KR20210012074A - The manufacturing method for petroleum based high softning point pitch - Google Patents

Abstract

The present invention relates to a manufacturing method of a petroleum-based high-softening-point pitch, and more specifically, to the manufacturing method of a petroleum-based high-softening-point having low quinolone insoluble (QI) content, capable of adjusting beta-resin content, and having low heteroatom content such as nitrogen, sulfur, and oxygen.

Description

The manufacturing method of petroleum-based high softening point pitch {THE MANUFACTURING METHOD FOR PETROLEUM BASED HIGH SOFTNING POINT PITCH}

The present invention relates to a method of manufacturing a petroleum-based high softening point pitch, and more particularly, a quinoline insoluble content (QI) content is low, a beta resin content can be adjusted, and the content of heteroatoms such as nitrogen, sulfur and oxygen is It relates to a method of manufacturing a small petroleum-based high softening point pitch.

In general, coal tar pitch is used for various carbon electrodes and graphite molded articles. However, coal tar pitch has a problem due to pretreatment problems and environmental regulations, and a high softening point pitch derived from petroleum is used instead of coal tar pitch.

The high softening point pitch derived from petroleum is used for coke, carbon fiber, negative electrode material for lithium secondary batteries, pitch for negative electrode material coating, Si-based composite negative electrode material, or various additives. However, the petroleum-derived high softening point pitch poses a problem with the content of quinoline insolubles for use as a carbon product. There has been a problem that the performance of the negative electrode material to which the high softening point pitch derived from petroleum is applied is deteriorated. In addition, since the petroleum-derived high softening point pitch has a high content of heterogeneous elements, there is a problem that the physical properties of carbon are deteriorated.

Therefore, the content of quinoline insoluble and heterogeneous elements is small, and a high softening point pitch suitable for use as a carbon material is required.

An object of the present invention is to provide a method for producing a petroleum-based high softening point pitch having a low quinoline insoluble content, a beta resin content, and a low content of heteroatoms such as nitrogen, sulfur, and oxygen.

In order to solve the above technical problem, according to one aspect of the present invention, (a) the content of indene and indene derivatives is 3% by weight or less by pretreating the petroleum-based residual oil raw material, and the content of styrene and styrene derivatives is Preparing a petroleum-based residual oil having a softening point of less than or equal to 0.3% by weight and a softening point of 20°C to 150°C. There is provided a method of manufacturing a petroleum-based high softening point pitch comprising a reduced pressure heat treatment step of heating in a reduced pressure state.

The manufacturing method of the petroleum-based high softening point pitch according to the present invention can significantly reduce the high quinoline insoluble matter content, which is a problem in the high softening point pitch, it is possible to control the beta resin content helpful in the carbonization yield, nitrogen, sulfur and It is possible to manufacture a high-quality petroleum-based high softening point pitch with a reduced content of heteroatoms such as oxygen.

In addition, the method of manufacturing a petroleum-based high-softening point pitch according to the present invention does not require a catalyst and high-pressure conditions, so a separate process for removing the catalyst is not required, and an expensive high-pressure container is not used. Softening point pitch can be produced.

In addition, the manufacturing method of the petroleum-based high softening point pitch according to the present invention does not use a peroxide-based compound, so it is economical, and there is no risk of explosion during the manufacturing process and does not cause environmental pollution.

In addition, the petroleum-based high softening point pitch manufactured according to the method of manufacturing a petroleum-based high softening point pitch according to the present invention has a remarkably reduced content of quinoline insolubles, as an example of product application. Capacity, life, and charging/discharging efficiency can be increased.

1 is a schematic process flow diagram of a method of manufacturing a petroleum-based high softening point pitch according to an embodiment of the present invention.

Advantages and features of the present invention, and a method of achieving them will become apparent with reference to the following embodiments. However, the present invention is not limited to the embodiments disclosed below, but will be implemented in a variety of different forms, only these embodiments make the disclosure of the present invention complete, and common knowledge in the technical field to which the present invention pertains. It is provided to completely inform the scope of the invention to those who have, and the invention is only defined by the scope of the claims.

