CN107880921B - Petroleum-series multifunctional asphalt resin and preparation method thereof - Google Patents
Petroleum-series multifunctional asphalt resin and preparation method thereof Download PDFInfo
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- CN107880921B CN107880921B CN201711115381.8A CN201711115381A CN107880921B CN 107880921 B CN107880921 B CN 107880921B CN 201711115381 A CN201711115381 A CN 201711115381A CN 107880921 B CN107880921 B CN 107880921B
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- 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
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Abstract
The invention relates to a petroleum series multifunctional asphalt resin and a manufacturing method thereof, wherein petroleum series aromatic hydrocarbon components are taken as raw materials, the raw materials are mixed with gas oil generated by a system before entering a device, mixed oil is preheated by using the waste heat of the system and then subjected to component separation to remove hydrocarbon components which are extremely volatile, and the rest components are heated to a high enough temperature for heat treatment, wherein the main reactions in the process comprise thermal cracking, thermal polymerization, aromatization and the like. The heat-treated material is subjected to component separation in modes of flash evaporation, quenching, normal pressure or negative pressure distillation and the like, so that small molecular components are further separated, and the rest components are the target product of the invention, namely petroleum multifunctional asphalt resin. The asphalt has high residual carbon value, low solid content (QI is almost zero) and low viscosity, and has excellent service performance when used as raw materials of binder asphalt, impregnant asphalt, coating asphalt, C/C composite material and carbon fiber.
Description
Technical Field
The invention belongs to the technical field of petrochemical industry, and particularly relates to a method for manufacturing petroleum multifunctional asphalt resin.
Background
In the carbon industry, a binder is needed in the kneading and forming process of a carbon product, and the binder plays a role in endowing the material with plasticity by wetting, permeating and adsorbing the binder to the surface of the solid material, so that the carbon product is beneficial to next-step forming. According to the principle of chemical similarity, the more similar the substances in contact with each other in chemical property, the stronger the interaction between the substances, so that the pitch is generally used as the binder in the carbon product at present.
The carbon product is formed for the first time, pores exist in the carbon product and on the surface of the carbon product in different degrees, the pores account for about 25% of the volume of the carbon product, the existence of the pores can influence the performance of the carbon product, including the strength, the electric conduction, the heat conduction, the ablation resistance and the like of the product, for example, the carbon products such as a large graphite electrode, an electric brush, a C/C composite material and the like need to be subjected to densification treatment, the technical indexes such as the density, the strength, the electric conductivity, the heat conductivity, the ablation resistance and the like of the carbon product are improved, and the application requirement of the carbon product can be met.
Carbon article densification processes typically include both liquid phase impregnation processes and Chemical Vapor Infiltration (CVI) processes, with liquid phase impregnation still being the primary process currently employed for carbon article densification. At present, the impregnant mainly comprises resin and asphalt, but the performance of the impregnant has important influence on the impregnation process, such as impregnation cost, product density uniformity, carbon structure and the like.
According to the dipping process, the required impregnant has the following requirements of ① high residual carbon value, which can reduce dipping times and reduce cost, ② low solid content (low QI value), which causes solid particles to easily block pore channels in the dipping process and even forms a filter cake on the surface of a product, thus affecting dipping efficiency and increasing dipping cost, ③ viscosity which affects dipping effect, and low viscosity which causes the impregnant to easily flow into pores, thus being beneficial to dipping operation and reducing operation cost, and ④ wettability which causes the impregnant to have good wettability with the product and is beneficial to the impregnant to enter the pores.
At present, no special impregnant asphalt exists in China, but the impregnant asphalt is replaced by the binder asphalt, the solid content in the binder asphalt is high, the impregnation effect is poor, and therefore, the performance requirement of the carbon product is met by increasing the impregnation times, and the impregnation cost is increased. In addition, for high-power and over-power graphite electrodes, special impregnant is needed, and the performance index of the electrodes cannot be met by replacing the impregnant with binder asphalt. The special impregnant asphalt used in China at present mainly depends on import.
