Preparation method and application of high-softening-point coated asphalt with ultralow quinoline insoluble content

Abstract

The invention discloses a preparation method and application of high-softening-point coated asphalt with ultralow quinoline insoluble content, and relates to the technical field of asphalt preparation and detection.The preparation method comprises the following steps that ethylene tar and catalytic slurry oil are mixed, settled and heated to obtain a pretreated product, the pretreated product is subjected to an oxidation cross-linking catalytic reaction and a polycondensation catalytic reaction, and the high-softening-point coated asphalt with ultralow quinoline insoluble content is obtained; according to the method disclosed by the invention, the temperature and pressure conditions in the detection working process can be dynamically limited and compensated, the effective temperature rise and heating coverage range of water bath heating is enlarged, the holding of the effective heating temperature of a heating medium on the detection work is relieved, and the detection efficiency is improved. According to the present invention, the flow characteristic, the viscosity and the needle penetration detection requirements of the high softening point covering asphalt are met, the heating balance of the covering asphalt during the detection work process is improved, the energy dissipated during the heating work process can be reutilized, and the energy saving effect of the detection work is improved.

Description

Technical Field

[0001] The present invention relates to the technical field of asphalt preparation and detection, and specifically to a preparation method and application of high softening point coated asphalt with ultra-low quinoline insoluble content. Background Technique

[0002] After the coated asphalt is used to modify the anode material of lithium batteries, the performance of the anode material will be significantly improved. Commercial anode materials for lithium batteries require the coated asphalt to have a high softening point and coking value, as well as a low quinoline insoluble content. At the same time, it is necessary to ensure that the prepared asphalt product has a high yield. During the preparation process of the coated asphalt, corresponding equipment is required to detect the relevant performance parameters of the coated asphalt. A Chinese patent discloses an inspection device for polymer modified asphalt, with the application number: 202222510490.2. This patent facilitates pouring the asphalt into the placement bucket, thereby improving the detection efficiency of the asphalt.

[0003] However, in the current detection method, during the preparation process of high softening point coated asphalt, it is impossible to provide suitable pre-temperature conditions for the flow characteristic detection and viscosity detection stably and sufficiently. The flow characteristic detection and viscosity detection are restricted by the heat medium temperature, and the detection work requires an additional power source to drive multiple external driving devices to work together, resulting in poor energy conservation of the detection work and an increase in the detection cost. Summary of the Invention

[0004] The present invention provides a preparation method of high softening point coated asphalt with ultra-low quinoline insoluble content, which can effectively solve the problems proposed in the above background technique, that is, in the current detection method, during the preparation process of high softening point coated asphalt, it is impossible to provide suitable pre-temperature conditions for the flow characteristic detection and viscosity detection stably and sufficiently. The flow characteristic detection and viscosity detection are restricted by the heat medium temperature, and the detection work requires an additional power source to drive multiple external driving devices to work together, resulting in poor energy conservation of the detection work and an increase in the detection cost.

[0005] To achieve the above object, the present invention provides the following technical solution: A preparation method of high softening point coated asphalt with ultra-low quinoline insoluble content, including the following steps:

[0006] S1. Pretreatment: Mix ethylene tar and catalytic slurry in a mass ratio of 9:1, perform physical stirring at a rotation speed of 220 rpm for 10 hours at room temperature, add an AS204 slurry settling agent, and the mass ratio of the settling agent to the total amount of ethylene tar and catalytic slurry is 1:5. Perform sedimentation for 36 hours, and perform heat treatment on the sedimented mixture at 120 °C for 1 hour to obtain a pretreatment product. Put the pretreatment product into a high-temperature and high-pressure reaction kettle for multi-stage heating reaction;

[0007] S2. Catalytic reaction: A mixed gas of oxygen and nitrogen with an oxygen content of 8% is introduced at a ventilation rate of 1000 sccm. Vinyltriethoxysilane is added, and its dosage is 1 / 60 of the total mass of the raw materials. An oxidative cross-linking catalytic reaction is carried out at a temperature of 280 °C for 4 hours. Then nitrogen is introduced at a ventilation rate of 2000 sccm. Atactic poly-α-olefin and ferric trichloride are added, and their dosage is 1 / 30 of the total mass of the raw materials. A polycondensation catalytic reaction is carried out at a temperature of 340 °C for 8 hours to obtain a crude asphalt product;

[0008] S3. Product refinement: The crude asphalt product is naturally cooled for 1 hour. Quinoline is added to the crude asphalt, and the mass ratio of quinoline to the crude asphalt product is 2:1. Extraction is carried out 3 times, and coated asphalt is obtained after drying;

[0009] S4. Performance detection: An appropriate amount of the prepared coated asphalt is taken to make a sample. The coated asphalt is added to the detector, and its flow characteristics, viscosity, penetration, and softening point are detected by the boosting detection machine and the partition outward expansion mechanism. The determination of quinoline insoluble content, coking value, and yield is completed using the corresponding equipment.

[0010] According to the above technical solution, the application of a high softening point coated asphalt with ultra-low quinoline insoluble content is characterized in that the coated asphalt prepared according to the preparation method of the high softening point coated asphalt with ultra-low quinoline insoluble content is used for but not limited to lithium batteries.

[0011] According to the above technical solution, a boosting detection mechanism is installed on one side of the top of the detector, and the boosting detection mechanism includes a cylinder;

[0012] A cylinder is installed on one side of the top of the detector. A heat conduction cylinder is installed inside the cylinder. A round box is installed at the bottom of the heat conduction cylinder. A guide seat is embedded at the top edge of the heat conduction cylinder. Pressure-resistant pipes are symmetrically installed on both sides of the outer curved surface of the guide seat. A notch is opened at the bottom edge of the round box. A turbine is rotatably installed inside the round box;

[0013] A shaft seat is installed at the end of the turbine. A pin shaft is slidably clamped at the top of the shaft seat. A torque sensor is installed at the top of the pin shaft. A shaft cylinder is installed at the end of the torque sensor. A number of rod bodies are evenly installed at equal intervals on both sides of the outer curved surface of the shaft cylinder. A temperature sensor is embedded in the middle of the outer curved surface of the shaft cylinder. A number of heating rods are installed on the outer side of the heat conduction cylinder at equal angles along the circumferential direction. A coil is wound around the outer curved surface of the cylinder;

[0014] A discharge valve is installed at the bottom of the outer curved surface of the heat conduction cylinder. A water replenishing valve is embedded at the top of the outer curved surface of the cylinder. A top cover is installed at the top of the cylinder.

