An apparatus and method for preparing high-performance carbon materials

Abstract

This invention relates to the field of needle coke preparation technology, specifically to an apparatus and method for preparing high-performance carbon materials. The gas buffer assembly includes a buffer tank and a counterweight rod. The inner cavity of the buffer tank is connected to the inner cavity of a heating furnace. A T-shaped counterweight rod is vertically installed at the upper end of the buffer tank, and a piston block that is sealed and slidably installed on the inner wall of the buffer tank is installed at the lower end of the counterweight rod. The advantages are: by using a U-shaped measuring tube to replace the traditional drainage method for gas quantity detection, and by using the cooperation of through holes and solenoid valves, excess gas at the corresponding temperature is discharged during switching to achieve equilibrium with the atmosphere, thereby reducing experimental errors and avoiding repeated equipment testing and adjustment. The horizontal insertion of the insert allows for position switching, facilitating comparison of gas production without the need for extensive weighing and calculation, greatly improving the convenience of the experiment.

Description

Technical Field

[0001] This invention relates to the field of needle coke preparation technology, specifically to an apparatus and method for preparing high-performance carbon materials. Background Technology

[0002] Needle coke, due to its advantages such as low sulfur content, low ash content, low metal content, and easy graphitization, is currently the main material used in ultra-high power graphite electrodes and lithium-ion battery anode materials, and has a key impact on its application performance.

[0003] The existing reaction vessels for preparing needle coke are of the vessel type, which is not conducive to coke removal. The coke remaining at the bottom of the vessel cannot be completely removed. Furthermore, the flow meter used for subsequent measurement is prone to clogging. In addition, the gas composition is high, and there is a large amount of inert gas, making it impossible to accurately measure changes in gas flow rate.

[0004] In actual production, it is necessary to determine the optimal preparation temperature through experiments to improve the efficiency of gas preparation. However, the existing methods are mostly water displacement methods, which require weighing and calculation for comparison and repeated equipment adjustments. This is not conducive to eliminating gas variables in the experiment, resulting in low detection accuracy. Summary of the Invention

[0005] The purpose of this invention is to provide an apparatus and method for preparing high-performance carbon materials, so as to solve the problems mentioned in the background art.

[0006] To achieve the above objectives, the present invention provides the following technical solution:

[0007] An apparatus for preparing high-performance carbon materials, the apparatus comprising:

[0008] A heating furnace, wherein a detachable upper end cover and a lower base are respectively provided at the upper and lower ends of the heating furnace, and a motor-driven stirring device is provided inside the heating furnace;

[0009] A gas buffer assembly includes a buffer tank and a counterweight rod. The inner cavity of the buffer tank is connected to the inner cavity of the heating furnace. A T-shaped counterweight rod is vertically installed at the upper end of the buffer tank, and a piston block that is sealed and slidably installed on the inner wall of the buffer tank is installed at the lower end of the counterweight rod.

[0010] The measuring component includes multiple linearly distributed U-shaped measuring tubes filled with water. A float is vertically mounted on one end of the U-shaped measuring tube and suspended on the water surface. A scale rod is vertically mounted on the float. A connecting block for connecting to the regulating air intake component is mounted on the other end of the U-shaped measuring tube.

[0011] An adjustable intake assembly includes an adjusting frame and a strip. The adjusting frame has output interfaces corresponding to U-shaped measuring tubes. The strip is slidably inserted into the adjusting frame and contains an electromagnetic control valve. The input end of the electromagnetic control valve is connected to a buffer tank, and the output end of the battery control valve has a connecting port. The connecting port is connected to multiple sets of output interfaces through the sliding insertion of the strip.

[0012] Preferably, the upper end cover is provided with a feed inlet for adding raw materials, a vent for balancing internal and external pressure, and an air hole. The air hole is connected to the lower inner cavity of the buffer tank through a connecting pipe, and the upper end cover is provided with a motor-driven stirring blade.

[0013] Preferably, the lower base is sealed and installed at the lower end of the heating furnace, and an air inlet pipe is provided on the lower base. A gas flow meter is provided on the air inlet pipe, and a thermometer is provided on the lower base.

[0014] Preferably, the front end of the adjustment frame is provided with a slot, the insert is slidably inserted into the adjustment frame along the slot, the front end of the adjustment frame is provided with an extension frame, the front end of the insert is provided with a telescopic rod fixed on the extension frame, and the telescopic end of the telescopic rod is fixed to the front end of the insert.

[0015] Preferably, the front end of the extension frame is provided with a cross-shaped fixing rod, the middle of the cross-shaped fixing rod is provided with a through hole, one end of the telescopic rod is provided with a screw inserted into the through hole, and the end of the telescopic rod is fixed to the cross-shaped fixing rod by a bolt fastener that is threadedly rotated on the screw.