Hereinafter, a method of manufacturing a petroleum-based high softening point pitch according to the present invention will be described in detail.

According to an aspect of the present invention, (a) the content of indene and indene derivatives is 3% by weight or less by pretreating the petroleum-based residual oil raw material, the content of styrene and styrene derivatives is 0.3% by weight or less, and the softening point is 20 Preparing a petroleum-based residual oil of ℃ to 150 ℃ step (S1), (b) the result of the oxidation heat treatment step (S2), (c) (b) of heating while mixing an oxidizing gas in the petroleum-based residual oil There is provided a method of manufacturing a petroleum-based high softening point pitch comprising a reduced pressure heat treatment step (S3) of heating in a reduced pressure state.

First, in the manufacturing method of the present invention, (a) the petroleum-based residual oil raw material is pretreated so that the content of indene and indene derivative is 3% by weight or less, the content of styrene and styrene derivative is 0.3% by weight or less, and the softening point is 20 It includes a step (S1) of preparing a petroleum-based residual oil of ℃ to 150 ℃.

In general, petroleum-based residual oil has a higher carbonization yield and aromatic ratio than light oil, so it can be suitably used as a raw material for carbon materials. However, petroleum-based residual oils have different chemical and physical properties depending on the process conditions, and in particular, petroleum-based residual oils contain a large amount of indene, indene derivatives, styrene, or styrene derivatives that may deteriorate product quality. The indene, indene derivatives, styrene, and styrene derivatives are representative reactive materials and may be converted into insoluble components by excessive polymerization reactions occurring under high temperature conditions or oxidation reaction conditions. Indene, indene derivatives, styrene, and styrene derivatives converted into insoluble components may be transformed into solid materials in the reactor to interfere with the continuous manufacturing process, and may cause deterioration of product quality.

More specifically, indene, indene derivatives, styrene, and styrene derivatives are contained in a high proportion in Pyrolysis Fuel Oil, which is one type of petroleum-based residual oil. According to the data (Appl. Chem. Eng., Vol 22, No, 5, 495) analyzed the pyrolysis residue by GC-Mass, the pyrolysis residue contains 15% of indene, inden derivative, styrene, and styrene derivative. Included above. In addition, the results of the inventors' analysis of the pyrolysis residue by GC-Mass are shown in Table 1 below.

ingredient content(%) Benzene 0.17 Toluene 0.04 p-Xylene 0.09 o-Xylene 0.08 Styrene 0.93 Styrene derivatives (methyl-) 1.27 Indane 0.17 1H-Indene 2.36 1H-Indene derivatives (methyl-) 3.28 1H-Indene derivatives (dimethyl-) 1.46 1H-Indene derivatives (trimethyl-) 0.17 Naphthalene 9.67 2-Methylnaphthalene 3.04 1-Methylnaphthalene 2.43 Naphthalene derivatives (dimethyl-) 2.56 Naphthalene derivatives (trimethyl-) 0.09 Naphthalene derivatives (ethenyl-) 0.16 Naphthalene derivatives (propenyl-) 0.77 Acenaphthene 0.52 1,1'-Biphenyl 1.55 2-Methyl-1,1'-biphenyl 0.35 4-Methyl-1,1'-biphenyl 0.21 1,1'-Biphenyl derivatives (dimethyl-) 0.25 9H-Fluorene 0.94 Dihydrofluorene 0.35 9H-Fluorene derivatives (methyl-) 1.01 Penanthrene 1.44 Anthracene 0.15 Phenanthrene derivatives (methyl-) 0.90 Fluoranthene 0.17 Pyrene 0.23 Others 63.19

As can be seen in Table 1, the thermal decomposition residue contains 9% or more of indene, indene derivatives, styrene, and styrene derivatives.

As such, the content of indene, indene derivatives, styrene, and styrene derivatives contained in the pyrolysis residual oil varies depending on the production method, region, and time, but overall, the pyrolysis residual oil includes indene, indene derivatives, styrene, And styrene derivatives are contained in a high proportion. A high proportion of indene, indene derivatives, styrene, and styrene derivatives can interfere with the continuous manufacturing process and cause deterioration of product quality. Petroleum residues used as raw materials for carbon materials The selection and processing of the material is important.

