CN114806622A - Process for preparing impregnated asphalt - Google Patents
Process for preparing impregnated asphalt Download PDFInfo
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- CN114806622A CN114806622A CN202111598861.0A CN202111598861A CN114806622A CN 114806622 A CN114806622 A CN 114806622A CN 202111598861 A CN202111598861 A CN 202111598861A CN 114806622 A CN114806622 A CN 114806622A
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- Prior art keywords
- impregnated
- coal tar
- solvent
- pitch
- supernatant
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- 239000010426 asphalt Substances 0.000 title claims abstract description 66
- 238000004519 manufacturing process Methods 0.000 title description 8
- 238000000034 method Methods 0.000 claims abstract description 80
- 239000002904 solvent Substances 0.000 claims abstract description 61
- 239000006228 supernatant Substances 0.000 claims abstract description 38
- 238000002156 mixing Methods 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 23
- 238000004821 distillation Methods 0.000 claims abstract description 21
- 239000000126 substance Substances 0.000 claims abstract description 20
- 239000007787 solid Substances 0.000 claims abstract description 15
- 238000010908 decantation Methods 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 238000005119 centrifugation Methods 0.000 claims abstract description 4
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 claims description 98
- 239000011280 coal tar Substances 0.000 claims description 57
- 239000011295 pitch Substances 0.000 claims description 44
- 125000003118 aryl group Chemical group 0.000 claims description 39
- 239000011294 coal tar pitch Substances 0.000 claims description 26
- AWJUIBRHMBBTKR-UHFFFAOYSA-N isoquinoline Chemical compound C1=NC=CC2=CC=CC=C21 AWJUIBRHMBBTKR-UHFFFAOYSA-N 0.000 claims description 14
- 239000011269 tar Substances 0.000 claims description 14
- 238000009835 boiling Methods 0.000 claims description 13
- 239000011347 resin Substances 0.000 claims description 13
- 229920005989 resin Polymers 0.000 claims description 13
- 239000006229 carbon black Substances 0.000 claims description 9
- 150000001491 aromatic compounds Chemical class 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000005292 vacuum distillation Methods 0.000 claims description 4
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000003245 coal Substances 0.000 abstract description 9
- 238000000926 separation method Methods 0.000 description 17
- GTPSFNHCIVIGMV-UHFFFAOYSA-N isoquinoline Chemical compound C1=NC=CC2=CC=CC=C21.C1=NC=CC2=CC=CC=C21 GTPSFNHCIVIGMV-UHFFFAOYSA-N 0.000 description 16
- 238000011084 recovery Methods 0.000 description 12
- 239000003208 petroleum Substances 0.000 description 11
- 239000003350 kerosene Substances 0.000 description 7
- 239000011259 mixed solution Substances 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000003575 carbonaceous material Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- RQQDJYROSYLPPK-UHFFFAOYSA-N N1=CC=CC2=CC=CC=C21.N1=CC=CC2=CC=CC=C21 Chemical compound N1=CC=CC2=CC=CC=C21.N1=CC=CC2=CC=CC=C21 RQQDJYROSYLPPK-UHFFFAOYSA-N 0.000 description 3
- 125000001931 aliphatic group Chemical group 0.000 description 3
- 239000000571 coke Substances 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000006068 polycondensation reaction Methods 0.000 description 3
- 239000003849 aromatic solvent Substances 0.000 description 2
- 239000011305 binder pitch Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 238000004939 coking Methods 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 238000005087 graphitization Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000002198 insoluble material Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- 239000011271 tar pitch Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- WHRZCXAVMTUTDD-UHFFFAOYSA-N 1h-furo[2,3-d]pyrimidin-2-one Chemical compound N1C(=O)N=C2OC=CC2=C1 WHRZCXAVMTUTDD-UHFFFAOYSA-N 0.000 description 1
- 235000006173 Larrea tridentata Nutrition 0.000 description 1
- 244000073231 Larrea tridentata Species 0.000 description 1
- 229960002126 creosote Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Images
Classifications
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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
- C10C3/08—Working-up pitch, asphalt, bitumen by selective extraction
-
- 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
- C10C3/002—Working-up pitch, asphalt, bitumen by thermal means
-
- 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
- C10C3/005—Working-up pitch, asphalt, bitumen by mixing several fractions (also coaltar fractions with petroleum fractions)
-
- 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
- C10C3/007—Working-up pitch, asphalt, bitumen winning and separation of asphalt from mixtures with aggregates, fillers and other products, e.g. winning from natural asphalt and regeneration of waste asphalt
-
- 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
- C10C3/06—Working-up pitch, asphalt, bitumen by distillation
Abstract
The invention relates to a preparation method of impregnated asphalt, which comprises the following steps: mixing a coal tar-like raw material substance and a solvent to prepare a mixture; separating the supernatant and the underflow including the solid components from the mixture by centrifugation or decantation (decanting); recovering the solvent from the supernatant to obtain a residue; and performing a distillation process and a heat treatment process on the residue.
