalite tar to prepare needle coke
Method.
Background technique
Increasingly in short supply with petroleum resources, the processing and utilization of coal tar is paid attention to.Coal tar include high temperature coal-tar,
Medium temperature coal tar and coalite tar, at present about the processing technology comparative maturity of high temperature coal-tar, application is relatively broad, such as makes
As binder or needle coke is prepared etc. when standby isotropic graphite material.Middle coalite tar is in production semi-coke during institute
The liquid product obtained passes through the resulting product of low temperature distillation, destructive distillation mainly using low-order coals such as dross coal or weakly caking coals as raw material
Temperature mainly contains aromatic hydrocarbons, alkane, phenols and unsaturated hydro carbons etc. generally at 650~750 DEG C, and fragrance point is lower, using compared with
It is few.China's coal chemical industry can all generate coalite tar byproduct in a large amount of every year, due to lacking good recovery method,
It is most of to be incinerated because of that recycle as fuel, a large amount of resource is also wasted while polluting environment.
If needle coke can be used to produce by middle coalite tar, both middle coalite tar can be made to be utilized effectively, can also reduced
The preparation cost of needle coke not only has significant economic benefit, while also having apparent social benefit.
Needle coke is the quality material for manufacturing high power and ultra-high power graphite electrode, and manufactured electrode has thermal shock resistance
By force, the advantages that high mechanical strength, oxidation resistent susceptibility are good, consumption of electrode is low and current density is big.Currently, needle coke is extensive
Applied to high-tech such as ultra-high power graphite electrodes used in electric furnace steel making, manufacture nuclear reactor decelerating material and manufacture rocket launching
Field.The raw material that industrially can be used to produce needle coke mainly has catalytic cracking clarified oil, black petroleum products, ethylene bottom oil, coal tar
Oil etc. can be divided into needle coke oil system needle coke and coal-based needle coke according to the difference of raw material sources, but no matter which kind of needle coke,
It has certain requirement to raw material.It in general, the necessary arene content of the ingredient requirement of needle coke is high, but does not include that condensed ring is big
Molecule aromatic hydrocarbons, content of heteroatoms is low, tenor is low, ash content is low, asphalt content is low.In addition, needle-shape coke raw material require have compared with
High thermal stability, i.e., the high reaction activity constituent content in raw material by thermal excitation wants low, to be conducive to raw material in thermal transition
It keeps being unlikely to too fast charing rate in the process, and then forms preferable fibrous mesophase structure and big sheet interphase knot
Structure, these structures are the typical microstructures of needle coke.
In recent years since, crude steel production capacity has been dissolved with steel industry and has thoroughly shut down and removed more than 100,000,000 tons of main frequency furnaces, intermediate frequencies
The development of the work such as furnace " bar steel " production capacity, in addition continuous improvement of the country to requirement energy-saving in steelmaking process, electric furnace refining
Development of the steel in China is getting faster, and has driven ultra-high power graphite electrode demand, is correspondingly also increased to the demand of needle coke obviously,
Cause needle coke big bulge in price, calcined coke increases to 3.5~40,000/ton by initial 4000 yuan/ton.Simultaneously with domestic needle-shaped
For coke in the application in lithium cell cathode material field, higher demand is presented in needle coke in terms of negative electrode material.It is expected that 2020,
Negative electrode material field will break through 200,000 tons to the yearly demand amount of needle coke.The coming years, the demand of needle coke is by sustainable growth.
It therefore, is raw material, the high-quality needle that application and preparation is extensive, supply falls short of demand based on cheap and easy to get, abundance middle coalite tar
Shape coke is of great significance.
Summary of the invention
The object of the present invention is to provide a kind of method that middle coalite tar prepares needle coke, this method simple process, instead
Mild condition is answered, it is low for equipment requirements, it is not necessarily to high temperature and pressure, strong operability is at low cost.The it is proposed of the process, is not only opened up
The range for having opened up needle-shape coke raw material reduces the production cost of needle coke, also solves middle coalite tar processing and utilization mentions
A new way new method is supplied.High power and ultra-high power graphite electrode material can be used for using needle coke prepared by the method for the present invention
Material, lithium ion battery negative material etc..