[0015] According to the above technical solution, a ring shell is installed at the bottom end of the round box, an insertion tube is installed on one side of the outer curved surface of the ring shell, a sliding cavity is opened at a position corresponding to the end of the insertion tube inside the detector, a round plug is slidably installed inside the sliding cavity, an exhaust port is opened on the other side of the outer curved surface of the sliding cavity corresponding to the round plug, a gas guiding valve is embedded and installed at a position corresponding to the top of the round plug on the outer curved surface of the sliding cavity, and a pressure sensor is embedded and installed in the middle of the top end of the sliding cavity.

[0016] According to the above technical solution, a water bath cavity is formed by enclosing the inner wall of the cylinder body and the outer wall of the heat conduction cylinder. The heating rod is located inside the water bath cavity. The water replenishing valve is communicated with the water bath cavity, and the bottom of the guide seat is directly communicated with the water bath cavity.

[0017] According to the above technical solution, the pressure-resistant tube is spiral, an inner clamping cavity is opened at a position corresponding to the pressure-resistant tube on the side wall of the cylinder body, and the guide seat is connected to the round box through the pressure-resistant tube.

[0018] According to the above technical solution, the ring shell is communicated with the round box through a notch. The thickness of the round plug is greater than the diameter of the exhaust port. Air is filled at a position corresponding to the top of the round plug inside the sliding cavity. The output ends of the torque sensor, the temperature sensor and the pressure sensor are all connected to the input end of the detector. The input end of the detector is electrically connected to the output end of the external power supply through a coil.

[0019] According to the above technical solution, a partition expanding mechanism is installed on the outside of the shaft cylinder. The partition expanding mechanism includes a transmission seat;

[0020] A transmission seat is installed at the top end of the top cover. A top seat is installed at the top end of the transmission seat. Electric push rods are installed at positions corresponding to both sides of the top seat on the top end of the detector. An impeller is rotatably installed inside the top seat. A rotating rod is embedded and rotatably installed at the bottom end of the top cover. An air suction port is opened in the middle of the top end of the top seat. A gas guiding column is installed on one side of the outer curved surface of the top seat. A connecting pipe is installed on the top of the outer curved surface of the transmission seat;

[0021] A number of detection needles are embedded and slidably installed at the bottom end of the transmission seat along the circumferential direction at equal angles. A piston plate is installed at the top end of the detection needle. A displacement sensor is embedded and installed in the middle of the top end of the piston plate. A vertical cavity is opened at a position corresponding to the piston plate inside the transmission seat. A circular block is slidably installed inside the gas guiding column. An air exhaust port is opened on the top of the outer curved surface of the gas guiding column corresponding to the circular block. A pressure sensor is embedded and installed at the end of the gas guiding column. A gas nozzle is embedded and installed at a position close to the pressure sensor on the top of the outer curved surface of the gas guiding column;

[0022] A partition board is rotatably installed at the top of the outer curved surface of the torque sensor. A softening point detection bracket assembly is installed at the bottom end of the partition board. At the bottom end of the softening point detection bracket assembly, clamping rods are symmetrically installed. At the positions corresponding to the clamping rods at the bottom end of the heat conduction cylinder, rod sleeves are installed. At the position between the heat conduction cylinder and the round box on the outer curved surface of the shaft seat, a paddle is installed. A plurality of side holes are equiangularly formed in the middle of the outer curved surface of the heat conduction cylinder along the circumferential direction. A bottom hole is formed in the middle of the bottom end of the heat conduction cylinder.

[0023] According to the above technical solution, air is filled inside the air guide column corresponding to the air nozzle position. The thickness of the circular block is greater than the diameter of the air discharge port. The force-bearing area of the circular block is the same as the force-bearing area of the piston plate. The output ends of the displacement sensor and the pressure sensor are both connected to the input end of the detector. The input end of the electric push rod is electrically connected to the output end of the external power supply.

[0024] According to the above technical solution, the impeller is connected to the shaft cylinder through a rotating rod, and both the transmission seat and the top seat are rotatably connected to the rotating rod. The clamping rod is slidably connected to the rod sleeve. The inner diameter of the bottom hole is greater than the outer diameter of the shaft seat.

[0025] Compared with the prior art, the beneficial effects of the present invention are as follows: The structure of the present invention is scientific and reasonable, and it is safe and convenient to use;

[0026] 1. By mixing and settling vinyl tar and catalytic oil slurry, the raw materials are fully mixed and impurities are removed, which can improve the effects of oxidative crosslinking and polycondensation reactions. At the same time, under the action of a catalyst, oxidative crosslinking and polycondensation reactions are carried out in sequence. Through oxidative crosslinking, the remaining light components in the asphalt can be promoted to crosslink into macromolecules, which can effectively increase the residual carbon value of the coated asphalt. When coating, it is beneficial to carbonize the asphalt to form more amorphous carbon, thereby improving the electrochemical performance of the negative electrode material;

[0027] Through the polycondensation reaction, the dehydrogenation and aromatization of unsubstituted aromatic hydrocarbons in the asphalt can be accelerated, and the softening point of the asphalt can be greatly increased. By means of extraction, the content of quinoline insoluble substances in the coated asphalt is effectively reduced. Therefore, the softening point and coking value of the prepared coated asphalt can be effectively increased, and the content of its quinoline insoluble substances can be reduced, so that the softening point, quinoline insoluble substance content, coking value and yield of the prepared coated asphalt can simultaneously meet the commercial requirements of the coated asphalt for the negative electrode material. After the prepared coated asphalt is coated on the negative electrode material of the lithium-ion battery, the actual specific capacity and cycle stability of the battery negative electrode material can be effectively improved.