Description
Technical Field
The present invention relates to a method for preparing impregnated asphalt, and more particularly, to a method for preparing high-quality impregnated asphalt, comprising: the content of Quinoline Insolubles (QI) is significantly reduced and the content of β -resin in the impregnated pitch is more than 10 wt% of the total weight of the impregnated pitch and the softening point of the impregnated pitch is 60 ℃ to 120 ℃.
Background
Conventionally, carbon fired products are produced as products of graphite electrodes, graphite blocks, etc. for steel making by using binder pitch as a binding material in coke and undergoing firing, graphitization, and processing processes. However, in the heat treatment process, pores are generated in the carbon material along with the escape or thermal decomposition of volatile components of the coke and the binder pitch, thereby reducing the mechanical strength, the bulk density, and the like of the carbon material and improving the electrical resistance.
The impregnation process, which is a process of introducing pitch into the above-mentioned pores and firing to increase the bulk density of the carbon material, can solve the above-mentioned problems. At this time, the pore permeability of the impregnated pitch used should be good, and the amount of fixed carbon remaining after the firing and graphitization processes should be high. Therefore, the raw material of pitch which can be used is limited, and coal tar pitch is generally used. However, since coal tar pitch contains Quinoline Insolubles (QI) and hinders the pitch from permeating into the pores, a process of removing a part of the quinoline insolubles is required. Although there is a method for producing an impregnated pitch by removing quinoline insolubles, commercially, an impregnated pitch containing an extremely small amount of quinoline insolubles is required for producing a high-quality carbon material. In order to produce such an impregnated pitch containing a very small amount of quinoline insolubles, there are limitations on raw materials, and there are problems that need to be solved by using a solvent, a separation method, and the like.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing high-quality impregnated pitch with significantly reduced Quinoline Insoluble (QI) content from a plurality of coal tar-based raw material substances including at least one of coal tar, coal tar-based carbon black oil, heavy tar, and coal tar pitch having a softening point of 10 ℃ to 90 ℃.
According to the concept of the invention, the process for the preparation of the impregnated bitumen comprises the following steps: mixing a coal tar-like raw material substance with a solvent to prepare a mixture; separating the supernatant and the underflow including the solid components from the mixture by centrifugation or decantation (decanting); recovering the solvent from the supernatant to obtain a residue; and performing a distillation process and a heat treatment process on the residue, wherein the coal tar type raw material substance comprises at least one of coal tar, heavy tar, coal tar type carbon black raw oil and coal tar pitch with a softening point of 10-90 ℃, the solvent comprises 1 to 4 substituted or unsubstituted aromatic rings, the aromatic index of the solvent is 0.7 to 1, the solvent has a boiling point of from 100 ℃ to 350 ℃, based on the total weight of the impregnated pitch, the content of quinoline and isoquinoline (isoquinoline) in the solvent may be 0 to 5.0 wt%, the softening point of the impregnating pitch may be 60 ℃ to 120 ℃, relative to the total weight of the impregnating pitch, the content of quinoline insoluble in the impregnated pitch may be from 0.0001 wt% to 0.5 wt%, relative to the total weight of the impregnated pitch, the content of beta-resin in the impregnating pitch may be 10 wt% to 30 wt%.
According to the method for producing impregnated pitch of the present invention, not only coal tar pitch, which is generally used in a large amount, but also various coal tar-based raw materials including heavy tar containing a large amount of solid components, which is a waste remaining after refining coal tar, can be used as raw material substances, and therefore, the method is economical.
The softening point of the impregnated asphalt prepared by the method for preparing impregnated asphalt of the present invention may be 60 to 120 ℃, the content of quinoline insoluble in the impregnated asphalt may be 0.5 wt% or less, and the content of β -resin in the impregnated asphalt may be 10 wt% or more. Thus, according to the present invention, high-quality impregnated asphalt can be produced.
