CN109135789B - Method for preparing needle coke from medium-low temperature coal tar - Google Patents
Method for preparing needle coke from medium-low temperature coal tar Download PDFInfo
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- CN109135789B CN109135789B CN201810932497.9A CN201810932497A CN109135789B CN 109135789 B CN109135789 B CN 109135789B CN 201810932497 A CN201810932497 A CN 201810932497A CN 109135789 B CN109135789 B CN 109135789B
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- needle coke
- coal tar
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- temperature coal
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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
Abstract
A method for preparing needle coke from medium-low temperature coal tar comprises the following steps: distilling medium-low temperature coal tar to obtain a heavy component, uniformly mixing two of a polar solvent, a non-polar solvent, a mixture of the polar solvent and the non-polar solvent according to a mass ratio of 1: 10-10: 1 to obtain a mixed solvent, feeding the heavy component of the medium-low temperature coal tar into a reaction kettle, heating to 60-200 ℃, uniformly stirring, adding the mixed solvent into the reaction kettle, stirring at 50-200 ℃ for 1-10 h, standing for 1-20 h, removing high-reaction activity substances by adopting a physical separation method, resolving a clarified liquid obtained after removing the high-reaction activity substances, resolving out unreacted mixed solvent in the clarified liquid to obtain needle coke raw material pitch, and coking and calcining the needle coke raw material pitch to obtain needle coke. The method has the advantages of simple process, mild reaction conditions, low requirements on equipment, no need of high temperature and high pressure, strong operability and low cost.
Description
Technical Field
The invention relates to the field of medium and low temperature coal tar deep processing, in particular to a method for preparing needle coke from medium and low temperature coal tar.
Background
With the increasing shortage of petroleum resources, the processing and utilization of coal tar are regarded as important. Coal tar comprises high-temperature coal tar, medium-temperature coal tar and low-temperature coal tar, and the processing technology of the high-temperature coal tar is mature at present and is widely applied, such as being used as a binder or preparing needle coke when preparing isotropic graphite materials. The medium-low temperature coal tar is a liquid product obtained in the semi-coke production process, mainly takes low-rank coal such as non-caking coal or weakly caking coal and the like as raw materials, and is a product obtained through low-temperature dry distillation, wherein the dry distillation temperature is generally 650-750 ℃, the product mainly contains aromatic hydrocarbon, alkane, phenols, unsaturated hydrocarbon and the like, the aromatic content is low, and the application is less. A large amount of medium-low temperature coal tar byproducts are generated in the coal chemical industry of China every year, and due to the lack of a good recovery method, most of the coal tar byproducts cannot be recycled and burnt as fuels, so that the environment is polluted, and a large amount of resources are wasted. If the medium and low temperature coal tar can be used for producing the needle coke, the medium and low temperature coal tar can be effectively utilized, the preparation cost of the needle coke can be reduced, and the method has remarkable economic benefit and obvious social benefit.
The needle coke is a high-quality material for manufacturing high-power and ultrahigh-power electrodes, and the manufactured electrodes have the advantages of strong thermal shock resistance, high mechanical strength, good oxidation resistance, low electrode consumption, large current density and the like. At present, needle coke is widely used in high-tech fields such as electric furnace steelmaking, manufacturing of nuclear reactor deceleration materials, manufacturing of ultra-high power electrodes for rocket launching and the like. The raw materials industrially used for producing needle coke mainly include catalytic cracking clarified oil, petroleum heavy oil, ethylene tar, coal tar and the like, and needle coke can be classified into oil-based needle coke and coal-based needle coke according to the source of the raw materials, but any needle coke has certain requirements on the raw materials. In general, the raw material of needle coke is required to have high aromatic hydrocarbon content, but does not contain polycyclic macromolecular aromatic hydrocarbon, and has low heteroatom content, low metal content, low ash content and low asphaltene content. In addition, the needle coke raw material is required to have higher thermal stability, that is, the content of the high-reactivity components excited by heating in the raw material is low, so that the raw material is favorable for maintaining a carbonization rate which is not too fast in the thermal conversion process, and a better fibrous mesophase structure and a large flaky mesophase structure are formed, and the structures are typical microstructures of the needle coke.