The present invention is a petroleum-based residual oil raw material containing indene and indene derivatives of 3% by weight or less, styrene and styrene derivatives of 0.3% by weight or less, and a softening point of 20°C to 150°C. To manufacture.

In the present invention, indene derivatives mean that one or more hydrogen atoms or double bonds bonded to indene are substituted with other functional groups, and the functional group is not particularly limited, but as an example, the functional group is a methyl group, an ethyl group, a propyl group. , Or cycloalkyl. In addition, styrene derivatives in the present invention mean that at least one hydrogen atom bonded to styrene is substituted with another functional group, and the functional group is not particularly limited, but as an example the functional group is a methyl group, an ethyl group, a propyl group, Or cycloalkyl.

The petroleum-based residual oil raw materials are PFO (Pyrolysis Fuel Oil), Naphtha Cracking Bottom Oil (NCB), Ethylene Bottom Oil (EBO), and FCC-DO (Fluid Catalytic Cracking Decant). Oil), RFCC-DO (Residue Fluid Catalytic Cracking Decant Oil), Aromatic Extract (AE), and hydrogenated petroleum-based residual oil may be at least one selected from the group.

In the present invention, the petroleum-based residual oil raw material may be pretreated by atmospheric distillation, reduced pressure distillation, polymerization, or hydrogenation to prepare a petroleum-based residual oil having a softening point of 20°C to 150°C.

Here, the petroleum-based residual oil having a softening point of less than 20° C. may decrease the carbonization yield due to a large amount of hard content, thereby reducing the efficiency of the process. In addition, the content of indene, indene derivatives, styrene, and styrene derivatives may increase, resulting in a problem that the content of quinoline insolubles in the final product, pitch, increases. Petroleum-based residual oils having a softening point of more than 150° C. may cause carbonization reactions during the manufacturing process, and problems may occur during transport due to an increase in viscosity.

Next, the manufacturing method of the present invention includes (b) an oxidation heat treatment step (S2) of heating while mixing an oxidizing gas into the petroleum-based residual oil.

In general, a catalyst is used under high pressure conditions to increase the softening point of the final product, the pitch. In addition, a peroxide-based compound is additionally used in the oxidizing gas to reduce the content of quinoline insolubles in the final product, pitch. However, when the catalyst is used under high pressure conditions to increase the softening point, an expensive high-pressure container is required as well as a separate process for removing the catalyst, which is not economical in producing a high softening point pitch. In addition, when a peroxide-based compound is additionally used in an oxidizing gas to reduce the content of quinoline insolubles in the final product, the peroxide-based compound has a high reactivity, so there is a risk of explosion during the manufacturing process, management of dangerous substances, wastewater treatment, Or, environmental pollution problems may arise. In addition, since the peroxide-based compound is expensive, it is economically difficult to produce a large-scale pitch.

In the present invention, the content of indene, indene derivative, styrene and styrene derivative is controlled by step (a), and oxidation heat treatment is performed by heating while mixing oxidizing gas in petroleum-based residual oil having a softening point of 20°C to 150°C. do.

The present invention has the effect of increasing the molecular weight of the petroleum-based residual oil by the oxidation heat treatment step to improve the yield of the final product, a high softening point pitch. In particular, the present invention does not require a high pressure condition in the oxidation heat treatment process, and does not use a catalyst, so that a high-quality petroleum-based high softening point pitch can be economically produced. In addition, since the present invention does not use peroxide compounds in the oxidation heat treatment process, there is no risk of explosion during the manufacturing process, and environmental pollution problems do not occur.

More specifically, in step (b), while mixing oxidizing gas at a flow rate of 0.1 L/min to 2.0 L/min relative to 1 kg of the petroleum-based residual oil raw material of step (a), 1 hour to 15 hours at 250° C. to 400° C. During the heat treatment can be performed.