[0028] 2. A boosting detection mechanism is provided. By the cooperation of a cylinder body, a heating rod, a coil heat conduction cylinder, a round box, a guide seat, a pressure-resistant pipe and a notch, a temperature limiting structure can be constructed, which can provide stable preconditions for the temperature control work in the process of detecting the coated asphalt, greatly improving the convenience and stability of temperature control. And by effectively using the pressure limiting and regulating functions of an annular shell, an insertion pipe, a sliding cavity, a round plug, an exhaust port, a gas guiding valve and a pressure sensor, the temperature and pressure conditions in the detection process can be dynamically limited and compensated. On the one hand, the effective heating coverage range of water bath heating can be effectively increased, the restriction of the effective heating temperature of the heat medium on the detection work can be removed, the detection requirements for the flow characteristics, viscosity and penetration of the coated asphalt with a high softening point can be fully met, the required temperature for the detection work can be provided more conveniently and efficiently, and the detection work can be carried out more efficiently and stably;

[0029] On the other hand, the stability of the heating work can be greatly improved, and the heat balance during the detection of the flow characteristics, viscosity and penetration of the coated asphalt can be greatly improved, so that the detection effect is improved and the detection work is more accurate and reliable. On the other hand, by cooperating with a turbine, a shaft seat, a pin shaft, a torque sensor, a shaft cylinder, a rod body and a temperature sensor, a detection execution structure can be formed, which can reuse the energy dissipated during the heating process, convert the kinetic energy of water vapor into the power source of the detection work, and realize the detection of the flow characteristics and viscosity of the coated asphalt without an additional power source and a driving device. While improving the energy-saving effect of the detection work and making the detection work more energy-saving and emission-reducing, the demand for electrical equipment can be reduced, the cost demand for detection equipment can be reduced, the detection cost can be effectively reduced, the detection work can be made more efficient, the effectiveness of the detection work can be effectively improved, the coordination and synchronization among various detection works can be improved, and the detection work can be made more stable.

[0030] 3. A partition expansion mechanism is provided. By the cooperation of a transmission seat, a top seat, an impeller and a rotating rod, a mechanical transmission conversion structure can be constructed, which can reuse the kinetic energy in the process of detecting the flow characteristics. Coupled with the transmission conversion functions of an air suction port, a gas guiding column, a connecting pipe, a piston plate and a vertical cavity, it can cooperate with a detection needle and a displacement sensor to realize the multiple reuse of kinetic energy and synchronously realize the penetration detection of the coated asphalt. It can cooperate with the boosting detection mechanism to realize the dynamic monitoring of the coated asphalt under different temperature and pressure conditions, and realize the synchronous detection of the coated asphalt from multiple dimensions, comprehensively detect and measure the performance of the coated asphalt from multiple levels, greatly improving the sufficiency, comprehensiveness and effectiveness of the detection work, and making the detection results more accurate and reliable;

[0031] By cooperating with a circular block, an air outlet, an air nozzle and a pressure sensor, a pneumatic pressure regulating structure can be constructed, which, in cooperation with a boosting detection mechanism, can provide different temperature and pressure conditions for the penetration test work. While improving the convenience of adjusting the test conditions, the test work can be made more flexible and efficient. By cooperating with a clamping rod, a rod sleeve and a partition plate, a partition limiting structure can be constructed, which can partition and limit a heat conducting cylinder and limit a softening point test support assembly, providing a more stable and adaptable precondition for the softening point test work, and simultaneously realizing the softening point test work of coated asphalt. While improving the convenience of the test work, the use range of the test device can be effectively expanded, and the functionality of the test device can be effectively enriched. By cooperating with a paddle, side holes and bottom holes, dynamic water bath heating can be realized, further promoting the temperature balance of the heating work and making the test work more efficient and stable.

[0032] In summary, by cooperating with a boosting detection mechanism and a partition expanding mechanism, the covered temperature range of the water bath heating can be effectively increased, the traditional industry bottleneck can be effectively broken through, the precondition temperature condition requirements for the high softening point coated asphalt test work can be effectively met, the comprehensive tests of the flow characteristics, viscosity, penetration and softening point of the coated asphalt can be realized simultaneously, making the test work more comprehensive and efficient, simultaneously improving the test efficiency and effect, and the energy in the test work can be utilized multiple times, effectively improving the energy saving effect of the test work and reducing the test cost. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] The drawings are used to provide a further understanding of the present invention, and constitute a part of the specification. They are used together with the embodiments of the present invention to explain the present invention, and do not constitute a limitation to the present invention.

[0034] In the drawings:

[0035] Figure 1 is a flowchart of the steps of the preparation method of the present invention;

[0036] Figure 2 is a three-dimensional structural schematic diagram of the present invention;

[0037] Figure 3 is a schematic diagram of the heat conducting cylinder installation structure of the present invention;

[0038] Figure 4 is a schematic diagram of the round box installation structure of the present invention;

[0039] Figure 5 is a schematic diagram of the boosting detection mechanism structure of the present invention;

[0040] Figure 6 is a schematic diagram of the guide seat installation structure of the present invention;

[0041] Figure 7 is a schematic diagram of the shaft cylinder installation structure of the present invention;

[0042] Figure 8 is a schematic structural diagram of the partition expansion mechanism of the present invention;

[0043] Figure 9 is a schematic structural diagram of the detection needle installation of the present invention;

[0044] Reference numerals in the figure: 1, detector; 11, discharge valve; 12, water replenishing valve; 13, top cover; 14, electric push rod; 15, softening point detection bracket assembly;

[0045] 200, boost detection mechanism; 201, cylinder body; 202, heat conduction cylinder; 203, round box; 204, guide seat; 205, pressure-resistant pipe; 206, notch; 207, turbine; 208, shaft seat; 209, pin shaft; 210, torque sensor; 211, shaft cylinder; 212, rod body; 213, temperature sensor; 214, heating rod; 215, coil; 216, ring shell; 217, insertion tube; 218, sliding cavity; 219, round plug; 220, exhaust port; 221, air guide valve; 222, air pressure sensor;

[0046] 2021, water bath cavity; 2051, inner clamping cavity;

[0047] 300, partition expansion mechanism; 301, transmission seat; 302, top seat; 303, impeller; 304, rotating rod; 305, suction port; 306, air guide column; 307, connecting pipe; 308, detection needle; 309, piston plate; 310, displacement sensor; 311, vertical cavity; 312, circular block; 313, exhaust port; 314, air nozzle; 315, pressure sensor; 316, isolation plate; 317, clamping rod; 318, rod sleeve; 319, paddle; 320, side hole; 321, bottom hole. Specific embodiments

[0048] The following is a description of the preferred embodiments of the present invention with reference to the accompanying drawings. It should be understood that the preferred embodiments described herein are only for the purpose of illustrating and explaining the present invention, and are not intended to limit the present invention.