In the preparation process of the lithium ion secondary battery, natural graphite is a main source of a negative electrode material due to high charge and discharge capacity, a good charge and discharge platform, wide sources and low cost, but the natural graphite has high graphitization degree, so that the difference between the crystal structure and other physical and chemical properties between the edge and the bottom surface of a microcrystal is large, and the decomposition reaction with an electrolyte mainly occurs at the edge part of the microcrystal. Therefore, the produced purification membrane has poor compactness, and co-intercalation of solvated lithium ions is likely to occur during charging, which causes expansion and collapse of graphite layers and increases irreversible capacity. In addition, natural graphite has the defect of poor bonding property with a polar plate after being treated by a physical or chemical method, and is easy to fall off from the polar plate in the cyclic charge-discharge process, so that the cyclic life is influenced, and particularly, the cyclic life of large-current charge-discharge is reduced. In order to improve the electrochemical performance of natural graphite materials, people perform physical and chemical modification and surface modification on natural graphite through various methods, and the main method adopted at present is to coat asphalt on the surface of the natural graphite.
The technical requirements for coating bitumens are, on the one hand, a high residual carbon number and, on the other hand, a good adhesion, which are in accordance with the requirements for binder bitumens and impregnant bitumens.
The pitch resin can be applied to raw materials for producing C/C composite materials and carbon fibers because the pitch resin can easily form an intermediate phase.
Disclosure of Invention
The invention relates to a petroleum series multifunctional asphalt resin and a manufacturing method thereof, the method takes petroleum series aromatic hydrocarbon components as raw materials, the raw materials are firstly mixed with gas oil (called as 'gas oil' for short) generated by a system before entering a device, the mixed oil is preheated and heated by utilizing the waste heat of the system, the components of the mixed oil are separated after being heated, the hydrocarbon components which are extremely easy to volatilize are removed, the residual components are further heated to a high enough temperature for heat treatment, a series of chemical reactions can occur in the process, and the main reactions comprise thermal cracking, thermal polymerization, aromatization and the like. The heat-treated material is subjected to component separation in modes of flash evaporation, normal pressure or negative pressure distillation and the like (or any combination of a plurality of separation modes), so that small molecular components are further separated, and the residual component is the target product of the invention, namely the petroleum multifunctional asphalt resin.
Specifically, the method for producing a petroleum-based multifunctional asphalt resin according to the present invention comprises the steps of:
(1) mixing a fresh raw material and gas oil, preheating by using system waste heat, and preheating the mixed oil to 250-380 ℃; wherein the raw material is selected from FCC catalytic cracking clarified oil, FCC catalytic cracking crude oil slurry, ethylene cracking tar, C9 distillate oil and/or components of the raw material after component separation, and the like, and the ash content in the raw material is preferably and strictly controlled, and is generally less than 500PPm, and the optimal content is less than 200 PPm.
Wherein, the raw materials involved above are respectively:
catalytic cracking of crude oil slurry: the distillate oil thrown from the bottom of the fractionating tower of the catalytic cracking unit is called crude oil slurry because of containing a small amount of catalyst powder; the oil slurry contains rich aromatic hydrocarbon components.
Catalytic cracking of clarified oil: the catalytic cracking crude oil slurry is treated by settling, distilling or filtering to remove catalyst powder (generally, the catalyst powder is reduced to below 500 PPm). The oil product contains rich aromatic hydrocarbon components.
Ethylene cracking tar: the by-product obtained in the ethylene cracking process due to the occurrence of secondary reaction. The oil product contains rich aromatic hydrocarbon components.
C9 distillate oil: is the distillate oil which is the byproduct of ethylene cracking.
Gas oil: is the middle distillate oil obtained by the process during atmospheric distillation or vacuum distillation.