The oxidizing gas may include a first gas containing at least one of air, oxygen, and ozone, or a second gas obtained by diluting the first gas with an inert gas containing at least one of nitrogen and argon. . For example, as the oxidizing gas, air in the atmosphere may be used directly, or may be used after diluting the air in the atmosphere with an inert gas. In addition, the oxidizing gas may be used by diluting oxygen with nitrogen to adjust the concentration of oxygen.

When oxidizing gas is mixed at a flow rate of less than 0.1 L/min compared to 1 kg of the petroleum-based residual oil raw material, the reaction rate is slow, the yield of the generated high softening point pitch is low, and the physical properties of the high softening point pitch cannot be satisfied. Can occur. When oxidizing gas is mixed at a flow rate of 2.0 L/min or more compared to 1 kg of petroleum-based residual oil raw material, the amount of oxidizing gas injected is excessive, and the content of toluene insoluble matter, a heavy component, increases rapidly, and quinoline insoluble matter (QI ) May also cause a problem of increasing the content.

In addition, when the oxidation heat treatment reaction temperature is less than 250° C., the molecular weight of the petroleum-based residual oil is not sufficiently increased, so that the yield of the final product, the high softening point pitch, may decrease. When the oxidation heat treatment reaction temperature is higher than 400° C., the content of toluene insoluble matter and the content of quinoline insoluble matter (QI) are rapidly increased, and a coking phenomenon may occur.

In addition, if the oxidation heat treatment reaction time is less than 1 hour, the oxidation heat treatment reaction time is too short to cause sufficient reaction, and if the oxidation heat treatment reaction time exceeds 15 hours, excessive polymerization reaction is caused, resulting in the final product of high softening point pitch. Physical properties may change.

Next, the manufacturing method of the present invention includes a reduced pressure heat treatment step (S3) of heating the resultant of step (c) (b) under reduced pressure.

The petroleum-based residual oil subjected to oxidation heat treatment in step (b) is heat treated under reduced pressure conditions. In the present invention, by removing the middle oil remaining in the petroleum-based residual oil subjected to oxidation heat treatment in step (c), the softening point is increased and the content of beta resin is increased to improve the carbonization yield. In particular, when the reaction is carried out under pressurized conditions in step (c), it is difficult to remove heavy oil and raise the softening point. In step (c), a reduced pressure condition is required.

More specifically, the depressurization condition in step (c) may be 300 torr or less, and preferably 200 torr or less. More preferably, it may be 100 torr or less.

In addition, the heat treatment temperature in step (c) may be 300°C to 400°C. When the heat treatment temperature is less than 300° C., it is difficult to remove heavy oils, and the production of beta resin is reduced, so that it is difficult to manufacture a high softening point pitch. When the heat treatment temperature is higher than 400° C., coking may occur due to the petroleum-based residual oil, and coke may be formed, and the content of toluene insoluble matter and the content of quinoline insoluble matter (QI) may be rapidly increased.

In addition, the reaction time under reduced pressure heat treatment in step (c) may be 1 hour to 15 hours. Preferably it may be 2 hours to 8 hours, more preferably 2 hours to 4 hours. If the vacuum heat treatment reaction time is less than 1 hour, the pressure reduction heat treatment reaction time is too short to produce a high softening point pitch, and if the pressure reduction heat treatment reaction time exceeds 15 hours, excessive polymerization reaction is caused, which is not economical.

Additionally, in order to more easily remove heavy oil in step (c), an inert gas such as nitrogen or argon relative to 1 kg of petroleum-based residual oil may be mixed at a flow rate of 0.1 L/min to 2.0 L/min.

The pitch prepared by the steps (a) to (c) of the present invention may have a softening point of 220° C. to 300° C., and a quinoline insoluble content (QI) content of 0.5% by weight or less. The quinoline insoluble (QI) means solid particles that are insoluble components in the quinoline solvent. The pitch produced by the production method of the present invention exhibits a high softening point of 220° C. to 300° C., and at the same time, the content of quinoline insoluble matters in the high softening point pitch can be significantly reduced.