Compared with the existing preparation method, the preparation method of the impregnated asphalt has simple preparation process, can be used for continuous preparation, has high recovery amount of beta-resin, and can prepare the impregnated asphalt with high carbonization yield.
Drawings
Fig. 1 is a flow chart for explaining a method of preparing impregnated asphalt according to an embodiment of the present invention.
Fig. 2 is a schematic process diagram for explaining a method of preparing impregnated asphalt according to an embodiment of the present invention.
Detailed Description
In order to fully understand the structure and effects of the present invention, preferred embodiments of the present invention will be described with reference to the accompanying drawings. However, the present invention is not limited to the embodiments disclosed below, and may be implemented in various forms and may be variously modified. The present embodiments are provided only for the purpose of making a complete disclosure of the present invention through the description of the present embodiments, and for informing those skilled in the art of the scope of the present invention in full, having ordinary knowledge.
Fig. 1 is a flow chart for explaining a method of preparing impregnated asphalt according to an embodiment of the present invention.
Fig. 2 is a schematic process diagram for explaining a method of preparing impregnated asphalt according to an embodiment of the present invention.
Referring to fig. 1 and 2, a method for preparing impregnated asphalt according to an embodiment of the present invention may include the steps of: a step (S1) of mixing a coal tar-based raw material substance and a solvent to prepare a mixture; a step of separating a supernatant and a underflow including solid components from the mixture by a centrifugal separation method or a decantation (settling) (S2); a step (S3) of recovering the solvent from the supernatant to obtain a residue; and a step of performing a distillation process and a heat treatment process on the residue (S4).
The method for preparing the impregnated asphalt according to an embodiment of the present invention may include the step of mixing coal tar-based raw material substances and a solvent to prepare a mixture (S1). The step of mixing the coal tar-based raw material and the solvent to prepare a mixture (S1) may be performed in a mixer. The coal tar type raw material substance may include at least one of coal tar, coal tar type carbon black oil, heavy tar, and coal tar pitch having a softening point of 10 ℃ to 90 ℃. The coal tar may be a substance obtained when coal is subjected to high-temperature dry distillation. In the present specification, the heavy tar is a byproduct remaining after coal tar is refined for commercial use of coal tar, and may be a coal tar sludge containing various byproducts in the form of sludge and moisture.
That is, according to the present invention, a variety of coal tar-type feedstock materials can be used to produce the impregnated asphalt. Typically, heavy tar is considered a waste, but according to the present invention, it can be used as a feedstock for high quality impregnated bitumen.
The solvent may include a single aromatic compound or a mixed aromatic compound. Quinoline Insolubles (QIs) can be removed from the coal tar-like feedstock material by means of the solvent. As an example, the solvent may include 1 to 4 aromatic rings which may be substituted or unsubstituted, and the aromatic index of the solvent may be 0.7 to 1. In the present specification, the aromatic index may refer to a value calculated using a Brown-Ladner method.
On the other hand, for example, when petroleum kerosene containing a large amount of aliphatic components is used as a raw material, if a solvent having an aromatic index of less than 0.7 is used, the recovery efficiency of tar components may be lowered. Further, in order to use petroleum-based kerosene containing a large amount of aliphatic components as a raw material, relatively high-temperature mixing conditions of 150 ℃ or higher may be required. Therefore, in this case, in the subsequent step (S2) of separating the supernatant and the underflow including the solid components from the mixture by the centrifugal separation method or the decantation (decanting) method, only the layer separation may occur, and the recovery efficiency of the tar component may be lowered.
The solvent may include a single aromatic compound or a mixed aromatic compound. The boiling point of the solvent may be 100 ℃ to 350 ℃. On the other hand, if the boiling point of the solvent is less than 100 ℃, the process operation may be disadvantageous because odor and volatility are strong, and if the boiling point of the solvent exceeds 350 ℃, the viscosity may increase or a large amount of energy may be required for recovery, thereby reducing the economical efficiency.