[0049] Embodiment: As Figure 1 shown, the present invention provides a technical solution, a method for preparing high softening point coated pitch with ultra-low quinoline insoluble content, including the following steps:

[0050] S1. Pretreatment: Mix vinyl tar and catalytic slurry oil at a mass ratio of 9:1, conduct physical stirring at a rotation speed of 220 rpm for 10 hours at room temperature, add AS204 slurry settling agent, with the mass ratio of the settling agent to the total amount of vinyl tar and catalytic slurry oil being 1:5, conduct settling for 36 hours, and conduct heat treatment on the settled mixture at 120 °C for 1 hour to obtain a pretreated product. Place the pretreated product in a high-temperature and high-pressure reactor for multi-stage heating reaction;

[0051] S2. Catalytic reaction: Pass in a mixture of oxygen and nitrogen with an oxygen content of 8%, with a gas flow rate of 1000 sccm, add vinyltriethoxysilane, with the dosage being 1 / 60 of the total mass of the raw materials, conduct oxidative cross-linking catalytic reaction at a temperature of 280 °C for 4 hours, pass in nitrogen, with a gas flow rate of 2000 sccm, add random poly-α-olefin and ferric trichloride, with the dosage being 1 / 30 of the total mass of the raw materials, conduct polycondensation catalytic reaction at a temperature of 340 °C for 8 hours to obtain a crude asphalt product;

[0052] S3. Product refinement: Naturally cool the crude asphalt product for 1 hour, add quinoline to the crude asphalt, with the mass ratio of quinoline to the crude asphalt product being 2:1, conduct extraction 3 times, and obtain coated asphalt after drying;

[0053] S4. Performance detection: Take an appropriate amount of the prepared coated asphalt to make a sample, add the coated asphalt to detector 1, and detect its flow characteristics, viscosity, penetration, and softening point through the boosting detection mechanism 200 and the partition expansion mechanism 300, and use the corresponding equipment to complete the determination of the quinoline insoluble content, coking value, and yield.

[0054] As Figures 2 - 9 shown, on one side of the top of detector 1, a boosting detection mechanism 200 is installed. The boosting detection mechanism 200 includes a cylinder body 201, a heat-conducting cylinder 202, a round box 203, a guide seat 204, a pressure-resistant pipe 205, a notch 206, a turbine 207, a shaft seat 208, a pin shaft 209, a torque sensor 210, a shaft cylinder 211, a rod body 212, a temperature sensor 213, a heating rod 214, a coil 215, a ring shell 216, an insertion pipe 217, a sliding cavity 218, a round plug 219, an exhaust port 220, a gas guide valve 221, and a pressure sensor 222;

[0055] On one side of the top end of the detector 1, a cylinder body 201 is installed. Inside the cylinder body 201, a heat-conducting cylinder 202 is installed. At the bottom of the heat-conducting cylinder 202, a round box 203 is installed. At the edge of the top end of the heat-conducting cylinder 202, a guide seat 204 is embedded. On both sides of the outer curved surface of the guide seat 204, pressure-resistant tubes 205 are symmetrically installed. The pressure-resistant tubes 205 are spiral-shaped. At the position corresponding to the pressure-resistant tubes 205 on the side wall of the cylinder body 201, an inner clamping cavity 2051 is opened. And the guide seat 204 is connected to the round box 203 through the pressure-resistant tubes 205 to convert and utilize the driving force. At the edge of the bottom end of the round box 203, a notch 206 is opened. Inside the round box 203, a turbine 207 is rotatably installed;

[0056] At the end of the turbine 207, a shaft seat 208 is installed. At the top of the shaft seat 208, a pin shaft 209 is slidably clamped. At the top of the pin shaft 209, a torque sensor 210 is installed. At the end of the torque sensor 210, a shaft cylinder 211 is installed. On both sides of the outer curved surface of the shaft cylinder 211, a number of rod bodies 212 are evenly installed at equal intervals. In the middle of the outer curved surface of the shaft cylinder 211, a temperature sensor 213 is embedded. Along the circumferential direction at equal angles on the outer side of the heat-conducting cylinder 202, a number of heating rods 214 are installed. Between the inner wall of the cylinder body 201 and the outer wall of the heat-conducting cylinder 202, a water bath cavity 2021 is formed. The heating rods 214 are located inside the water bath cavity 2021. The water replenishing valve 12 is communicated with the water bath cavity 2021. The bottom of the guide seat 204 is directly communicated with the water bath cavity 2021 to provide the temperature conditions required for detection. On the outer curved surface of the cylinder body 201, a coil 215 is wound;

[0057] At the bottom of the outer curved surface of the heat-conducting cylinder 202, a discharge valve 11 is installed. On the top of the outer curved surface of the cylinder body 201, a water replenishing valve 12 is embedded. At the top end of the cylinder body 201, a top cover 13 is installed;

[0058] At the bottom end of the round box 203, a ring shell 216 is installed. On one side of the outer curved surface of the ring shell 216, an insertion tube 217 is installed. At the position corresponding to the end of the insertion tube 217 inside the detector 1, a sliding cavity 218 is opened. Inside the sliding cavity 218, a round plug 219 is slidably installed. On the other side of the outer curved surface of the sliding cavity 218 corresponding to the round plug 219, an exhaust port 220 is opened. On the outer curved surface of the sliding cavity 218 at the position above the round plug 219, a gas guide valve 221 is embedded;