In recent years, along with the development of the work of melting and resolving the capacity of crude steel in the steel industry, completely shutting down and dismantling the capacity of 1 hundred million tons of power frequency furnaces and medium frequency furnaces, and the like, and the continuous improvement of the national requirements on energy conservation and consumption reduction in the steel making process, the electric furnace steel making is developed more and more quickly in China, the demand of ultrahigh power electrodes is driven, the demand of needle coke is correspondingly increased obviously, the price of the needle coke is increased obviously, and the calcined coke is increased to 3.5-4 ten thousand/ton from the original 4000 yuan/ton. Meanwhile, with the application of the needle coke made in China in the field of lithium battery cathode materials, the needle coke has higher requirements on the aspect of cathode materials. The annual demand for needle coke in the field of negative electrode materials is expected to break through 20 million tons by 2020. The demand for needle coke will continue to grow in the coming years. Therefore, the method has important significance for preparing high-quality needle coke with wide application and short supply and demand based on the medium-low temperature coal tar which is cheap and easy to obtain and has rich yield as the raw material.
Disclosure of Invention
The invention aims to provide a method for preparing needle coke from medium-low temperature coal tar, which has the advantages of simple process, mild reaction conditions, low requirement on equipment, no need of high temperature and high pressure, strong operability and low cost. The process method not only expands the range of the raw materials of the needle coke and reduces the production cost of the needle coke, but also provides a new approach and a new method for solving the problems of treatment and utilization of medium and low temperature coal tar. The needle coke prepared by the method can be used for high-power and ultrahigh-power electrode materials, lithium ion battery cathode materials and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing needle coke from medium-low temperature coal tar comprises the following steps:
distilling medium-low temperature coal tar to obtain a heavy component, uniformly mixing two of a polar solvent, a non-polar solvent, a mixture of the polar solvent and the non-polar solvent according to a mass ratio of 1: 10-10: 1 to obtain a mixed solvent, feeding the heavy component of the medium-low temperature coal tar into a reaction kettle, heating to 60-200 ℃, uniformly stirring, adding the mixed solvent into the reaction kettle, stirring at 50-200 ℃ for 1-10 h, standing for 1-20 h, removing high-reaction activity substances by adopting a physical separation method, resolving a clear liquid obtained after removing the high-reaction activity substances, resolving unreacted mixed solvent in the clear liquid to obtain needle coke raw material pitch, and coking and calcining the needle coke raw material pitch to obtain needle coke.
The distillation is one or more of atmospheric distillation, reduced pressure distillation and thin film evaporation.
The polar solvent is methanol, ethanol, acetic acid, pyridine, acetone, chloroform, propanol or tetrahydrofuran.
The nonpolar solvent is benzene, toluene, carbon tetrachloride, dichloroethane, chloroform, n-hexane, hexane or heptane.
The mixture of the polar solvent and the non-polar solvent is kerosene, wax oil, wash oil, mono-anthracene oil, di-anthracene oil, naphthalene oil, phenol oil or coker heavy oil.
The physical separation method is one or more of overflow, filtration and suction filtration.
Compared with the prior art, the invention has the beneficial effects that:
the method has the advantages of simple process, mild reaction conditions, low requirements on equipment, no need of high temperature and high pressure, strong operability and low cost. The method expands the range of raw materials of the needle coke, reduces the production cost of the needle coke, provides a new approach and a new method for treating medium and low temperature coal tar, and effectively utilizes resources.
Drawings
FIG. 1 is a partial microscopic structure of a needle coke produced in example 1 of the present invention.
FIG. 2 is a partial microscopic structure of the needle coke produced in example 2 of the present invention.
FIG. 3 is a partial microscopic structure of a needle coke produced in example 3 of the present invention.
FIG. 4 is a partial microscopic structure of the needle coke prepared in example 4 of the present invention.
FIG. 5 is a partial microscopic structure of the needle coke produced in example 5 of the present invention.
FIG. 6 is a partial microscopic structure of the needle coke produced in example 6 of the present invention.
FIG. 7 is a microscopic structure diagram of the coke produced by the direct coking of medium and low temperature coal tar.
Detailed Description
The present invention is described in detail below, but it should be noted that the practice of the present invention is not limited to the following embodiments.