To achieve the above object, the present invention is implemented with the following technical solutions:
A kind of method that middle coalite tar prepares needle coke, includes the following steps:
Middle coalite tar is obtained into heavy component through distillation, by polar solvent, nonpolar solvent, polar solvent and non-pole
Property solvent two kinds therein of mixture in mass ratio for 1:10~10:1 be uniformly mixed obtain mixed solvent, by middle low temperature coal tar
The heavy component of oil is sent into reaction kettle, is heated to 60~200 DEG C and stirs evenly, then mixed solvent is added into reaction kettle, described
The mass ratio of mixed solvent and heavy component is 0.5:1~3:1, and 1~20h is stood after 50~200 DEG C of 1~10h of stirring, is used
The method of physical separation removes high reaction activity substance, will remove the clarified solution obtained after high reaction activity substance and parses,
The unreacted mixed solvent in clarified solution is parsed, needle-shape coke raw material pitch is obtained, by the needle-shape coke raw material pitch through coke
Change and calcine technology obtains needle coke.
The distillation is one or more of air-distillation, vacuum distillation, thin film evaporation.
The polar solvent is methanol, ethyl alcohol, acetic acid, pyridine, acetone, chloroform, propyl alcohol or tetrahydrofuran.
The nonpolar solvent is benzene, toluene, carbon tetrachloride, dichloroethanes, chloroform, n-hexane, hexane or heptane.
The mixture of the polar solvent and nonpolar solvent be kerosene, wax oil, washing oil, a carbolineum, anthracene oil, naphtalene oil,
Carbolic oil or coking heavy oil.
The method of the physical separation is one or more of overflow, filtering, suction filtration.
Compared with prior art, the beneficial effects of the present invention are:
Present invention process method is simple, and reaction condition is mild, low for equipment requirements, be not necessarily to high temperature and pressure, strong operability, at
This is low.While expanding needle-shape coke raw material range, the production cost of needle coke, the also processing for middle coalite tar are reduced
A new way new method is provided, resource is efficiently used, which not only has significant economic benefit, simultaneously
Also there is apparent social benefit.
Detailed description of the invention
Fig. 1 is its Pianguan County's micro-structure diagram of needle coke obtained by the embodiment of the present invention 1.
Fig. 2 is its Pianguan County's micro-structure diagram of needle coke obtained by the embodiment of the present invention 2.
Fig. 3 is its Pianguan County's micro-structure diagram of needle coke obtained by the embodiment of the present invention 3.
Fig. 4 is its Pianguan County's micro-structure diagram of needle coke obtained by the embodiment of the present invention 4.
Fig. 5 is its Pianguan County's micro-structure diagram of needle coke obtained by the embodiment of the present invention 5.
Fig. 6 is its Pianguan County's micro-structure diagram of needle coke obtained by the embodiment of the present invention 6.
Fig. 7 is Pianguan County's micro-structure diagram of coke obtained by the direct coking of middle coalite tar.
Specific embodiment
The present invention is described in detail below, it should be noted that implementation of the invention embodiment party not limited to the following
Formula.
A kind of method that middle coalite tar prepares needle coke, includes the following steps:
Middle coalite tar is obtained into heavy component through distillation, by polar solvent, nonpolar solvent, polar solvent and non-pole
Property solvent two kinds therein of mixture in mass ratio for 1:10~10:1 be uniformly mixed obtain mixed solvent, by middle low temperature coal tar
The heavy component of oil is sent into reaction kettle, is heated to 60~200 DEG C and stirs evenly, then mixed solvent is added into reaction kettle, described
The mass ratio of mixed solvent and heavy component is 0.5:1~3:1, and 1~20h is stood after 50~200 DEG C of 1~10h of stirring, is used
The method of physical separation removes high reaction activity substance, will remove the clarified solution obtained after high reaction activity substance and parses,
The unreacted mixed solvent in clarified solution is parsed, needle-shape coke raw material pitch is obtained, by the needle-shape coke raw material pitch through coke
Change and calcine technology obtains needle coke.
Middle coalite tar is coalite tar or medium temperature coal tar or two kinds of mixing.Coalite tar is by coal or oily page
Rock is through oil product obtained by low temperature distillation.Medium temperature coal tar is as coal or oil shale through oil product obtained by medium temperature carbonization.
The distillation is one or more of air-distillation, vacuum distillation, thin film evaporation.
The polar solvent is methanol, ethyl alcohol, acetic acid, pyridine, acetone, chloroform, propyl alcohol or tetrahydrofuran.
The nonpolar solvent is benzene, toluene, carbon tetrachloride, dichloroethanes, chloroform, n-hexane, hexane or heptane.
The mixture of the polar solvent and nonpolar solvent be kerosene, wax oil, washing oil, a carbolineum, anthracene oil, naphtalene oil,
Carbolic oil or coking heavy oil.
The method of the physical separation is one or more of overflow, filtering, suction filtration.