The content of quinoline (quinoline) and isoquinoline (isoquinoline) in the solvent may be from 0.0001 wt% to 5.0 wt%, relative to the total weight of the impregnated pitch. However, even if the aromatic index of the solvent is 0.7 or more, if a solvent in which the content of quinoline (quinoline) and isoquinoline (isoquinoline) in the aromatic solvent is 5.0 wt% or more based on the total weight of the impregnated pitch is used, the tar component can be dissolved well to improve the recovery rate, and on the contrary, the efficiency of removing impurities including quinoline insoluble materials (QI) may be reduced. For example, the content of quinoline (quinoline) and isoquinoline (isoquinoline) in the coal tar-based wash oil having a boiling point of 240 ℃ to 310 ℃ may be about 10% based on the total weight of the impregnated pitch, and when this is used as a solvent, the tar component is well dissolved to increase the recovery rate, whereas the efficiency of removing impurities including quinoline insoluble material (QI) may be reduced.
In one embodiment of the present invention, the solvent may not contain quinoline or isoquinoline. That is, the content of quinoline and isoquinoline in the solvent may be 0 wt%. Further, as described above, the solvent of the present invention may contain a small amount of quinoline and isoquinoline, and therefore, the content of quinoline and isoquinoline in the solvent of the present invention may be 0 wt% to 5.0 wt%.
As an example, the weight ratio of the coal tar-based feedstock substance to the solvent may be from 90:10 to 20: 80. On the other hand, when the amount of the solvent is less than 10 parts by weight based on 100 parts by weight of the mixture, the recovery efficiency of the coal tar component may be lowered, and the content of Quinoline Insolubles (QI) in the coal tar pitch may exceed 0.5 wt%. Also, when the weight part of the solvent exceeds 80 parts by weight with respect to 100 parts by weight of the mixture, although the recovery efficiency of the coal tar component can be improved and the content of Quinoline Insoluble (QI) can be maintained at 0.5 wt% or less, the cost required for the process increases, which may reduce the economical efficiency.
The step of mixing the coal tar-based raw material with the solvent to prepare a mixture (S1) may further include a stirring process. The step of preparing the mixture may be performed at 20 ℃ to 150 ℃. Thus, the step of separating the supernatant and the underflow including the solid components from the mixture (S2) can be smoothly performed by the subsequent centrifugal separation method or decantation (decanting) method.
The preparation method of the impregnated asphalt according to an embodiment of the present invention may include the step of separating a supernatant and a underflow including solid components from the mixture by a centrifugal separation method or a decantation (decanting) method (S2). The underiayer liquid may contain a large amount of solid components. The solid content may be a solid content contained in coal tar, and examples thereof include ash, Quinoline Insoluble (QI: Quinoline Insoluble), coal, coke, cenospheres (Cenosphere), and the like. The mixture may be separated into the supernatant and the subnatant by centrifugation or decantation (decantation).
The content of the solid component in the supernatant may be 0.0001 wt% to 0.5 wt%, may be 0.0001 wt% to 0.3 wt%, or may be 0.0001 wt% to 0.1 wt% with respect to the total weight of the supernatant. Most of the solid components may be composed of Quinoline Insolubles (QI) which may remain in the coal tar pitch after separation of Light oil, wash oil, creosote oil, etc. from the coal tar-based raw material by a subsequent distillation process. That is, the content of Quinoline Insolubles (QI) in the supernatant may be 0.0001 to 0.5 wt%, may be 0.0001 to 0.3 wt%, or may be 0.0001 to 0.1 wt%, relative to the total weight of the supernatant.
As for the temperature at which the step of separating the supernatant and the subnatant from the mixture is performed, the higher the temperature is, the more advantageous in the temperature range in which the solvent is not evaporated. As an example, the step of separating the supernatant and the subnatant from the mixture may be performed at 20 ℃ to about 150 ℃.
The centrifugal force (G-force) of the centrifugal separation method or the decantation (decanting) method may be 1,000G to 10,000G. As the value of the centrifugal force (G-force) increases, the removal rate of solid components from the coal tar-based raw material and the recovery rate of coal tar increase.
According to the present invention, the impregnated asphalt can be prepared by the centrifugal separation method or the decantation (settling) method, so that the impregnated asphalt can be prepared by a continuous process.
The preparation method of the impregnated asphalt according to an embodiment of the present invention may include the step of recovering the solvent from the supernatant to obtain a residue (S3). The step of recovering the solvent from the supernatant may further comprise the step of subjecting the supernatant to a distillation process. As an example, the distillation process may include an atmospheric distillation process or a vacuum distillation process. The solvent may be distilled and recovered by the atmospheric distillation process or the vacuum distillation process. Thus, a residue from which Quinoline Insolubles (QI) were removed can be obtained from the supernatant. The recovered solvent may be recycled for reuse.