(2) Carrying out component separation on the preheated mixed oil by using a fractionating device, and removing extremely volatile hydrocarbon components;
(3) heating the residual components obtained in the step (2) to 350-580 ℃ by heating equipment, and then performing heat treatment operation, wherein the pressure is controlled within the range of 0.7-3.2 Mpa, and the heat treatment time is controlled within 15-650 seconds. Under the process condition, the materials can generate a series of chemical reactions, wherein the main reactions comprise thermal cracking, thermal polymerization, aromatization and other chemical reactions; in the process, the heating and temperature raising of the mixed oil material and the heat treatment reaction can be carried out simultaneously or in two steps (the simultaneous operation means that the material heating and the chemical reaction are carried out and finished in the same equipment;
(4) performing component separation on the material reacted in the step (3) in a flash evaporation, quenching, normal pressure distillation, negative pressure distillation or any combination mode to remove volatile components, wherein the flash evaporation temperature is controlled within the range of 280-530 ℃, and the flash evaporation pressure is controlled within the range of 0.3-1.8 Mpa; the quenching and distillation temperature is controlled within 240-380 ℃, and the distillation pressure is controlled within 5-860 mmHg (absolute pressure);
(5) and (4) granulating or flaking the residual components (distillation residual components) prepared in the step (4) to obtain the target product, namely the petroleum multifunctional asphalt resin.
For the above-mentioned method for producing a petroleum-based multifunctional asphalt resin, it is preferable that the remaining components obtained in the step (2) are heated to 350 to 580 ℃ by a heating device.
In the above-mentioned method for producing a petroleum-based multifunctional asphalt resin, the temperature for preheating the mixed oil in the step (1) is preferably 270 to 340 ℃.
In the above-mentioned method for producing a petroleum-based multifunctional asphalt resin, it is preferable that the pressure in the step (3) is controlled to 1.0 to 2.2 MPa.
In the above-mentioned method for producing a petroleum-based multifunctional asphalt resin, the heat treatment time in the step (3) is preferably controlled to 55 to 450 seconds.
The multifunctional asphalt resin prepared by the process has excellent performance, and the main technical indexes comprise ① softening point 80-150 ℃, ② carbon residue value 42-63%, ③ Toluene Insoluble (TI) 4-18%, ④ solid content (QI) 0-0.08%, ⑤ density 1.16-1.25 g/cm3⑥ the carbon content is 92-95%.
The multifunctional asphalt resin has high residual carbon value, low solid content (QI is almost zero) and low viscosity, and has excellent service performance when used as binder asphalt and impregnant asphalt. The method is mainly applied to the binder or densification treatment of graphite electrodes, graphite carbon brushes and C/C composite materials. Is particularly suitable for preparing high-power and ultrahigh-power graphite electrodes, fills up the domestic blank and replaces the import. Meanwhile, the pitch resin can also be used as a coating agent of a negative electrode material of a lithium ion secondary battery and is an ideal raw material for preparing mesophase pitch and isotropic pitch-based carbon fiber.
In the technical scheme, the temperature for separating the components is raised to 250-380 ℃.
Compared with the traditional intermittent preparation process, the continuous preparation process has the advantages that:
① because the heat treatment time of the process is short (15-650 seconds), the reaction degree is easy to control, namely the generation of macromolecular components, namely QI components, is strictly controlled and is used as the impregnated asphalt resin, the solid content (QI) is a very important control index, the solid content (QI) of the target product is 0-0.08%, and the index is extremely difficult to achieve by a batch preparation process;
② the process combines reaction process and separation process to make the molecular weight distribution of the target product-pitch resin narrow, the target product belongs to mesomorphic pitch resin, and is an ideal raw material for preparing pitch-based carbon fiber and mesophase pitch;
③ the process has high product yield (not less than 85%), easy control, and stable product quality;
④ the process has high operation flexibility, strong adaptability to raw materials, and little influence of the variability of the raw materials on the target product;
⑤ the process has high production efficiency, full utilization of system waste heat in the process, energy saving, emission reduction, low cost and easy industrial conversion.
Drawings
FIG. 1 is a flow chart of the process for preparing the multifunctional asphalt resin of the present invention;
Detailed Description
The following non-limiting examples will allow one of ordinary skill in the art to more fully understand the present invention, but are not intended to limit the invention in any way.