Embodiment one:
Take coalite tar in 200g to be placed in reaction kettle, air-distillation isolates heavy component to 360 DEG C, by methanol and
Benzene 7:3 in mass ratio is uniformly mixed and obtains mixed solvent, and the above-mentioned heavy component isolated is sent into reaction kettle, is heated to 60 DEG C
It stirs evenly, then mixed solvent is added into reaction kettle, the mass ratio of mixed solvent and heavy component is 1:0.5, at 60 DEG C
3h is stirred, stops stirring stratification 3h at 60 DEG C, high reaction activity substance is isolated using the method for filtering, will be removed high anti-
It answers the clarified solution obtained after active material to be parsed, parses unreacted mixed solvent, obtain needle-shape coke raw material pitch 1#,
Acquired needle-shape coke raw material pitch 1#Needle coke 1 is obtained through coking and calcine technology#, Pianguan County's microstructure is as shown in Figure 1.
Embodiment two:
Take coalite tar in 200g to be placed in reaction kettle, air-distillation isolates heavy component to 380 DEG C, by acetic acid and
Heptane 5:5 in mass ratio is uniformly mixed and obtains mixed solvent, and the above-mentioned heavy component isolated is sent into reaction kettle, is heated to 90
It DEG C stirs evenly, then mixed solvent is added into reaction kettle, the mass ratio of mixed solvent and heavy component is 1:2, at 90 DEG C
2h is stirred, stops stirring stratification 4h at 90 DEG C, high reaction activity substance is isolated using the method for overflow, will be removed high anti-
It answers the clarified solution obtained after active material to be parsed, parses unreacted mixed solvent, obtain needle-shape coke raw material pitch 2#,
Acquired needle-shape coke raw material pitch 2#Needle coke 2 is obtained through coking and calcine technology#, Pianguan County's microstructure is as shown in Figure 2.
Embodiment three:
Take coalite tar in 200g to be placed in reaction kettle, vacuum distillation isolates heavy component to 320 DEG C, by wax oil and
One carbolineum 4:6 in mass ratio is uniformly mixed and obtains mixed solvent, and the above-mentioned heavy component isolated is sent into reaction kettle, is heated to
140 DEG C stir evenly, then mixed solvent are added into reaction kettle, and mixed solvent and heavy component are 1:1 in mass ratio,
4h is stirred at 140 DEG C, stops stirring stratification 5h at 140 DEG C, high reaction activity substance is isolated using the method for suction filtration, it will
It removes the clarified solution obtained after high reaction activity substance to be parsed, parses unreacted mixed solvent, obtain needle coke original
Expect pitch 3#, acquired needle-shape coke raw material pitch 3#Needle coke 3 is obtained through coking and calcine technology#, Pianguan County's microstructure is as schemed
Shown in 3.
Example IV:
Take coalite tar in 200g to be placed in reaction kettle, vacuum distillation isolates heavy component to 340 DEG C, by pyridine and
Chloroform 7:3 in mass ratio is uniformly mixed and obtains mixed solvent, and the above-mentioned heavy component isolated is sent into reaction kettle, heating
It is stirred evenly to 60 DEG C, then mixed solvent is added into reaction kettle, the mass ratio of mixed solvent and heavy component is 2:1,60
3h is stirred at DEG C, stops stirring stratification 6h at 60 DEG C, high reaction activity substance is isolated using the method for filtering, will be removed
The clarified solution obtained after high reaction activity substance is parsed, and unreacted mixed solvent is parsed, and obtains needle-shape coke raw material drip
Blueness 4#, acquired needle-shape coke raw material pitch 4#Needle coke 4 is obtained through coking and calcine technology#, Pianguan County's microstructure such as Fig. 4 institute
Show.
Embodiment five
Take coalite tar in 200g to be placed in reaction kettle, thin film evaporation isolates heavy component to 280 DEG C, by acetone and
Hexane 8:2 in mass ratio is uniformly mixed and obtains mixed solvent, and the above-mentioned heavy component isolated is sent into reaction kettle, is heated to 80
It DEG C stirs evenly, then mixed solvent is added into reaction kettle, the mass ratio of mixed solvent and heavy component is 3:1, at 80 DEG C
4h is stirred, stops stirring stratification 4h at 80 DEG C, high reaction activity substance is isolated using the method for overflow, will be removed high anti-
It answers the clarified solution obtained after active material to be parsed, parses unreacted mixed solvent, obtain needle-shape coke raw material pitch 5#,
Acquired needle-shape coke raw material pitch 5#Needle coke 5 is obtained through coking and calcine technology#, Pianguan County's microstructure is as shown in Figure 5.