[0059] In the middle of the top end of the sliding cavity 218, a pressure sensor 222 is embedded. The ring shell 216 is communicated with the round box 203 through the notch 206. The thickness of the round plug 219 is greater than the diameter of the exhaust port 220. Inside the sliding cavity 218, air is filled at the position above the round plug 219. The output ends of the torque sensor 210, the temperature sensor 213 and the pressure sensor 222 are all connected to the input end of the detector 1. The input end of the detector 1 is electrically connected to the output end of the external power supply through the coil 215 to limit the heating temperature and perform the flow characteristic detection;

[0060] A partition outward expansion mechanism 300 is installed outside the shaft cylinder 211. The partition outward expansion mechanism 300 includes a transmission seat 301, a top seat 302, an impeller 303, a rotating rod 304, an air inlet 305, a gas guide column 306, a connecting pipe 307, a detection needle 308, a piston plate 309, a displacement sensor 310, a vertical cavity 311, a circular block 312, an air outlet 313, a gas nozzle 314, a pressure sensor 315, a partition plate 316, a clamping rod 317, a rod sleeve 318, a paddle 319, a side hole 320 and a bottom hole 321;

[0061] A transmission seat 301 is installed at the top end of the top cover 13. A top seat 302 is installed at the top end of the transmission seat 301. Electric push rods 14 are installed at positions on both sides of the top seat 302 corresponding to the top of the detector 1. An impeller 303 is rotatably installed inside the top seat 302. A rotating rod 304 is rotatably embedded at the bottom end of the top cover 13. An air inlet 305 is opened in the middle of the top of the top seat 302. A gas guide column 306 is installed on one side of the outer surface of the top seat 302. A connecting pipe 307 is installed at the top of the outer surface of the transmission seat 301;

[0062] A number of detection needles 308 are slidably embedded and installed at equal angles along the circumferential direction at the bottom end of the transmission seat 301. A piston plate 309 is installed at the top end of the detection needle 308. A displacement sensor 310 is embedded and installed in the middle of the top end of the piston plate 309. A vertical cavity 311 is opened inside the transmission seat 301 corresponding to the position of the piston plate 309. A circular block 312 is slidably installed inside the gas guide column 306. An air outlet 313 is opened at the top of the outer surface of the gas guide column 306 corresponding to the position of the circular block 312. A pressure sensor 315 is embedded and installed at the end of the gas guide column 306. A gas nozzle 314 is embedded and installed at a position near the pressure sensor 315 on the top of the outer surface of the gas guide column 306. Air is filled inside the gas guide column 306 corresponding to the position of the gas nozzle 314. The thickness of the circular block 312 is greater than the diameter of the air outlet 313. The force-bearing area of the circular block 312 is the same as the force-bearing area of the piston plate 309. The output ends of the displacement sensor 310 and the pressure sensor 315 are both connected to the input end of the detector 1. The input end of the electric push rod 14 is electrically connected to the output end of an external power supply to perform penetration testing;

[0063] An isolation plate 316 is rotatably installed at the top of the outer surface of the torque sensor 210. A softening point detection bracket assembly 15 is installed at the bottom end of the isolation plate 316. At the bottom end of the softening point detection bracket assembly 15, clamping rods 317 are symmetrically installed. At the positions corresponding to the clamping rods 317 at the bottom end of the heat conduction cylinder 202, rod sleeves 318 are installed. At the position on the outer surface of the shaft seat 208 between the heat conduction cylinder 202 and the round box 203, a paddle 319 is installed. A plurality of side holes 320 are equiangularly arranged along the circumferential direction in the middle of the outer surface of the heat conduction cylinder 202. A bottom hole 321 is opened in the middle of the bottom end of the heat conduction cylinder 202. The impeller 303 is connected to the shaft cylinder 211 through a rotating rod 304, and both the transmission seat 301 and the top seat 302 are rotatably connected to the rotating rod 304. The clamping rod 317 is slidably connected to the rod sleeve 318. The inner diameter of the bottom hole 321 is larger than the outer diameter of the shaft seat 208 to conduct power transmission and promote temperature stability during the detection process.

[0064] Application of the coated pitch prepared by the preparation method of high softening point coated pitch with ultra-low quinoline insoluble content in coating the negative electrode material of lithium ion battery.

[0065] The working principle and usage process of the present invention: When using the present preparation method to prepare the coated pitch, first, the raw materials are pretreated. According to actual needs, vinyl tar and catalytic slurry are mixed at a mass ratio of 9:1. For the convenience of description below, the mixture of vinyl tar and catalytic slurry is called the mixed raw material. At room temperature, the mixed raw material is physically stirred and mixed at a rotation speed of 220 rpm for 10 hours.

[0066] Subsequently, according to the actual situation, an AS204 slurry settling agent is added to the mixed raw material of vinyl tar and catalytic slurry. The mass ratio of the settling agent to the mixed raw material is 1:5, and the settling is carried out for 36 hours. Subsequently, at a temperature of 120 °C, the settled mixture is heated for 1 hour to obtain a pretreatment product. Then, the pretreatment product is put into a high-temperature and high-pressure reaction kettle for multi-stage heating reaction.

[0067] Then, a mixed gas of oxygen and nitrogen with an oxygen content of 8% is introduced at a ventilation rate of 1000 sccm. According to the actual preparation situation, vinyltriethoxysilane is added. The dosage of vinyltriethoxysilane is 1 / 60 of the total mass of the mixed raw material, and an oxidative cross-linking catalytic reaction is carried out at a temperature of 280 °C for 4 hours.

[0068] When changing from the oxidative cross-linking catalytic reaction stage to the polycondensation catalytic reaction, nitrogen is introduced at a ventilation rate of 2000 sccm. According to the actual preparation situation, random poly-α-olefin and ferric trichloride are added. The dosage is 1 / 30 of the total mass of the mixed raw material, and the temperature is raised at a rate of 5 °C / min. At a temperature of 340 °C, a polycondensation catalytic reaction is carried out for 8 hours to obtain a crude asphalt product.

[0069] Next, the crude asphalt product is naturally cooled for 1 hour. Subsequently, quinoline is added to the crude asphalt, and the mass ratio of quinoline to the crude asphalt product is 2:1. Extraction is carried out 3 times, and the coated asphalt is obtained after drying.

