CN116536070B - Method for preparing mesophase pitch by hydrogenating coal tar pitch components - Google Patents
Method for preparing mesophase pitch by hydrogenating coal tar pitch componentsInfo
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- CN116536070B CN116536070B CN202310544069.XA CN202310544069A CN116536070B CN 116536070 B CN116536070 B CN 116536070B CN 202310544069 A CN202310544069 A CN 202310544069A CN 116536070 B CN116536070 B CN 116536070B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/02—Working-up pitch, asphalt, bitumen by chemical means reaction
- C10C3/023—Working-up pitch, asphalt, bitumen by chemical means reaction with inorganic compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Working-Up Tar And Pitch (AREA)
Abstract
The invention discloses a method for preparing mesophase pitch by hydrogenating coal tar pitch components, which comprises the steps of sequentially obtaining A, B and C components or A, B, C and D components or A, B, C, D and E components from coal tar pitch by adopting a progressive extraction method, adding a hydrogen-supplying solvent and a catalyst into heavy components separated from the coal tar pitch, carrying out hydrogenation treatment to obtain hydrogenated heavy components, mixing the hydrogenated heavy components and unhydrogenated components according to a certain proportion to obtain modified pitch, and carrying out thermal polycondensation reaction on the modified pitch to obtain mesophase pitch. The modified asphalt provided by the invention has a molecular composition suitable for preparing mesophase asphalt, the molecular weight range is reasonable, the distribution is concentrated, the anisotropic content in the prepared mesophase asphalt is high, the optical structure is good, the modified asphalt is rich in a wide-area streamline structure, and the modified asphalt is a high-quality precursor for preparing carbon materials such as carbon fibers, needle coke and the like.
Description
Technical Field
The invention belongs to the field of deep processing of coal tar pitch, and particularly relates to a method for preparing mesophase pitch by hydrogenating a coal tar pitch component.
Background
The heavy aromatic compound can form mesophase pitch through liquid phase carbonization, and has anisotropic optical properties and a certain rheological property. The planar aromatic macromolecules which are regularly arranged in the mesophase pitch are easy to be piled up and arranged according to the structure of graphite under the high-temperature heat treatment condition, so that the mesophase pitch-based carbon material has a plurality of excellent performances. Therefore, the mesophase pitch is an excellent precursor for preparing high-elasticity carbon fibers, high-specific-surface-area activated carbon, ultra-high-power graphite electrodes and other advanced functional materials.
The coal tar pitch has high yield, low cost and high aromatic hydrocarbon content, and is widely applied to preparing mesophase pitch. However, coal tar pitch has a complex composition, high impurity content, and contains quinoline insoluble or highly reactive components, which are susceptible to excessive polycondensation during carbonization, which is detrimental to the formation of mesophase pitch molecules.
At present, in order to improve the hydrogen-carbon ratio, remove quinoline insoluble substances (QI) and adjust molecular composition, a method for preparing an intermediate phase aiming at modifying a coal tar pitch raw material is mainly hydrogenation modification. The method for preparing the intermediate phase asphalt by using coal tar pitch as a raw material through hydrocatalysis-hydrogen supply treatment is disclosed in patent CN110699107A, and the intermediate phase asphalt prepared by the method has moderate softening point and high intermediate phase content, but the preparation method needs secondary hydrogenation of the raw material, has complex process, uses a large amount of hydrogen supply solvent, is difficult to control the hydrogenation depth and has higher preparation cost.
In the hydrogenation reaction process, because the molecular composition distribution of the coal tar pitch is wider, light components are easy to excessively hydrogenate, and the hydrogenation depth of heavy components is insufficient, the problems of low yield of an intermediate phase, non-ideal optical structure and the like are caused. The patent on the aspects of accurately adjusting the raw material composition, preventing excessive hydrogenation and the like for coal tar pitch hydrogenation is rarely related.
Disclosure of Invention
This section is intended to outline some aspects of embodiments of the application and to briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section as well as in the description of the application and in the title of the application, which may not be used to limit the scope of the application.
The present invention has been made in view of the above and/or problems occurring in the prior art.
Therefore, the invention aims to overcome the defects in the prior art and provide a method for preparing mesophase pitch by hydrogenating coal tar pitch components, which is characterized in that the components with different properties are obtained by gradually extracting the coal tar pitch, wherein heavy components are mixed with unhydrogenated components according to a certain proportion after hydrogenation, so that the molecular composition of the pitch is changed, the molecular weight distribution is proper, a naphthenic structure and an aliphatic side chain are added, stable growth and fusion of mesophase pellets are promoted, and the prepared mesophase pitch has high anisotropic phase content and is mainly of a wide-area streamline structure.