Embodiment six
Take coalite tar in 200g to be placed in reaction kettle, thin film evaporation isolates heavy component to 300 DEG C, by kerosene and
Coking heavy oil 5:5 in mass ratio is uniformly mixed and obtains mixed solvent, and the above-mentioned heavy component isolated is sent into reaction kettle, heating
It is stirred evenly to 160 DEG C, then mixed solvent is added into reaction kettle, the mass ratio 2:1 of mixed solvent and heavy component, 160
4h is stirred at DEG C, stops stirring stratification 5h at 160 DEG C, high reaction activity substance is isolated using the method for suction filtration, will be removed
It goes the clarified solution obtained after high reaction activity substance to be parsed, parses unreacted mixed solvent, obtain needle-shape coke raw material
Pitch 6#, acquired needle-shape coke raw material pitch 6#Needle coke 6 is obtained through coking and calcine technology#, Pianguan County's microstructure such as Fig. 6
It is shown.
Above-described embodiment shows to be refined using suitable technique centering coalite tar, and the coke polarisation of preparation is aobvious
Micro-structure is mostly fiber and big chip architecture, hence it is evident that better than the thin mosaic texture of coke obtained by the direct coking of middle coalite tar
(see Fig. 7).
The above described is only a preferred embodiment of the present invention, being not that the invention has other forms of limitations, appoint
What those skilled in the art changed or be modified as possibly also with the technology contents of the disclosure above equivalent variations etc.
Imitate embodiment.But without departing from the technical solutions of the present invention, according to the technical essence of the invention to above embodiments institute
Any simple modification, equivalent variations and the remodeling made, still fall within the protection scope of technical solution of the present invention.
Claims (6)
1. a kind of method that middle coalite tar prepares needle coke, which comprises the steps of:
Middle coalite tar is obtained into heavy component through distillation, polar solvent, nonpolar solvent, polar solvent and nonpolarity is molten
Two kinds therein of the mixture of agent is uniformly mixed for 1:10~10:1 obtains mixed solvent in mass ratio, by middle coalite tar
Heavy component is sent into reaction kettle, is heated to 60~200 DEG C and stirs evenly, then mixed solvent is added into reaction kettle, the mixing
The mass ratio of solvent and heavy component is 0.5:1~3:1,1~20h is stood after 50~200 DEG C of 1~10h of stirring, using physics
Isolated method removes high reaction activity substance, will remove the clarified solution obtained after high reaction activity substance and parses, parses
Unreacted mixed solvent in clarified solution out, obtains needle-shape coke raw material pitch, by the needle-shape coke raw material pitch through coking and
Calcine technology obtains needle coke.
2. the method that a kind of middle coalite tar according to claim 1 prepares needle coke, which is characterized in that the distillation
For one or more of air-distillation, vacuum distillation, thin film evaporation.
3. the method that a kind of middle coalite tar according to claim 1 prepares needle coke, which is characterized in that the polarity
Solvent is methanol, ethyl alcohol, acetic acid, pyridine, acetone, chloroform, propyl alcohol or tetrahydrofuran.
4. the method that a kind of middle coalite tar according to claim 1 prepares needle coke, which is characterized in that the non-pole
Property solvent be benzene, toluene, carbon tetrachloride, dichloroethanes, chloroform, n-hexane, hexane or heptane.
5. the method that a kind of middle coalite tar according to claim 1 prepares needle coke, which is characterized in that the polarity
The mixture of solvent and nonpolar solvent is kerosene, wax oil, washing oil, a carbolineum, anthracene oil, naphtalene oil, carbolic oil or coking heavy oil.
6. the method that a kind of middle coalite tar according to claim 1 prepares needle coke, which is characterized in that the physics
Isolated method is one or more of overflow, filtering, suction filtration.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111013626A (en) * | 2019-12-18 | 2020-04-17 | 中钢集团鞍山热能研究院有限公司 | Monoatomic metal graphene catalyst based on needle coke and preparation method thereof |
| CN113637493A (en) * | 2021-08-26 | 2021-11-12 | 西北大学 | Method for preparing needle coke by using component blended medium-low temperature coal tar pitch raw material |
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| CN111013626A (en) * | 2019-12-18 | 2020-04-17 | 中钢集团鞍山热能研究院有限公司 | Monoatomic metal graphene catalyst based on needle coke and preparation method thereof |
| CN113637493A (en) * | 2021-08-26 | 2021-11-12 | 西北大学 | Method for preparing needle coke by using component blended medium-low temperature coal tar pitch raw material |
| CN113637493B (en) * | 2021-08-26 | 2022-09-02 | 西北大学 | Method for preparing needle coke by using component blended medium-low temperature coal tar pitch raw material |
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