In addition, the pitch prepared by steps (a) to (c) of the present invention may have a beta resin content of 10% by weight or more. The beta resin refers to a substance remaining from the amount of toluene insolubles excluding the amount of quinoline insolubles. The production method of the present invention produces a large amount of beta resin, so that the pitch produced by the production method of the present invention may contain 10% by weight or more of beta resin.

In addition, the pitch prepared by steps (a) to (c) of the present invention has an ash content of 0.1 wt% or less, an oxygen content of 0.3 wt% or less, a nitrogen content of 0.1 wt% or less, and a sulfur content of 0.1 wt% It can be below.

In general, pitches used as carbon materials should contain a small amount of heterogeneous elements such as oxygen, nitrogen, or sulfur. This is because when the content of heterogeneous elements in the pitch is high, a problem occurs in that the physical properties of the carbon material manufactured using the pitch as a raw material are deteriorated. The pitch produced by the production method of the present invention has the effect of significantly reducing the content of heterogeneous elements such as oxygen, nitrogen, and sulfur, and maintaining the inherent physical properties of the carbon material.

Hereinafter, specific embodiments of the present invention are presented. However, the examples described below are for illustrative purposes only, and the present invention should not be limited thereto.

Example

Example One

Pyrolysis fuel oil (PFO) having an indene, inden derivative, styrene and styrene derivative content of 9.47% by weight was used as a raw material, and a petroleum-based residual oil was prepared by vacuum distillation at 200°C under a pressure of 150 torr. The petroleum-based residue prepared at this time had a softening point of 38° C., the content of indene and indene derivatives was 1.8% by weight, and the content of styrene and styrene derivatives was 0.12% by weight.

800 g of the petroleum-based residual oil was put into the reactor, air was introduced into the reactor at a flow rate of 0.7 L/min, and oxidation heat treatment was performed at 360° C. for 4 hours. Thereafter, the pressure was reduced to a pressure of 100 torr, and a pitch was prepared by heat treatment under reduced pressure at 380° C. for 5 hours.

Example 2

Using the same pyrolysis fuel oil (PFO) as in Example 1 as a raw material, a petroleum-based residual oil was prepared through atmospheric distillation at 320°C at atmospheric pressure. At this time, the prepared petroleum-based residual oil had a softening point of 43° C., the content of indene and indene derivatives was 1.4% by weight, and the content of styrene and styrene derivatives was 0.08% by weight.

800 g of the petroleum-based residual oil was put into the reactor, air was introduced into the reactor at a flow rate of 0.5 L/min, and oxidation heat treatment was performed at 370° C. for 4 hours. Thereafter, the pressure was reduced to a pressure of 100 torr, and a pitch was prepared by heat treatment under reduced pressure at 380° C. for 5 hours.

Example 3

800 g of the same petroleum-based residual oil as in Example 1 was put into the reactor, a mixed gas of 30 vol% of oxygen and 70 vol% of nitrogen was added to the reactor at a flow rate of 0.3 L/min, followed by oxidation heat treatment at 350° C. for 4 hours. Thereafter, the pressure was reduced to 50 torr, and the pitch was prepared by heat treatment under reduced pressure at 380° C. for 5 hours.

Comparative example One

800 g of pyrolysis fuel oil (PFO) used in Example 1 was put into the reactor, air was introduced into the reactor at a flow rate of 0.7 L/min, and oxidative heat treatment was performed at 360° C. for 4 hours. Thereafter, the pressure was reduced to a pressure of 100 torr, and a pitch was prepared by heat treatment under reduced pressure at 380° C. for 5 hours.

Comparative example 2

800 g of the same petroleum residual oil as in Example 2 was put into the reactor, air was introduced into the reactor at a flow rate of 1.0 L/min, and oxidative heat treatment was performed at 360° C. for 5 hours. After that, the pitch was prepared without a vacuum heat treatment process.

Comparative example 3

800 g of pyrolysis fuel oil (PFO) used in Example 1 was put into the reactor, air was introduced into the reactor at a flow rate of 1.2 L/min, and oxidative heat treatment was performed at 370° C. for 5 hours. After that, the pitch was prepared without a vacuum heat treatment process.