In order to solve the technical problems, the invention provides a method for preparing mesophase pitch by hydrogenating a coal tar pitch component, which comprises the following steps of,
Step-by-step extraction is carried out on the coal tar pitch by using different extractants to obtain A, B and C three components or A, B, C and D four components or A, B, C, D and E five components;
Adding hydrogen-supplying solvent into one or more of B, C, D or E components, mixing with a catalyst, and obtaining hydrogenated heavy components after hydrogenation treatment;
mixing the hydrogenated heavy component and the unhydrogenated component to obtain a modified asphalt;
and performing thermal condensation polymerization on the modified asphalt to obtain the mesophase pitch.
As a preferred embodiment of the method of the present invention, the step-wise extraction of coal tar pitch with different extractants comprises,
Adding an extractant a into the coal tar pitch, standing after extraction, and separating raffinate 1 and supernatant to obtain an extract, and recovering the extractant a through reduced pressure distillation to obtain a component A;
Vacuum drying the raffinate 1 to constant weight, mixing with the extractant B, standing after extraction, separating the raffinate 2 and supernatant to obtain an extract, and recovering the extractant B through reduced pressure distillation to obtain a component B;
and (3) vacuum drying the raffinate 2 to constant weight, mixing with the extractant C, standing after extraction, separating the raffinate and the supernatant to obtain an extract, and recovering the extractant C through reduced pressure distillation to obtain the component C.
In the step, four extractants are adopted in the step-by-step extraction process to sequentially obtain A, B, C and D four components, and five extractants are adopted to sequentially obtain A, B, C, D and E five components.
As a preferred embodiment of the process according to the invention, the extractant is selected from the group consisting of n-hexane, n-heptane, toluene, pyridine, chloroform, acetone, tetrahydrofuran, quinoline, anthracene oil, wash oil and naphthalene oil.
The method is characterized by comprising the step-by-step extraction, wherein the mass ratio of the extractant to the asphalt is 5:1-20:1, and the extraction condition is that the stirring is carried out for 50-90 min at the temperature of 50-120 ℃.
As a preferable scheme of the method, the hydrogen supply solvent is one or a mixture of more than two of dihydropyrene, dihydroanthracene, tetrahydroanthracene, dihydronaphthalene, tetrahydronaphthalene, dihydrophenanthrene, octahydrophenanthrene, tetrahydroquinoline, coal direct liquefaction hydrogen supply solvent and coal tar distillate hydrogenation products;
the catalyst is one or a mixture of more than two of Fe 2O3、FeS2、ZnO、ZnCl2、SnO2, co, mo and Ni catalysts.
As a preferable scheme of the method, the hydrogen supply solvent is 5-60 wt% of the mass of the heavy components;
the hydrotreating is carried out under the condition of hydrogen or nitrogen of 2-8 MPa, and the temperature is 340-440 ℃.
As a preferred embodiment of the process according to the invention, the heavy components are mixed with unhydrogenated components, wherein,
When the coal tar pitch is extracted into 3 components, the mass ratio of the unhydrogenated components to the hydrogenated heavy components is 10% -20%, 20% -50% and 10% -40%;
when the coal tar pitch is extracted into 4 components, the mass ratio of the unhydrogenated components to the hydrogenated heavy components is 10% -20%, 20% -50%, 10% -30% and 10% -20%;
When the coal tar pitch is extracted into 5 components, the mass ratio of the unhydrogenated components to the hydrogenated heavy components is 10% -20%, 20% -50%, 10% -30%, 10% -20% and 10% -20%.
As a preferable scheme of the method, the thermal polycondensation process is to heat up to 320-480 ℃ at a heating rate of 0.5-5 ℃ per minute, and the heat preservation time is 3-15 h.
As a preferable scheme of the method, the modified asphalt is subjected to thermal polycondensation, wherein the stirring speed is 50-500 r/min, and the initial pressure of nitrogen is 0.1-5 MPa.
As a preferable scheme of the method, the mesophase pitch product is mesophase pitch with anisotropic phase content of more than or equal to 80%, wide-area streamline optical texture content of more than or equal to 60% and softening point of 120-380 ℃.
The invention has the beneficial effects that:
(1) The invention provides a method for preparing high-quality mesophase pitch by taking coal tar pitch as a raw material, adjusting the composition of the raw material through solvent extraction and separation of components, hydrogenation of heavy components and blending modification.