[0070] Subsequently, using a detection device, the prepared coated asphalt is detected. The exhaust port 220 is connected to an external exhaust pipe, and the air guide valve 221 is connected to an external gas transmission device. The air pressure sensor 222 will real-time feedback the air pressure at the top of the round plug 219 to the detector 1. According to actual needs, based on the correspondence between the boiling point of water and air pressure, the air pressure at the top of the round plug 219 can be preliminarily regulated to initially control the water bath temperature during the water bath heating process.

[0071] Next, the electric push rod 14 is started to drive the top seat 302 to rise, forcing the top cover 13 to rise synchronously under its drive, so that it disengages from the cylinder body 201. An appropriate amount of coated asphalt sample is taken and added to the heat conduction cylinder 202. Under the interception of the isolation plate 316, the coated asphalt sample will stay above the isolation plate 316. Subsequently, the electric push rod 14 is driven to reset, so that the top cover 13 seals the heat conduction cylinder 202 again. The water replenishing valve 12 is connected to an external water supply pipe, and an appropriate amount of clean water is injected into the water bath cavity 2021 through the water replenishing valve 12. Subsequently, the detector 1 can be started, the coil 215 is energized, and the detection work begins.

[0072] After the coil 215 is energized, a magnetic field is formed inside it, forcing the heating rod 214 to heat up under the action of electromagnetic induction, heating the clean water inside the water bath cavity 2021, causing the clean water to heat up accordingly, and heating the coated asphalt sample inside the heat conduction cylinder 202 to provide the temperature required for detection.

[0073] During this process, as the water temperature rises, water vapor will be produced correspondingly, causing the air pressure inside the water bath cavity 2021 to increase. The water vapor will also enter the guide seat 204 under the action of air pressure, and then enter the round box 203 through the pressure-resistant pipe 205, forcing the turbine 207 to rotate accordingly under its pressure. Subsequently, it will pass through the notch 206 into the ring shell 216 and enter the sliding cavity 218 through the insertion pipe 217, forcing the air pressure received at the bottom of the round plug 219 to rise and fall synchronously with the air pressure inside the water bath cavity 2021.

[0074] When the pressing force exerted on the round plug 219 is sufficient to overcome the air pressure on the top of the round plug 219, the round plug 219 will rise accordingly under its oppression, causing the exhaust port 220 to communicate with the sliding cavity 218. The water vapor will pass through the exhaust port 220 and be discharged into the external exhaust pipe. When the pressing force exerted by the water vapor on the round plug 219 is sufficient to overcome the air pressure on the top of the round plug 219, the round plug 219 will block the exhaust port 220 under the action of the top air pressure, automatically dynamically regulating the water vapor pressure, so that the air pressure received at the bottom of the round plug 219 is balanced with the air pressure received at the top of the round plug 219, that is, the air pressure inside the water bath cavity 2021 is balanced with the air pressure received at the top of the round plug 219;

[0075] Furthermore, during the detection process of the coated asphalt, by using an external gas transmission device and charging and discharging the air inside the sliding cavity 218 through the air guide valve 221, the air pressure received at the top of the round plug 219 can be controlled. Furthermore, according to the correspondence between the boiling point of water and the air pressure, the air pressure inside the water bath cavity 2021 can be synchronously and dynamically regulated, and the boiling point temperature of the clean water inside the water bath cavity 2021 can be controlled to achieve synchronous adjustment of the water bath heating temperature;

[0076] By the above method, while improving the controllability of the water bath heating temperature and expanding its temperature coverage range, further, according to the correspondence between the boiling point of water and the air pressure, by controlling the rising speed of the air pressure inside the water bath cavity 2021, the rising rate of the water bath heating temperature can be limited to provide suitable temperature conditions for the detection process of the coated asphalt;

[0077] During the detection process of the coated asphalt, as the turbine 207 rotates, it will drive the pin shaft 209 to rotate synchronously through the shaft seat 208. Further, it will force the torque sensor 210 to drive the shaft cylinder 211 to rotate synchronously under the drive of the pin shaft 209. During this process, each rod body 212 will also rotate accordingly, stirring the coated asphalt sample inside the heat conduction cylinder 202. Correspondingly, the coated asphalt sample inside the heat conduction cylinder 202 will give a reverse resistance to the rod body 212;

[0078] Under the drive of the shaft cylinder 211, the resistance will act on the torque sensor 210. Further, the torque sensor 210 will feedback the force information during the stirring process to the detector 1. After being processed by the detector 1, the viscosity and fluidity information of the coated asphalt will be generated. During this process, the temperature sensor 213 will feedback the temperature of the coated asphalt after heating to the detector 1 in real time. According to the real-time temperature feedback by the temperature sensor 213, the water bath heating temperature can be further regulated. Further, the viscosity and fluidity of the coated asphalt under different temperature conditions can be detected in real time, and the performance of the coated asphalt can be preliminarily evaluated;

[0079] Meanwhile, driven by the rotating rod 304, the impeller 303 will rotate accordingly. Under the traction of the impeller 303, external air will enter the top seat 302 through the air suction port 305, and then flow into the air guide column 306, enter the transmission seat 301 through the connecting pipe 307, causing the air pressure inside the transmission seat 301 to rise, and applying pressure to each piston plate 309, forcing the piston plate 309 to push the detection needle 308 downward under the action of the pressure, causing the detection needle 308 to insert into the asphalt sample at the bottom. The displacement sensor 310 will feedback the downward depth of the piston plate 309, that is, the insertion depth of the detection needle 308, to the detector 1. After being processed by the detector 1, the penetration information of the coated asphalt will be generated, and the performance of the coated asphalt will be evaluated synchronously from another aspect;

[0080] During this process, the air pressure inside the air guide column 306 can be regulated through the air nozzle 314 to control the air pressure received by the end face of the circular block 312 close to the pressure sensor 315. Here, this air pressure is used as the standard air pressure, and during the detection process, the air flow conveyed by the impeller 303 will press the other end face of the circular block 312;