A method for preparing needle coke from medium-low temperature coal tar comprises the following steps:
distilling medium-low temperature coal tar to obtain a heavy component, uniformly mixing two of a polar solvent, a non-polar solvent, a mixture of the polar solvent and the non-polar solvent according to a mass ratio of 1: 10-10: 1 to obtain a mixed solvent, feeding the heavy component of the medium-low temperature coal tar into a reaction kettle, heating to 60-200 ℃, uniformly stirring, adding the mixed solvent into the reaction kettle, stirring at 50-200 ℃ for 1-10 h, standing for 1-20 h, removing high-reaction activity substances by adopting a physical separation method, resolving a clear liquid obtained after removing the high-reaction activity substances, resolving unreacted mixed solvent in the clear liquid to obtain needle coke raw material pitch, and coking and calcining the needle coke raw material pitch to obtain needle coke.
The medium-low temperature coal tar is low-temperature coal tar or medium-temperature coal tar or a mixture of the two. The low-temperature coal tar is an oily product obtained by low-temperature dry distillation of coal or oil shale. The medium-temperature coal tar is an oily product obtained by performing medium-temperature dry distillation on coal or oil shale.
The distillation is one or more of atmospheric distillation, reduced pressure distillation and thin film evaporation.
The polar solvent is methanol, ethanol, acetic acid, pyridine, acetone, chloroform, propanol or tetrahydrofuran.
The nonpolar solvent is benzene, toluene, carbon tetrachloride, dichloroethane, chloroform, n-hexane, hexane or heptane.
The mixture of the polar solvent and the non-polar solvent is kerosene, wax oil, wash oil, mono-anthracene oil, di-anthracene oil, naphthalene oil, phenol oil or coker heavy oil.
The physical separation method is one or more of overflow, filtration and suction filtration.
The first embodiment is as follows:
putting 200g of medium-low temperature coal tar into a reaction kettle, distilling at normal pressure to 360 ℃ to separate out heavy components, uniformly mixing methanol and benzene according to the mass ratio of 7:3 to obtain a mixed solvent, feeding the separated heavy components into the reaction kettle, heating to 60 ℃, uniformly stirring, adding the mixed solvent into the reaction kettle, stirring for 3 hours at 60 ℃, stopping stirring, standing for layering for 3 hours at 60 ℃, separating out high-reaction-activity substances by adopting a filtering method, resolving clarified liquid obtained after removing the high-reaction-activity substances, resolving out unreacted mixed solvent to obtain needle coke raw material asphalt 1#The obtained needle coke raw material asphalt 1#Needle coke 1 is obtained by coking and calcining process#The off-set microstructure is shown in FIG. 1.
Example two:
200g of medium-low temperature coal tar is taken and placed in a reaction kettle, the normal pressure distillation is carried out to 380 ℃, heavy components are separated, and acetic acid and heptane are mixed according to the mass ratio of 5:5, uniformly mixing to obtain a mixed solvent, feeding the separated heavy component into a reaction kettle, heating to 90 ℃, uniformly stirring, adding the mixed solvent into the reaction kettle, wherein the mass ratio of the mixed solvent to the heavy component is 1:2, stirring for 2 hours at 90 ℃, stopping stirring, standing and layering for 4 hours at 90 ℃, separating out high-reaction activity substances by adopting an overflow method, resolving a clear solution obtained after removing the high-reaction activity substances, resolving out unreacted mixed solvent, and obtaining needle coke raw material asphalt 2#Obtaining needle cokeRaw material asphalt 2#Needle coke 2 is obtained by coking and calcining process#The off-set microstructure is shown in FIG. 2.
Example three:
putting 200g of medium-low temperature coal tar into a reaction kettle, distilling under reduced pressure to 320 ℃ to separate out heavy components, uniformly mixing wax oil and anthracene oil according to the mass ratio of 4:6 to obtain a mixed solvent, sending the separated heavy components into the reaction kettle, heating to 140 ℃, uniformly stirring, adding the mixed solvent into the reaction kettle, stirring the mixed solvent and the heavy components according to the mass ratio of 1:1 at 140 ℃ for 4 hours, stopping stirring, standing at 140 ℃ for layering for 5 hours, separating out high-reaction-activity substances by adopting a suction filtration method, resolving clarified liquid obtained after removing the high-reaction-activity substances, resolving out unreacted mixed solvent to obtain needle coke raw material asphalt 3#The obtained needle coke raw material asphalt 3#Needle coke 3 is obtained by coking and calcining process#The off-set microstructure is shown in FIG. 3.