Comparative example 4

800 g of coal tar pitch with a softening point of 35° C. and a quinoline insoluble content of 0.02 wt% was put into the reactor, air was introduced into the reactor at a flow rate of 0.5 L/min, and oxidative heat treatment was performed at 350° C. for 4 hours. Thereafter, the pressure was reduced to 150 torr, and a pitch was prepared by heat treatment under reduced pressure at 360° C. for 4 hours.

Experimental example

Measurement of pitch properties

The physical properties of the pitches prepared in Examples 1 to 3 and Comparative Examples 1 to 4 are shown in Table 2 below.

Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Softening point (℃) 245 265 282 242 196 211.2 282 Quinoline insoluble content (% by weight) 0.11 0.08 0.21 1.82 0.17 3.53 18.5 Beta resin (wt%) 19.5 28.4 36.9 21.3 2.7 4.59 46.2 Ash (% by weight) 0.02 0.03 0.03 0.02 0.02 0.02 0.01 Oxygen (% by weight) 0.13 0.11 0.14 0.15 0.58 0.72 0.87 Nitrogen (% by weight) 0.02 0.02 0.01 0.02 0.01 0.01 1.28 Sulfur (% by weight) 0.03 0.01 0.01 0.06 0.04 0.03 0.36

As shown in Table 2, the pitch of Examples 1 to 3 exhibits a high softening point of 220° C. or higher, the content of quinoline insoluble content is 0.5% by weight or less, the content of beta resin is 10% by weight or more, and the content of ash is 0.1 The content of oxygen, which is a hetero atom, is 0.3% by weight or less, and the content of sulfur and nitrogen is 0.1% by weight or less.

On the other hand, the pitch of Comparative Example 1 was prepared using a raw material having a high content of indene, indene derivatives, styrene and styrene derivatives, and thus it is not suitable for use in carbon products due to high quinoline insoluble content.

In addition, the pitch of Comparative Example 2 is produced without a reduced pressure heat treatment process, even if a raw material with a controlled content of indene, inden derivative, styrene and styrene derivative is used, so that the softening point and the content of beta resin are low, and the content of oxygen is high. Not suitable for use in the product.

In addition, the pitch of Comparative Example 3 uses a raw material having a high content of indene, inden derivatives, styrene and styrene derivatives, and as it is prepared without a vacuum heat treatment process, the quinoline insoluble content is high, the softening point and the content of beta resin are low, Due to its high oxygen content, it is not suitable for use in carbon products.

In addition, since the pitch of Comparative Example 4 was manufactured using coal tar pitch as a raw material instead of a petroleum-based residual oil raw material, the quinoline insoluble content was high and the content of heterogeneous elements such as oxygen, nitrogen and sulfur was high, so the required physical properties of the petroleum-based high softening point pitch A high softening point pitch different from that is produced.

Secondary battery Charge and discharge Capacity and initial efficiency measurements

Each of the pitch 3g prepared according to Example 1 and Comparative Example 3 was mixed with 97 g of natural graphite having an average diameter of 30 μm. Then, the pitch was coated on the surface of natural graphite using a mechanical stirrer. After the coating was completed, heat treatment was performed at 1,100° C. for 1 hour to prepare negative active materials, respectively.

Each of the negative electrode active materials was mixed with water in a weight ratio of negative active material: carbon black: carboxylmethylcellulose: styrene butadiene = 91:5:2:2 to prepare a negative electrode slurry composition. The composition for negative electrode slurry was coated on a copper current collector, dried and rolled in an oven at 110° C. for about 1 hour to prepare a negative electrode for a secondary battery.

Thereafter, the negative electrode for the secondary battery, a separator, and an electrolyte (the electrolyte was a solvent mixed in a weight ratio of 1:1 of ethylene carbonate: dimethyl carbonate, and 1.0M LiPF6 was added), followed by a lithium electrode in the form of a coin cell. A secondary battery was prepared.

Charge/discharge capacity and initial efficiency were measured for the prepared secondary battery according to the following conditions.