The preparation method of the impregnated asphalt according to an embodiment of the present invention may include the step of performing a distillation process and a heat treatment process on the residue (S4). As an example, the distillation process may be an atmospheric distillation process or a vacuum distillation process. As an example, the heat treatment temperature of the heat treatment process may be 230 ℃ to 400 ℃. The coal tar distillate in the impregnated pitch may be removed by performing the steps of a distillation process and a heat treatment process on the residue (S4). Specifically, by performing the steps of the distillation process and the heat treatment process on the residue (S4), the light fraction and/or the heavy fraction in the residue may be removed, and the content of the β -resin may be increased by the polycondensation reaction occurring by heat. In addition, the softening point of the impregnating pitch can be increased.
On the other hand, in the case where the heat treatment temperature of the heat treatment process is less than 230 ℃, the light fraction and the heavy fraction may not be sufficiently removed, and the polycondensation reaction may not sufficiently occur, so that it may be difficult to prepare high-quality impregnated asphalt. In the case where the heat treatment temperature of the heat treatment process exceeds 400 ℃, an excessive polycondensation reaction proceeds, so that a Coking (Coking) phenomenon may occur, or a quinoline-insoluble intermediate phase (mesophase) is generated, so that the impregnability of the impregnated asphalt may be hindered. Thus, it may be difficult to prepare high quality impregnated asphalt.
The step of performing the distillation process and the heat treatment process on the residue (S4) may further include an injection process of an inert gas or steam (steam). The inert gas may include nitrogen or argon, as an example. The light fraction and the heavy fraction can be sufficiently removed by the injection process of the inert gas or steam (steam).
The softening point of the impregnated asphalt produced by the method for producing impregnated asphalt according to an embodiment of the present invention may be 60 to 120 ℃. The content of quinoline insoluble in the impregnated pitch may be from 0.0001 wt% to 0.5 wt% relative to the total weight of the impregnated pitch. The content of beta-resin in the impregnating pitch may be 10 to 30 wt% relative to the total weight of the impregnating pitch. The content of ash in the impregnated asphalt may be 0.0001 wt% to 0.3 wt% relative to the total weight of the impregnated asphalt. The yield of the impregnated pitch may be 30% to 90%. 30 to 90 wt% of the impregnating pitch can be obtained with respect to the total weight of the coal tar-type feedstock substance.
Conventionally, in order to remove quinoline insoluble components, an impregnated pitch has been prepared by removing quinoline insoluble components by a static precipitation method or a filtration method in which coal tar pitch is dissolved in an aromatic solvent using an aliphatic solvent. However, the method for producing an impregnated asphalt of the present invention has a simple production process and can produce an impregnated asphalt with a high carbonization yield by allowing continuous production and a high recovery amount of a β -resin, as compared with conventional production methods.
Examples
Example 1
A mixing process of mixing the coal tar pitch and the coal tar type aromatic fraction is performed. The softening point of the coal tar pitch was 40 ℃ and the content of quinoline insoluble matter was 3.8% by weight relative to the total weight of the coal tar pitch. The aromatic index of the coal tar type aromatic fraction is 0.87, the content of quinoline and isoquinoline is less than 3 wt% based on the total weight of the coal tar type aromatic fraction, and the atmospheric boiling point is 240-270 ℃. The mixing process is carried out at 90 ℃. The coal tar pitch and the coal tar-based aromatic fraction were mixed at a weight ratio of 60:40, and stirred using a mechanical stirrer (mechanical stirrer).
After preparing a mixed solution by a mixing process, it was put into a centrifugal separator and separated into a supernatant and a subnatant at a separation temperature of 90 ℃ and a centrifugal force (G-force) of 3500G. Then, the residue obtained by recovering the solvent from the supernatant was subjected to a reduced-pressure heat treatment process at 200 torr and 340 ℃ for 5 hours. As a result, the obtained impregnated asphalt had a softening point of 84 ℃. It was also confirmed that the impregnated asphalt contained 0.15 wt% of quinoline insolubles, 18.5 wt% of β -resin, and 0.02 wt% of ash, based on the total weight of the impregnated asphalt. And 72% of impregnated pitch with respect to the weight of coal tar pitch as a raw material substance can be obtained.