(2) According to the invention, components with different properties are obtained by extracting the coal tar pitch with an organic solvent and separating, so that impurities and high-reactivity substances in raw materials can be reduced, the thermal polycondensation reaction can be smoothly carried out, coking is inhibited, and the thermal stability of a system is improved.
(3) According to the invention, hydrogenation is carried out on heavy components of coal tar pitch to obtain hydrogenated heavy components, a naphthene structure and an alkyl side chain are introduced, active hydrogen is released in a thermal polycondensation reaction, excessive polycondensation of aromatic hydrocarbon molecules is effectively inhibited, mesophase pellets stably grow, and wide-area mesophase formation is facilitated.
(4) According to the invention, the modified asphalt is obtained after the unhydrogenated component and the hydrogenated heavy component are mixed, the molecular weight distribution of the modified asphalt is regulated, and a naphthene structure and an alkyl side chain are introduced, so that the thermal polycondensation reaction rate is regulated, the generation and development of a mesophase are promoted, and the content of the mesophase is promoted and the optical texture is improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art. Wherein:
FIG. 1 is a polarizing microscopic morphology of mesophase pitch prepared in example 1 of the present invention.
FIG. 2 is a polarizing microscopic morphology of mesophase pitch prepared in example 2 of the present invention.
FIG. 3 is a polarizing microscopic morphology of mesophase pitch prepared in example 3 of the present invention.
FIG. 4 is a process flow diagram of a method for preparing mesophase pitch by hydrogenating a coal tar pitch component in an embodiment of the present invention.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Further, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic can be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
The embodiment provides a method for preparing mesophase pitch by hydrogenating a coal tar pitch component, the process flow chart is shown in fig. 4, and the method comprises the following steps:
(1) Placing 100g of coal tar pitch and 500g of n-heptane into a beaker, stirring for 50min at a water bath temperature of 40 ℃, standing, separating raffinate 1 and supernatant, and distilling the obtained extract under reduced pressure to remove an organic solvent to obtain a component A;
Placing the raffinate 1 and 400g of toluene after vacuum drying for 24 hours into a beaker, stirring for 60 minutes in a water bath at 60 ℃, standing, separating the raffinate 2 and the supernatant, and removing the organic solvent from the obtained extract after reduced pressure distillation to obtain a component B;
placing the extract 2 dried in vacuum for 24 hours and 200g of tetrahydrofuran in a beaker, stirring for 60 minutes at the temperature of 70 ℃ in a water bath, standing, separating raffinate 3 and supernatant, and removing organic solvent after reduced pressure distillation of the obtained extract to obtain a component C;
Placing extract 3 dried in vacuum for 24h and 200g of quinoline in a beaker, stirring for 60min at 70 ℃ in water bath, standing, separating raffinate 4 and supernatant, distilling the obtained extract under reduced pressure, removing organic solvent to obtain component D, and drying raffinate 4 in vacuum for 24h to obtain component E;
(2) Putting 40g of component D,6g of tetrahydronaphthalene and 0.04g of cobalt-molybdenum catalyst into a reaction kettle, wherein the initial pressure of hydrogen is 4MPa, the stirring speed is 100 revolutions per minute, the temperature is raised to 390 ℃ at the temperature rising rate of 1.5 ℃ per minute, and the mixture is cooled to room temperature after keeping the temperature for 1h to obtain a hydrogenated component D1;
Putting 40g of component E,4g of tetrahydronaphthalene and 0.03g of cobalt-molybdenum catalyst into a reaction kettle, wherein the initial pressure of hydrogen is 4MPa, the stirring speed is 100 revolutions per minute, the temperature is raised to 410 ℃ at the temperature rising rate of 1.5 ℃ per minute, and the mixture is cooled to room temperature after keeping the temperature for 1h to obtain a hydrogenated component E1;
(3) 5g of component A, 12.5g of component B, 15g of component C, 10g of hydrogenated component D1 and 7.5g of hydrogenated component E1 are taken and placed in a beaker, and are stirred under strong magnetic force for 30min at the water bath of 90 ℃, and cooled to room temperature, so that modified asphalt is obtained;
(4) And (3) placing the modified asphalt into a reaction kettle, wherein the initial pressure of nitrogen is 0.5MPa, heating to 375 ℃ at the heating rate of 1.5 ℃ per minute, and keeping the temperature for 8 hours to obtain the mesophase asphalt.
The polarizing microscopic morphology of the prepared mesophase pitch is shown in fig. 1, and the measurement results of the anisotropic phase content and the optical structure composition are shown in table 1.