Example four:
putting 200g of medium-low temperature coal tar into a reaction kettle, distilling under reduced pressure to 340 ℃ to separate out heavy components, uniformly mixing pyridine and chloroform according to the mass ratio of 7:3 to obtain a mixed solvent, sending the separated heavy components into the reaction kettle, heating to 60 ℃, uniformly stirring, adding the mixed solvent into the reaction kettle, wherein the mass ratio of the mixed solvent to the heavy components is 2:1, stirring for 3 hours at 60 ℃, stopping stirring, standing and layering for 6 hours at 60 ℃, separating out high-reaction activity substances by adopting a filtering method, resolving clarified liquid obtained after removing the high-reaction activity substances, resolving out unreacted mixed solvent, and obtaining needle-shaped coke raw material asphalt 4#The obtained needle coke raw material asphalt 4#Needle coke 4 is obtained by coking and calcining process#The off-set microstructure is shown in FIG. 4.
EXAMPLE five
Putting 200g of medium-low temperature coal tar into a reaction kettle, evaporating a film to 280 ℃ to separate out heavy components, uniformly mixing acetone and hexane according to the mass ratio of 8:2 to obtain a mixed solvent, feeding the separated heavy components into the reaction kettle, heating to 80 ℃, and stirringUniformly mixing, adding a mixed solvent into the reaction kettle, wherein the mass ratio of the mixed solvent to the heavy component is 3:1, stirring for 4 hours at 80 ℃, stopping stirring, standing and layering for 4 hours at 80 ℃, separating out high-reaction-activity substances by adopting an overflow method, resolving clarified liquid obtained after removing the high-reaction-activity substances, resolving out unreacted mixed solvent, and obtaining needle coke raw material asphalt 5#The obtained needle coke raw material asphalt 5#Needle coke 5 is obtained by coking and calcining process#The off-set microstructure is shown in FIG. 5.
EXAMPLE six
Putting 200g of medium-low temperature coal tar into a reaction kettle, evaporating a film to 300 ℃ to separate out heavy components, uniformly mixing kerosene and coking heavy oil according to the mass ratio of 5:5 to obtain a mixed solvent, feeding the separated heavy components into the reaction kettle, heating to 160 ℃, uniformly stirring, adding the mixed solvent into the reaction kettle, stirring the mixed solvent and the heavy components according to the mass ratio of 2:1 at 160 ℃ for 4 hours, stopping stirring, standing at 160 ℃ for layering for 5 hours, separating out high-reaction active substances by adopting a suction filtration method, resolving clarified liquid obtained after removing the high-reaction active substances to obtain an unreacted mixed solvent, and obtaining needle-shaped coke raw material asphalt 6#The obtained needle coke raw material asphalt 6#Needle coke 6 is obtained by coking and calcining process#The off-set microstructure is shown in FIG. 6.
The above examples show that the suitable process for refining medium and low temperature coal tar is adopted, and the prepared coke polarization microstructure is mostly fiber and large sheet structure, which is obviously superior to the fine mosaic structure of coke prepared by directly coking medium and low temperature coal tar (see fig. 7).
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (1)
1. A method for preparing needle coke from medium-low temperature coal tar is characterized by comprising the following steps:
distilling medium-low temperature coal tar at 280-380 ℃ to obtain a heavy component, uniformly mixing a polar solvent and a nonpolar solvent according to a mass ratio of 1: 10-10: 1 to obtain a mixed solvent, feeding the heavy component of the medium-low temperature coal tar into a reaction kettle, heating to 60-200 ℃, uniformly stirring, adding the mixed solvent into the reaction kettle, wherein the mass ratio of the mixed solvent to the heavy component is 0.5: 1-3: 1, stirring at 50-200 ℃ for 1-10 h, standing for 1-20 h, removing high-reaction-activity substances by adopting a physical separation method, resolving a clarified liquid obtained after removing the high-reaction-activity substances to obtain an unreacted mixed solvent in the clarified liquid, obtaining needle coke raw material asphalt, and coking and calcining the needle coke raw asphalt to obtain needle coke; the physical separation method is one or more of overflow, filtration and suction filtration;
the polar solvent is methanol, ethanol, acetic acid, pyridine, acetone, chloroform, propanol or tetrahydrofuran;
the nonpolar solvent is benzene, toluene, carbon tetrachloride, dichloroethane, chloroform, n-hexane, hexane or heptane;
the distillation is one or more of atmospheric distillation, reduced pressure distillation and thin film evaporation.
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| CN111013626B (en) * | 2019-12-18 | 2023-04-28 | 中钢集团鞍山热能研究院有限公司 | Single-atom metal graphene catalyst based on needle coke and preparation method thereof |
| 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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