Example 2
The mixing process of mixing the carbon black raw oil and the aromatic fractions of the coal tar is performed. The softening point of the carbon black feedstock oil was 30 ℃ or lower, and the content of quinoline insoluble matter was 2.8 wt% based on the total weight of the carbon black feedstock oil. The aromatic index of the coal tar type aromatic fraction is 0.82, the content of quinoline and isoquinoline is less than 0.2 wt% relative to the total weight of the coal tar type aromatic fraction, and the atmospheric boiling point is 260-300 ℃. The mixing process was performed at 70 ℃. The carbon black feedstock oil and the coal tar-based aromatic fraction were mixed at a weight ratio of 50:50, and stirred with a mechanical stirrer (mechanical stirrer).
After preparing a mixed solution by a mixing process, it was put into a centrifugal separator and separated into a supernatant and a subnatant at a separation temperature of 70 ℃ and a centrifugal force (G-force) of 3000G. Then, the residue obtained by recovering the solvent from the supernatant was subjected to heat treatment under reduced pressure at 150 torr and 350 ℃ for 6 hours. As a result, the obtained impregnated asphalt had a softening point of 92 ℃. It was also confirmed that the impregnated asphalt contained 0.22 wt% of quinoline insoluble, 19.3 wt% of β -resin, and 0.03 wt% of ash, based on the total weight of the impregnated asphalt. And the impregnated pitch was obtained at 64% by weight based on the weight of the carbon black feedstock oil as the feedstock.
Example 3
A mixing process of mixing the heavy tar and the solvent is performed. The heavy tar contained 9.72 wt% of solid components relative to the total weight of the heavy tar. The solvent may include: a first coal tar-like aromatic fraction having an aromatic index of 0.92, a quinoline and isoquinoline content of 0.1 wt% or less relative to the total weight of the first coal tar-like aromatic fraction, and an atmospheric boiling point of 290 ℃ to 330 ℃; and a second coal tar-based aromatic fraction having an aromatic index of 0.87, a quinoline and isoquinoline content of 3 wt% or less relative to the total weight of the second coal tar-based aromatic fraction, and an atmospheric boiling point of 240 to 270 ℃. The solvent may mix the first coal tar-based aromatic fraction and the second coal tar-based aromatic fraction in a weight ratio of 50: 50. The solvent and the heavy tar were mixed in a weight ratio of 45:55 and stirred using a mechanical stirrer (mechanical stirrer).
After preparing a mixed solution by a mixing process, it was put into a centrifuge and separated into a supernatant and a subnatant at a separation temperature of 85 ℃ and a centrifugal force (G-force) of 2800G. Then, the residue obtained by recovering the solvent from the supernatant was subjected to a heat treatment under reduced pressure at 180 torr and 320 ℃ for 5 hours. As a result, the obtained impregnated asphalt had a softening point of 80.1 ℃. Further, it was confirmed that the impregnated asphalt contained 0.09 wt% of quinoline insoluble matter, 16.5 wt% of β -resin, and 0.01 wt% of ash, based on the total weight of the impregnated asphalt. And 47% of impregnated pitch with respect to the weight of heavy tar as a raw material was obtained.
Example 4
A mixing process of mixing coal tar and petroleum-based aromatic fractions is performed. In the coal tar, the content of quinoline insoluble matter was 1.4% by weight based on the total weight of the coal tar. The petroleum aromatic fraction has an aromatic index of 0.78, a quinoline and isoquinoline content of 0.01% or less relative to the total weight of the petroleum aromatic fraction, and an atmospheric boiling point of 140 ℃ to 320 ℃. The mixing process was performed at 50 ℃. The coal tar and the petroleum aromatic fraction were mixed at a weight ratio of 65:35, and stirred with a mechanical stirrer (mechanical stirrer).
After preparing a mixed solution by a mixing process, it was put into a centrifuge and separated into a supernatant and a subnatant at a separation temperature of 50 ℃ and a centrifugal force (G-force) of 3300G. Then, the residue obtained by recovering the solvent from the supernatant was subjected to heat treatment under reduced pressure at 360 ℃ at 100 torr for 3 hours. As a result, the obtained impregnated asphalt had a softening point of 82.8 ℃. It was also confirmed that the impregnated asphalt contained 0.38 wt% quinoline insolubles, 15.2 wt% β -resin, and 0.02 wt% ash, based on the total weight of the impregnated asphalt. And 42% of impregnated pitch with respect to the weight of coal tar as a raw material substance was obtained.