[0081] When the air flow pressure conveyed by the impeller 303 is sufficient to overcome the standard air pressure, the circular block 312 will slide correspondingly under its push, making the air discharge port 313 conductive, and the air flow conveyed by the impeller 303 will be discharged through the air discharge port 313. Furthermore, by regulating the standard air pressure, the air flow pressure conveyed by the impeller 303 can be limited. Further, under the conduction of the connecting pipe 307, the air pressure inside the transmission seat 301 can be limited, realizing the synchronous regulation of the pressure received by the top of the piston plate 309. Furthermore, combined with the temperature regulation effect, the penetration detection of the coated asphalt under different temperature and pressure conditions can be realized;

[0082] Similarly, during the detection process, before adding the coated asphalt sample into the heat-conducting cylinder 202, a part of the coated asphalt sample can be taken again, heated to a flowing state, injected into the external metal ring until it is slightly higher than the ring surface, and the surface is scraped flat after cooling to ensure no bubbles or cracks, thus making a specimen ring. The specimen ring is horizontally placed on the softening point detection support assembly 15, and the external steel ball is placed on the top of the specimen ring. After adding clean water, the specimen ring at the bottom of the isolation plate 316 will be immersed in the clean water;

[0083] Under the limiting effect of the clamping rod 317 and the rod sleeve 318, the softening point detection bracket assembly 15 will not rotate with the torque sensor 210, which can provide suitable conditions for the detection of the softening point of the coated asphalt. During the detection process, the synchronous detection of the softening point of the coated asphalt can be achieved. Driven by the shaft seat 208, coupled with the guiding effect of the side hole 320 and the bottom hole 321, the paddle 319 will rotate accordingly to agitate and divert the clean water, promoting the dynamic flow of the clean water and keeping the water temperature balanced and stable everywhere, further improving the external temperature stability of the softening point detection, fluidity detection, and penetration detection of the coated asphalt, and enhancing the detection effect.

[0084] After completing the above detection work, external detection equipment can be continued to be used to complete the detection of the quinoline insoluble content, coking value, and yield of the coated asphalt. Among them, the determination of the asphalt softening point is based on GB / T 4507-2014, the determination of the coking value is based on GB / T 8727-2008, and the determination of the quinoline insoluble is based on GB / T 2293-2019.

[0085] After ensuring that the performance of the prepared coated asphalt meets the standards, according to the actual situation, the prepared coated asphalt is mixed with the negative electrode material and subjected to high-temperature carbonization under a nitrogen atmosphere to obtain the coated negative electrode material.

[0086] Finally, it should be noted that the above are only preferred examples of the present invention and are not used to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, for those skilled in the art, they can still modify the technical solutions recorded in the foregoing embodiments, or perform equivalent replacements for some of the technical features. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims

1. A method for preparing a high softening point coated asphalt with ultra-low quinoline insoluble content, characterized in that: The steps include: S1. Pretreatment: Ethylene tar and catalytic slurry are mixed in a mass ratio of 8 to 9:1, stirred at a speed of 150 to 300 rpm for 8 to 12 hours at room temperature, AS204 slurry settler is added, the mass ratio of the settler to the total amount of ethylene tar and catalytic slurry is 1:3 to 6, and the mixture is settled for 24 to 48 hours, and the settled mixture is heated at 115° C. to 130° C. for 0.5 to 1 hour to obtain a pretreated product, and the pretreated product is placed in a high temperature and high pressure reactor for multi-stage heating reaction; S2, catalytic reaction: introducing a mixed gas of oxygen and nitrogen with an oxygen content of 5-10% at a ventilation rate of 800-1200 sccm, adding vinyl triethoxysilane or diisopropylbenzene peroxide in an amount of 1 / 30-1 / 100 of the total mass of the raw materials, and carrying out an oxidative cross-linking catalytic reaction at a temperature of 250-320°C for 3-5 hours, introducing nitrogen at a ventilation rate of 1500-3000 sccm, and introducing random poly-alpha olefin, ferric chloride or phosphoric acid in an amount of 1 / 20-1 / 50 of the total mass of the raw materials, and carrying out a condensation catalytic reaction at a temperature of 320-360°C for 6-10 hours to obtain a crude asphalt product; S3, product refining: the crude asphalt product is naturally cooled for 0.5 to 1 hour, quinoline or washing oil is added to the crude asphalt, the mass ratio of quinoline or washing oil to the crude asphalt product is 1 to 3:1, extraction is performed 2 to 4 times, and coated asphalt is obtained after drying; S4. Performance testing: Take an appropriate amount of prepared coated asphalt to make a sample, add the coated asphalt into the detector (1), and test its flow characteristics, viscosity, needle penetration and softening point through the auxiliary detection mechanism (200) and the partition extension mechanism (300), and use the corresponding equipment to complete the determination of quinoline insoluble content, coking value and yield.

2. An application of a high softening point coated asphalt with ultra-low quinoline insoluble content, characterized in that: The coated asphalt prepared by the method for preparing a high softening point coated asphalt with ultra-low quinoline insoluble content according to claim 1 is used for but not limited to lithium batteries.

3. The method for preparing a high softening point coated asphalt with ultra-low quinoline insoluble content according to claim 1, characterized in that: A power-assisted detection mechanism (200) is installed on one side of the top end of the detector (1), and the power-assisted detection mechanism (200) comprises a cylinder (201); A cylinder (201) is installed on one side of the top of the detector (1), a heat-conducting cylinder (202) is installed inside the cylinder (201), a round box (203) is installed at the bottom of the heat-conducting cylinder (202), a guide seat (204) is embedded and installed at the top edge of the heat-conducting cylinder (202), pressure-resistant tubes (205) are symmetrically installed on both sides of the outer curved surface of the guide seat (204), a notch (206) is opened at the bottom edge of the round box (203), and a turbine (207) is rotatably installed inside the round box (203); The end of the turbine (207) is provided with a shaft seat (208), the top of the shaft seat (208) is slidably engaged with a pin shaft (209), the top of the pin shaft (209) is provided with a torque sensor (210), the end of the torque sensor (210) is provided with a shaft cylinder (211), a plurality of rod bodies (212) are evenly and equidistantly provided on both sides of the outer curved surface of the shaft cylinder (211), a temperature sensor (213) is embedded in the middle of the outer curved surface of the shaft cylinder (211), a plurality of heating rods (214) are provided at equal angles on the outer side of the heat-conducting cylinder (202) along the circumferential direction, and a coil (215) is wound around the outer curved surface of the cylinder (201); A discharge valve (11) is installed at the bottom of the outer curved surface of the heat-conducting cylinder (202), a water replenishment valve (12) is embedded and installed at the top of the outer curved surface of the cylinder body (201), and a top cover (13) is installed at the top end of the cylinder body (201).