Example 1
Extracting about 30Kg of FCC catalytic cracking clarified oil serving as a raw material into a buffer tank, pumping the raw material out by a raw material conveying pump, mixing the raw material with gas oil, heating the mixed oil after heat exchange with a system waste heat exchanger to 310 ℃, fractionating the heated mixed oil in a fractionating device to remove low molecular components, heating the fractionated mixed oil in a heating device to 545 ℃, heating the mixed oil in a heat treatment device, controlling the heat treatment time within 90-95 seconds and the pressure within 2.0MPa, feeding the reacted material into a flash evaporation tank for flash evaporation, controlling the flash evaporation temperature to be 505 ℃ and the flash evaporation pressure to be 1.1MPa, feeding the flash evaporated material into a vacuum tower by a material conveying pump for distillation operation, controlling the distillation pressure to be 25mmHg (absolute pressure), controlling the distillation temperature to be 305 ℃, and pumping the bottom materials of the vacuum tower by an asphalt resin pump, sending the mixture into a buffer tank. The materials in the buffer tank are target products, and the detected technical indexes are shown in table 1 in detail.
Example 2
Extracting about 30Kg of aromatic oil (aromatic oil refers to that the catalytic cracking clarified oil is distilled and extracted by a solvent to remove saturated components and the residual aromatic fraction-rich oil) as a raw material into a buffer tank, pumping the raw material out by a raw material delivery pump and mixing with gas oil, raising the temperature of the mixed oil after heat exchange with a system waste heat exchanger to 290 ℃, feeding the mixed oil after temperature raising into a fractionating device for fractionating to remove low molecular components, feeding the mixed oil after fractionating into a heating device for further heating and raising the temperature, raising the temperature of the mixed oil to 495 ℃, feeding into a heat treatment device, controlling the heat treatment time within the range of 120-130 seconds, controlling the pressure to be 1.5MPa, feeding the reacted material into a flash tank for flash evaporation, controlling the flash evaporation temperature to be 470 ℃, controlling the flash evaporation pressure to be 0.7MPa, feeding the flash evaporated material into a vacuum tower through a material delivery pump for distillation operation, the distillation pressure was controlled to 16mmHg (absolute pressure), the distillation temperature was 370 ℃ and the vacuum column bottoms were pumped out by a pitch resin pump and sent into a buffer tank. The materials in the buffer tank are target products, and the detected technical indexes are shown in table 1 in detail.
Example 3
Extracting about 30Kg of raw material ethylene tar (ethylene cracking tar: a byproduct obtained by a secondary reaction in the process of preparing ethylene by steam cracking, wherein the oil contains rich aromatic hydrocarbon components) into a buffer tank, pumping out the raw material by a raw material conveying pump, mixing the raw material with gas oil, raising the temperature of the mixed oil after heat exchange with a system waste heat exchanger to 280 ℃, feeding the mixed oil after temperature raising into a fractionating device for fractionating to remove low molecular components, feeding the mixed oil after fractionation into a heating device for further heating to raise the temperature, raising the temperature of the mixed oil to 475 ℃, feeding the mixed oil into a heat treatment device, controlling the heat treatment time to be in the range of 370-380 seconds, controlling the pressure to be 1.9Mpa, feeding the reacted material into a flash tank for flash distillation, controlling the flash evaporation temperature to be 410 ℃, controlling the flash evaporation pressure to be 0.9Mpa, feeding the flash evaporated material into a vacuum tower through a material conveying pump for distillation operation, the distillation pressure was controlled to 74mmHg (absolute pressure), the distillation temperature was 320 ℃ and the vacuum column bottoms were pumped out by a pitch resin pump and sent into a buffer tank. The materials in the buffer tank are target products, and the detected technical indexes are shown in table 1 in detail.