Comparative example 1
A mixing process of mixing the coal tar pitch and the coal tar type aromatic fraction is performed. The softening point of the coal tar pitch is 40 ℃, and the content of quinoline insoluble substances is 3.8 wt% relative to the total weight of the coal tar pitch. The aromatic index of the coal tar type aromatic fraction is 0.89, the content of quinoline and isoquinoline is more than 14 wt% relative to the total weight of the coal tar type aromatic fraction, and the atmospheric boiling point is 235-270 ℃. The mixing process is performed at 90 ℃. The coal tar pitch and the coal tar-based aromatic fraction were mixed at a weight ratio of 60:40, and stirred using a mechanical stirrer (mechanical stirrer).
After preparing a mixed solution by a mixing process, it was put into a centrifugal separator and separated into a supernatant and a subnatant at a separation temperature of 90 ℃ and a centrifugal force (G-force) of 3500G. Then, the residue obtained by recovering the solvent from the supernatant was subjected to heat treatment under reduced pressure at 200 torr and 340 ℃ for 5 hours. As a result, the obtained impregnated asphalt had a softening point of 87 ℃. It was also confirmed that the impregnated asphalt contained 0.85 wt% of quinoline insoluble matter, 17.2 wt% of β -resin, and 0.04 wt% of ash, based on the total weight of the impregnated asphalt. And 74% of impregnated pitch with respect to the weight of coal tar pitch as a raw material substance can be obtained.
According to comparative example 1, it was confirmed that the content of quinoline insolubles in the impregnated asphalt prepared using a solvent containing high contents of quinoline and isoquinoline was higher than 0.5 wt% as a reference value.
Comparative example 2
A mixing process of mixing coal tar pitch and petroleum-based kerosene was performed. The softening point of the coal tar pitch is 40 ℃, and the content of quinoline insoluble substances is 3.8 wt% relative to the total weight of the coal tar pitch. The petroleum kerosene has an aromatic index of 0.03, a quinoline and isoquinoline content of 0.01 wt% or less relative to the total weight of the petroleum kerosene, and an atmospheric boiling point of 180 ℃ to 250 ℃. The mixing process is carried out at 90 ℃. The coal tar pitch and the petroleum kerosene were mixed at a weight ratio of 60:40, and stirred with a mechanical stirrer (mechanical stirrer).
After the mixed solution was prepared by the mixing process, the mixed solution was put into a centrifugal separator and subjected to centrifugal separation at a separation temperature of 90 ℃ and a centrifugal force (G-force) of 3500G, but only layer separation of the petroleum-based kerosene and the coal tar pitch occurred, and recovery of the coal tar pitch as a supernatant did not occur.
According to comparative example 2, in the case of using a solvent having a low aromatic index, the coal tar-based raw material substance and the solvent may not be mixed, and thus the recovery rate of the coal tar component may be low, and it may be confirmed that it may be difficult to prepare the impregnated pitch finally.
Claims (12)
1. A preparation method of impregnated asphalt comprises the following steps:
mixing coal tar type raw material substances and a solvent to prepare a mixture;
separating the supernatant and the underflow including the solid components from the mixture by centrifugation or decantation;
recovering the solvent from the supernatant to obtain a residue; and
performing a distillation process and a heat treatment process on the residue,
in the method for preparing the impregnated asphalt,
the coal tar type raw material substances comprise at least one of coal tar, heavy tar, coal tar type carbon black raw oil and coal tar pitch with a softening point of 10-90 ℃,
the solvent comprises 1 to 4 substituted or unsubstituted aromatic rings, the aromatic index of the solvent is 0.7 to 1,
the boiling point of the solvent is 100 to 350 ℃,
the content of quinoline and isoquinoline in the solvent is 0 to 5.0 wt% relative to the total weight of the impregnated pitch,
the softening point of the impregnating pitch is 60 ℃ to 120 ℃,
the content of quinoline insolubles in the impregnated pitch is from 0.0001 wt% to 0.5 wt% relative to the total weight of the impregnated pitch,
the content of beta-resin in the impregnating pitch is from 10 to 30 wt% relative to the total weight of the impregnating pitch.
2. The process for producing impregnated asphalt according to claim 1,
the solvent comprises a single aromatic compound or a mixed aromatic compound.