Example 2
The embodiment provides a method for preparing mesophase pitch by hydrogenating a coal tar pitch component, which comprises the following steps:
(1) Placing 100g of coal tar pitch and 500g of n-hexane in a beaker, stirring for 40min in a water bath, standing, separating raffinate 1 and supernatant, and distilling the obtained extract under reduced pressure to remove an organic solvent to obtain a component A;
Placing the raffinate 1 and 400g of toluene in a beaker, stirring for 40min at a water bath temperature of 60 ℃, standing, separating the raffinate 2 and the supernatant, and removing the organic solvent from the obtained extract by reduced pressure distillation to obtain a component B;
placing the raffinate 2 and 300g of chloroform into a beaker, stirring for 40min at a water bath temperature of 65 ℃, standing, separating the raffinate 3 and the supernatant, and removing the organic solvent from the obtained extract after reduced pressure distillation to obtain a component C;
placing the extract 3 and 200g of pyridine in a beaker, stirring for 50min at a water bath temperature of 70 ℃, standing, separating raffinate 4 and supernatant, distilling the obtained extract under reduced pressure, removing organic solvent to obtain a component D, and vacuum drying the raffinate 4 for 24h to obtain a component E;
(2) Putting 40g of component E,2g of dihydroanthracene and 0.03g of Fe 2O3 catalyst into a reaction kettle, wherein the initial pressure of hydrogen is 3MPa, the stirring speed is 100 revolutions per minute, heating to 400 ℃ at the heating rate of 1.5 ℃ per minute, keeping the temperature for 1h, and cooling to room temperature to obtain a hydrogenated component E1;
(3) 7.5g of component A, 10g of component B, 15g of component C, 10g of component D and 7.5g of hydrogenated component E1 are taken and placed in a beaker, and are stirred by strong magnetic force for 30min at the water bath of 90 ℃, and cooled to room temperature, so as to obtain modified asphalt;
(4) And (3) placing the modified asphalt into a reaction kettle, wherein the initial pressure of nitrogen is 0.5MPa, heating to 375 ℃ at the heating rate of 1.5 ℃ per minute, and keeping the temperature for 8 hours to obtain the mesophase asphalt.
The polarizing microscopic morphology of the obtained mesophase pitch is shown in fig. 2, and the measurement results of the anisotropic phase content and the optical structure composition are shown in table 1.
Example 3
The embodiment provides a method for preparing mesophase pitch by hydrogenating a coal tar pitch component, which comprises the following steps:
(1) Placing 100g of coal tar pitch and 500g of n-hexane in a beaker, stirring for 40min in a water bath, standing, separating raffinate 1 and supernatant, and distilling the obtained extract under reduced pressure to remove an organic solvent to obtain a component A;
Placing the raffinate 1 and 400g of toluene in a beaker, stirring for 40min at a water bath temperature of 60 ℃, standing, separating the raffinate 2 and the supernatant, and removing the organic solvent from the obtained extract by reduced pressure distillation to obtain a component B;
placing the raffinate 2 and 300g of chloroform into a beaker, stirring for 40min at a water bath temperature of 65 ℃, standing, separating the raffinate 3 and the supernatant, and removing the organic solvent from the obtained extract after reduced pressure distillation to obtain a component C;
placing the extract 3 and 200g of quinoline into a beaker, stirring for 50min at a water bath of 70 ℃, standing, separating raffinate 4 and supernatant, distilling the obtained extract under reduced pressure, removing organic solvent to obtain a component D, and vacuum drying the raffinate 4 for 24h to obtain a component E;
(2) Putting 40g of component D, 4g of tetrahydronaphthalene and 0.02g of cobalt-molybdenum catalyst into a reaction kettle, wherein the initial pressure of hydrogen is 5MPa, the stirring speed is 100 revolutions per minute, the temperature is raised to 400 ℃ at the temperature rising rate of 1.5 ℃ per minute, and the mixture is cooled to room temperature after keeping the temperature for 1h to obtain a hydrogenated component D1;
(3) 10g of component A, 17.5g of component B, 15g of component C and 11.5g of hydrogenated component D1 are taken and placed in a beaker, and are stirred by strong magnetic force for 15min at the water bath of 90 ℃, and cooled to room temperature, so as to obtain modified asphalt;
(4) And (3) placing the modified asphalt into a reaction kettle, wherein the initial pressure of nitrogen is 0.5MPa, heating to 375 ℃ at the heating rate of 1.5 ℃ per minute, and keeping the temperature for 7 hours to obtain the mesophase asphalt.
The polarizing microscopic morphology of the obtained mesophase pitch is shown in fig. 3, and the measurement results of the anisotropic phase content and the optical structure composition are shown in table 1.