It is assumed that 300mA per 1g of the secondary battery is 1C, and the charging condition was controlled at 0.2C with a constant current from 0.01V to 0.01V and a constant voltage from 0.01V to 0.01C. Discharge conditions were measured with a constant current up to 1.5V at 0.2C. The initial efficiency was expressed as the retention rate of the discharge capacity after 10 cycles compared to the initial discharge capacity.

The measured charge/discharge capacity and initial efficiency of the secondary battery are shown in Table 3 below.

Charge/discharge capacity (mAh/g) Initial efficiency (%) Example 1 357 91 Comparative Example 3 348 87

As shown in Table 3, when the pitch prepared according to Comparative Example 3 was used as a coating agent for natural graphite, the charge/discharge capacity was smaller than when the pitch prepared according to Example 1 was used as a coating agent for natural graphite, and the initial efficiency Also shows a deteriorating result. This is due to the relatively low softening point, high quinoline insoluble content, low beta resin content, and high oxygen content of the pitch prepared according to Comparative Example 3 compared to the pitch prepared according to Example 1.

As described above, one embodiment of the present invention has been described, but those of ordinary skill in the relevant technical field add, change, delete or add components within the scope not departing from the spirit of the present invention described in the claims. Various modifications and changes can be made to the present invention by means of the like, and it will be said that this is also included within the scope of the present invention.

Claims (9)

(a) Petroleum-based residual oil A petroleum-based residue with a pretreatment of raw materials, the content of indene and indene derivatives is 3% by weight or less, the content of styrene and styrene derivatives is 0.3% by weight or less, and a softening point of 20 ℃ to 150 ℃ Preparing a reason;
(b) an oxidation heat treatment step of heating the petroleum-based residual oil while mixing an oxidizing gas;
(c) a reduced pressure heat treatment step of heating the resultant of step (b) in a reduced pressure state; including
Method for producing petroleum-based high softening point pitch.
The method of claim 1,
The petroleum-based residual oil raw material in step (a) is PFO (Pyrolysis Fuel Oil), Naphtha Cracking Bottom Oil (NCB), Ethylene Bottom Oil (EBO), FCC-DO. (Fluid Catalytic Cracking Decant Oil), RFCC-DO (Residue Fluid Catalytic Cracking Decant Oil), Aromatic Extract (AE) and hydrogenated petroleum-based residual oil, characterized in that at least one selected from
Method for producing petroleum-based high softening point pitch.
The method of claim 1,
The oxidation heat treatment of step (b) is performed at 250° C. to 400° C. for 1 hour while mixing the oxidizing gas at a flow rate of 0.1 L/min to 2.0 L/min relative to 1 kg of the petroleum-based residual oil raw material of step (a). Characterized in that heat treatment for 15 hours
Method for producing petroleum-based high softening point pitch.
The method of claim 3,
The oxidizing gas in step (b) is a first gas containing at least one of air, oxygen, and ozone, or a second gas obtained by diluting the first gas with an inert gas containing at least one of nitrogen and argon. Characterized in that it contains a gas
Method for producing petroleum-based high softening point pitch.
The method of claim 1,
The reduced pressure heat treatment in step (c) is characterized in that the heat treatment is performed at 300 to 400 °C for 1 to 15 hours under a pressure of 300 torr or less.
Method for producing petroleum-based high softening point pitch.
The pitch prepared according to claim 1 has a softening point of 220°C to 300°C, and a quinoline insoluble content (QI) content of 0.5% by weight or less.
Method for producing petroleum-based high softening point pitch.
The pitch prepared according to claim 1 is characterized in that the beta resin content is 10% by weight or more.
Method for producing petroleum-based high softening point pitch.
The pitch prepared according to claim 1, characterized in that the ash content is 0.1% by weight or less.
Method for producing petroleum-based high softening point pitch.
The pitch prepared according to claim 1 is characterized in that the oxygen content is 0.3% by weight or less, the nitrogen content is 0.1% by weight or less, and the sulfur content is 0.1% by weight or less.
Method for producing petroleum-based high softening point pitch.

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