3. The process for producing impregnated asphalt according to claim 1,
the distillation process is a normal pressure distillation process or a reduced pressure distillation process,
the heat treatment temperature of the heat treatment process is 230 ℃ to 400 ℃.
4. The process for producing impregnated asphalt according to claim 1,
the steps of preparing the mixture and separating the supernatant and the subnatant from the mixture are performed in the range of 20 ℃ to 150 ℃.
5. The process for producing impregnated asphalt according to claim 1,
the weight ratio of the coal tar type raw material substances to the solvent is 90:10 to 20: 80.
6. The process for producing impregnated asphalt according to claim 1,
the content of quinoline insolubles in the supernatant is 0.0001 to 0.5 wt% relative to the total weight of the supernatant.
7. The process for producing impregnated asphalt according to claim 1,
the step of recovering the solvent from the supernatant includes the step of performing an atmospheric distillation process or a vacuum distillation process on the supernatant.
8. The process for producing impregnated asphalt according to claim 1,
removing the coal tar distillate in the impregnated pitch by performing the steps of a distillation process and a heat treatment process on the residue.
9. The process for producing impregnated asphalt according to claim 1,
the step of performing the distillation process and the heat treatment process on the residue further includes an injection process of an inert gas or steam.
10. The process for producing impregnated asphalt according to claim 9,
the inert gas comprises nitrogen or argon.
11. The process for producing impregnated asphalt according to claim 1,
the content of ash in the impregnated asphalt may be 0.0001 wt% to 0.3 wt% relative to the total weight of the impregnated asphalt.
12. The process for producing impregnated asphalt according to claim 1,
the yield of the impregnated pitch is 30% to 90%.
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| JP2004285130A (en) * | 2003-03-20 | 2004-10-14 | Jfe Chemical Corp | Method for manufacturing impregnating pitch |
| WO2009142807A2 (en) * | 2008-05-22 | 2009-11-26 | Graftech International Holdings Inc. | High coking value pitch |
| CN102399491A (en) * | 2011-09-14 | 2012-04-04 | 江苏斯泰达新能源科技发展有限公司 | Polyurethane prime coat specifically for concrete surface treatment |
| KR20140146003A (en) * | 2013-06-13 | 2014-12-24 | 오씨아이 주식회사 | Highly efficient method for manufacturing pitch as carbonaceous raw material |
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| US4317809A (en) * | 1979-10-22 | 1982-03-02 | Union Carbide Corporation | Carbon fiber production using high pressure treatment of a precursor material |
| JPS6045612A (en) * | 1983-08-17 | 1985-03-12 | Mitsubishi Chem Ind Ltd | Preparation of carbon yarn |
| JPS61238885A (en) * | 1985-04-16 | 1986-10-24 | Maruzen Sekiyu Kagaku Kk | Method of refining raw material used for production of carbon product |
| US5437780A (en) * | 1993-10-12 | 1995-08-01 | Conoco Inc. | Process for making solvated mesophase pitch |
| JPH08134468A (en) * | 1994-11-07 | 1996-05-28 | Showa Shell Sekiyu Kk | Production of isotropic pitch for carbon fiber |
| KR101423511B1 (en) * | 2012-12-27 | 2014-07-30 | 주식회사 포스코 | Method for purifying impurities from Tar or Pitch and apparatus thereof |
| WO2015076533A1 (en) * | 2013-11-19 | 2015-05-28 | 에스케이이노베이션 주식회사 | Method for preparing isotropic pitch for manufacturing carbon fiber |
| KR101961808B1 (en) * | 2016-10-13 | 2019-03-25 | 인하대학교 산학협력단 | Manufacturing method of high purity pitch from fluidized catalytic cracking decant oil |
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|---|---|---|---|---|
| JP2004285130A (en) * | 2003-03-20 | 2004-10-14 | Jfe Chemical Corp | Method for manufacturing impregnating pitch |
| WO2009142807A2 (en) * | 2008-05-22 | 2009-11-26 | Graftech International Holdings Inc. | High coking value pitch |
| CN102399491A (en) * | 2011-09-14 | 2012-04-04 | 江苏斯泰达新能源科技发展有限公司 | Polyurethane prime coat specifically for concrete surface treatment |
| KR20140146003A (en) * | 2013-06-13 | 2014-12-24 | 오씨아이 주식회사 | Highly efficient method for manufacturing pitch as carbonaceous raw material |
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