Table 1 mesophase pitch content and optical structural composition prepared in examples 1 to 3
According to the method for preparing the mesophase pitch by hydrogenating the coal tar pitch components, disclosed by the invention, a controllable new path is provided for preparing the mesophase pitch with high added value by gradually extracting the coal tar pitch and hydrogenating the heavy components to a proper depth.
It should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted without departing from the spirit and scope of the technical solution of the present invention, and it should be covered in the scope of the present invention.
Claims (10)
1. A method for preparing mesophase pitch by hydrogenating a coal tar pitch component is characterized by comprising the steps of,
Step-by-step extraction is carried out on the coal tar pitch by using different extractants to obtain A, B and C three components or A, B, C and D four components or A, B, C, D and E five components;
Adding hydrogen-supplying solvent into one or more of B, C, D or E components, mixing with a catalyst, and obtaining hydrogenated heavy components after hydrogenation treatment;
mixing the hydrogenated heavy component and the unhydrogenated component to obtain a modified asphalt;
and performing thermal condensation polymerization on the modified asphalt to obtain the mesophase pitch.
2. The method of claim 1, wherein the step-wise extraction of coal tar pitch with different extractants comprises,
Adding an extractant a into the coal tar pitch, standing after extraction, and separating raffinate 1 and supernatant to obtain an extract, and recovering the extractant a through reduced pressure distillation to obtain a component A;
Vacuum drying the raffinate 1 to constant weight, mixing with the extractant B, standing after extraction, separating the raffinate 2 and supernatant to obtain an extract, and recovering the extractant B through reduced pressure distillation to obtain a component B;
Vacuum drying the raffinate 2 to constant weight, mixing with the extractant C, standing after extraction, separating the raffinate and the supernatant to obtain an extract, and recovering the extractant C through reduced pressure distillation to obtain a component C;
in the steps, A, B, C and D components are sequentially obtained when four extracting agents are adopted in the step-by-step extraction process, and A, B, C, D and E components are sequentially obtained when five extracting agents are adopted.
3. The method of claim 2, wherein the extractant is selected from the group consisting of n-hexane, n-heptane, toluene, pyridine, chloroform, acetone, tetrahydrofuran, quinoline, anthracene oil, wash oil, and naphthalene oil.
4. The method of claim 2 or 3, wherein the step-by-step extraction is performed under the condition that the mass ratio of the extractant to the asphalt is 5:1-20:1 and the extraction condition is that the stirring is performed for 50-90 min at the temperature of 50-120 ℃.
5. The method according to claim 1, wherein the hydrogen-supplying solvent is one or a mixture of two or more of dihydropyrene, dihydroanthracene, tetrahydroanthracene, dihydronaphthalene, tetrahydronaphthalene, dihydrophenanthrene, octahydrophenanthrene, tetrahydroquinoline;
The catalyst is one or a mixture of two or more of Fe 2 O3、FeS2、ZnO、ZnCl2、SnO2, co, mo and Ni catalysts.
6. The method according to claim 5, wherein the hydrogen-donating solvent is 5wt% to 60wt% of the mass of the heavy component;
the hydrotreating is carried out under the condition of hydrogen or nitrogen of 2-8 MPa, and the temperature is 340-440 ℃.
7. The method according to claim 1, wherein the hydrogenated heavy component and the unhydrogenated component are mixed, wherein,
When the coal tar pitch is separated into 3 components, the mass ratio of the unhydrogenated components to the hydrogenated heavy components is 10% -20%, 20% -50% and 10% -40%;
when the coal tar pitch is separated into 4 components, the mass ratio of the unhydrogenated components to the hydrogenated heavy components is 10% -20%, 20% -50%, 10% -30% and 10% -20%;
When the coal tar pitch is separated into 5 components, the mass ratio of the unhydrogenated components to the hydrogenated heavy components is 10% -20%, 20% -50%, 10% -30%, 10% -20% and 10% -20%.
8. The method of claim 1, wherein the thermal polycondensation process is performed at a temperature rising rate of 0.5-5 ℃ per minute to 320-480 ℃ and a heat preservation time of 3-15 h.
9. The method of claim 1, wherein the modified asphalt is subjected to thermal polycondensation, wherein the stirring rate is 50-500 r/min, and the initial pressure of nitrogen is 0.1-5 MPa.
10. The method of claim 1, wherein the mesophase pitch product is a mesophase pitch having an anisotropic phase content of at least 80%, a wide area streamline optical texture content of at least 60%, and a softening point of 120-380 ℃.
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