Example 4
Extracting about 30Kg of distillate oil of raw material C9 to a buffer tank, pumping the raw material out by a raw material delivery pump, mixing the distillate oil with the raw material, raising the temperature of the mixed oil after heat exchange with a system waste heat exchanger to 270 ℃, feeding the mixed oil after temperature raising into a fractionating device for fractionating to remove low molecular components, feeding the fractionated mixed oil into a heating device for further heating and raising the temperature of the mixed oil to 380 ℃, feeding the mixed oil into a heat treatment device, controlling the heat treatment time to be within 60-70 seconds, controlling the pressure to be 1.9Mpa, feeding the reacted material into a flash evaporation tank for flash evaporation at the flash evaporation temperature of 330 ℃ and the flash evaporation pressure of 0.8Mpa, feeding the flash evaporated material into an atmospheric tower by a material delivery pump for distillation operation, controlling the distillation pressure to be 780mmHg (absolute pressure), controlling the distillation temperature to be 290 ℃, pumping the atmospheric tower bottom material by an asphalt resin pump, sending the mixture into a buffer tank. The materials in the buffer tank are target products, and the detected technical indexes are shown in table 1 in detail.
TABLE 1 test results of the examples
Claims (7)
1. A method for manufacturing petroleum multifunctional asphalt resin is characterized in that: the method comprises the following steps:
(1) mixing a fresh raw material and gas oil, preheating, and preheating the mixed oil to 250-380 ℃, wherein the ash content in the raw material is less than 500 PPm;
(2) carrying out component separation on the preheated mixed oil by using a fractionating device, and removing extremely volatile hydrocarbon components;
(3) raising the temperature of the residual components obtained in the step (2) to 350-580 ℃ through heating equipment, and then carrying out heat treatment operation, wherein the pressure is controlled within the range of 0.7-3.2 MPa, and the heat treatment time is controlled within 15-650 seconds;
(4) performing component separation on the material reacted in the step (3) by any combination of flash evaporation, quenching, normal pressure distillation, negative pressure distillation or several separation modes to remove volatile components, wherein the flash evaporation temperature is controlled within the range of 280-530 ℃, and the flash evaporation pressure is controlled within the range of 0.3-1.8 MPa; the quenching and distilling temperature is controlled within the range of 240-380 ℃, and the distilling pressure is controlled within the range of 5-860 mmHg;
(5) granulating or flaking the distillation residual components in the step (4) to obtain the target product of the invention, namely petroleum multifunctional asphalt resin;
(6) and (4) returning the gas oil produced in the step (4) to the system again to be mixed with the fresh raw material, and repeating the continuous production according to the steps (1) to (5).
2. The method of claim 1, wherein the raw material is selected from the group consisting of FCC catalytically cracked decant oil, FCC catalytically cracked crude oil slurry, ethylene cracked tar, C9 distillate, and any fraction of the raw materials after separation.
3. The method for producing a petroleum-based multifunctional asphalt resin according to claim 1, wherein the ash content in the raw material of the step (1) is less than 200 PPm.
4. The method for producing a petroleum-based multifunctional asphalt resin according to claim 1, wherein the temperature for preheating the mixed oil in the step (1) is 270 to 340 ℃.
5. The method for producing a petroleum-based multifunctional asphalt resin according to claim 1, wherein the pressure in the step (3) is controlled to 1.0 to 2.2 MPa.
6. The method for producing a petroleum-based multifunctional asphalt resin according to claim 1, wherein the heat treatment time in the step (3) is controlled to 55 to 450 seconds.
7. The petroleum multifunctional asphalt resin prepared by the method of claim 1 has the main technical indexes of ① softening point of 80-150 ℃, ② residual carbon value of 42-63%, ③ toluene insoluble substance of 4-18%, ④ solid content of 0-0.08%, ⑤ density of 1.16-1.25 g/cm3 and ⑥ carbon element content of 92-95%.
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| CN1032922C (en) * | 1987-06-18 | 1996-10-02 | 丸善石油化学株式会社 | Process for preparing mesophase pitches |
| JP5231316B2 (en) * | 1998-06-04 | 2013-07-10 | 東洋炭素株式会社 | Carbon fiber reinforced carbon composite material, member for single crystal pulling apparatus, and method for producing carbon fiber reinforced carbon composite material |
| CN1158415C (en) * | 2000-12-06 | 2004-07-21 | 辽阳石油化纤公司亿方化工实验二厂 | Prepn of petroleum asphalt-base common carbon fiber material |
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