4. The method for preparing a high softening point coated asphalt with ultra-low quinoline insoluble content according to claim 3, characterized in that: An annular shell (216) is installed at the bottom end of the circular box (203), and an insertion tube (217) is installed on one side of the outer curved surface of the annular shell (216). A sliding cavity (218) is provided inside the detector (1) at a position corresponding to the end of the insertion tube (217), and a round plug (219) is slidably installed inside the sliding cavity (218). An exhaust port (220) is provided at the other side of the outer curved surface of the sliding cavity (218) at a position corresponding to the round plug (219). An air guide valve (221) is embedded and installed on the outer curved surface of the sliding cavity (218) at a position at the top of the round plug (219), and an air pressure sensor (222) is embedded and installed in the middle of the top of the sliding cavity (218).

5. The method for preparing a high softening point coated asphalt with ultra-low quinoline insoluble content according to claim 3, characterized in that: The inner wall of the cylinder (201) and the outer wall of the heat-conducting cylinder (202) together form a water bath chamber (2021); the heating rod (214) is located inside the water bath chamber (2021); the water supply valve (12) is in communication with the water bath chamber (2021); and the bottom of the guide seat (204) is directly in communication with the water bath chamber (2021).

6. The method for preparing a high softening point coated asphalt with ultra-low quinoline insoluble content according to claim 3, characterized in that: The pressure-resistant tube (205) is spiral-shaped, an inner clamping cavity (2051) is provided on the side wall of the cylinder (201) at a position corresponding to the pressure-resistant tube (205), and the guide seat (204) is connected to the round box (203) through the pressure-resistant tube (205).

7. The method for preparing a high softening point coated asphalt with ultra-low quinoline insoluble content according to claim 4, characterized in that: The annular shell (216) is connected to the round box (203) through the notch (206); the thickness of the round plug (219) is greater than the diameter of the exhaust port (220); the interior of the sliding cavity (218) located at the top of the round plug (219) is filled with air; the output ends of the torque sensor (210), the temperature sensor (213) and the air pressure sensor (222) are all connected to the input end of the detector (1); and the input end of the detector (1) is connected to the output end of the external power supply through the coil (215).

8. The method for preparing a high softening point coated asphalt with ultra-low quinoline insoluble content according to claim 3, characterized in that: A partitioned extension mechanism (300) is installed on the outer side of the shaft cylinder (211), and the partitioned extension mechanism (300) includes a transmission seat (301); A transmission seat (301) is installed at the top of the top cover (13), a top seat (302) is installed at the top of the transmission seat (301), electric push rods (14) are installed at the positions on both sides of the top seat (302) corresponding to the top of the detector (1), an impeller (303) is rotatably installed inside the top seat (302), a rotating rod (304) is embedded in the bottom end of the top cover (13) and rotatably installed, an air intake (305) is opened in the middle of the top of the top seat (302), an air guide column (306) is installed on one side of the outer curved surface of the top seat (302), and a connecting pipe (307) is installed at the top of the outer curved surface of the transmission seat (301); A plurality of detection needles (308) are slidably mounted at equal angles along the circumferential direction in the bottom end of the transmission seat (301); a piston plate (309) is mounted on the top end of the detection needle (308); a displacement sensor (310) is embedded in the middle of the top end of the piston plate (309); a vertical cavity (311) is provided inside the transmission seat (301) at a position corresponding to the piston plate (309); a circular block (312) is slidably mounted inside the air guide column (306); an exhaust port (313) is provided at a position corresponding to the circular block (312) on the top of the outer curved surface of the air guide column (306); a pressure sensor (315) is embedded at the end of the air guide column (306); and a gas nozzle (314) is embedded at a position close to the pressure sensor (315) on the top of the outer curved surface of the air guide column (306); An isolation plate (316) is rotatably mounted on the top of the outer curved surface of the torque sensor (210), a softening point detection bracket assembly (15) is mounted on the bottom end of the isolation plate (316), a clamping rod (317) is symmetrically mounted on the bottom end of the softening point detection bracket assembly (15), a rod sleeve (318) is mounted at a position corresponding to the clamping rod (317) at the bottom end of the heat-conducting tube (202), a paddle (319) is mounted on the outer curved surface of the shaft seat (208) at a position between the heat-conducting tube (202) and the round box (203), a plurality of side holes (320) are opened at equal angles in the middle of the outer curved surface of the heat-conducting tube (202) along the circumferential direction, and a bottom hole (321) is opened in the middle of the bottom end of the heat-conducting tube (202).

9. The method for preparing a high softening point coated asphalt with ultra-low quinoline insoluble content according to claim 8, characterized in that: The interior of the air guide column (306) is filled with air at a position corresponding to the air nozzle (314); the thickness of the circular block (312) is greater than the diameter of the exhaust port (313); the force bearing area of ​​the circular block (312) is the same as the force bearing area of ​​the piston plate (309); the output ends of the displacement sensor (310) and the pressure sensor (315) are both connected to the input end of the detector (1); and the input end of the electric push rod (14) is electrically connected to the output end of an external power supply.

10. The method for preparing a high softening point coated asphalt with ultra-low quinoline insoluble content according to claim 8, characterized in that: The impeller (303) is connected to the shaft cylinder (211) via a rotating rod (304), and the transmission seat (301) and the top seat (302) are both rotatably connected to the rotating rod (304), the clamping rod (317) is slidably connected to the rod sleeve (318), and the inner diameter of the bottom hole (321) is larger than the outer diameter of the shaft seat (208).

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