[0016] Preferably, the connecting port is configured as an inwardly recessed groove, and an elastically compressed rubber sealing ring is provided on the inner wall of the connecting port. The upper end of the insert is provided with a pair of long strip-shaped sealing strips located on both sides of the connecting port, and the sealing strips are slidably inserted into the slot.

[0017] Preferably, the side wall of the insert is provided with an exhaust port, which is connected to the electromagnetic control valve. The adjustment frame is provided with multiple sets of through holes corresponding to the exhaust port, and the multiple sets of through holes are located between adjacent connecting ports.

[0018] Preferably, the front end of the insert is provided with an air inlet pipe, which is connected to the lower inner cavity of the buffer tank.

[0019] Preferably, the U-shaped measuring tube is mounted on a fixed base, and the fixed base is provided with multiple sets of linearly distributed slots, on which the multiple sets of linearly distributed U-shaped measuring tubes are fixedly clamped and mounted.

[0020] A method for preparing high-performance carbon materials according to the above-described apparatus, the method comprising the following steps:

[0021] One or more of the following raw materials are used: catalytic cracking slurry, ethylene tar, vacuum residue, rubber asphalt, and coal tar pitch. The mass G0 is recorded. The raw materials are added to 50%-80% of the reactor volume. After the addition is completed, the stirring components are used to achieve full stirring. After completion, the stirring shaft is lifted and disassembled, and then reinstalled on the flange of the reactor. After the airtightness is checked and qualified, the heating is started.

[0022] The reaction temperature was rapidly increased to 460℃ and held at that temperature for 0.5-1 hour. The increase in the scale reading was recorded.

[0023] Switch the position of the insert and connect another set of U-shaped measuring tubes to rapidly raise the reaction temperature to 470℃, hold the temperature for 0.5-1h, and record the scale increment.

[0024] Switch again, rapidly raise the reaction temperature to 480℃, hold the temperature for 0.5-1 hour, and record the increase in the scale reading.

[0025] Switch again, rapidly raise the reaction temperature to 490℃, hold the temperature for 0.5-1 hour, and record the increase in the scale reading.

[0026] Switch again, rapidly raise the reaction temperature to 500℃, hold the temperature for 0.5-1 hour, and record the increase in the scale reading.

[0027] By comparing the height differences of multiple sets of scale rods, the amount of gas produced at the corresponding temperature can be determined.

[0028] Compared with the prior art, the beneficial effects of the present invention are:

[0029] This invention uses a U-shaped measuring tube to replace the traditional drainage method for gas quantity detection. Simultaneously, by utilizing the combination of a through-hole and a solenoid valve, excess gas at the corresponding temperature is discharged during switching, achieving atmospheric balance and reducing experimental errors. It avoids repeated equipment testing and adjustments. The lateral insertion of the insert allows for position switching, facilitating comparison of gas production without requiring extensive weighing and calculation, greatly improving experimental convenience. Attached Figure Description

[0030] Figure 1 This is a schematic diagram of the structure of the present invention;

[0031] Figure 2 for Figure 1 Enlarged view of the structure at point B in the middle;

[0032] Figure 3 This is a schematic diagram of the three-dimensional structure of the insert of the present invention;

[0033] Figure 4 This is a three-dimensional structural diagram of the connection between the insert and the adjustment frame of the present invention;

[0034] Figure 5 This is a three-dimensional structural diagram of the adjustment frame of the present invention.

[0035] In the diagram: 1. Heating furnace; 2. Upper cover; 3. Lower base; 4. Thermometer; 5. Gas flow meter; 6. Stirring blade; 7. Feed inlet; 8. Vent; 9. Motor; 10. Buffer tank; 11. Connecting pipe; 12. Air vent; 13. Counterweight rod; 14. Adjusting frame; 15. Connecting block; 16. U-shaped measuring tube; 17. Float; 18. Fixed base; 19. Scale rod; 20. Slot; 21. Cross fixing rod; 22. Bolt fastener; 23. Telescopic rod; 24. Connecting port; 25. Sealing strip; 26. Exhaust port; 27. Air inlet pipe; 28. Output interface; 29. ​​Through hole; 30. Insert strip; 31. Slot; 32. Extension frame. Detailed Implementation

[0036] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0037] Please see Figures 1 to 5 The present invention provides a technical solution:

[0038] Example 1:

[0039] An apparatus for preparing high-performance carbon materials, comprising a heating furnace 1, a gas buffer assembly, a measuring assembly, and an regulating gas inlet assembly.

[0040] The upper and lower ends of the heating furnace 1 are respectively provided with a detachable upper cover 2 and a lower base 3. The heating furnace 1 is provided with a stirring device driven by a motor 9. The upper cover 2 is provided with a feed port 7 for adding raw materials, a vent port 8 for balancing internal and external pressure and an air hole 12. The air hole 12 is connected to the lower inner cavity of the buffer tank 10 through a connecting pipe 11. The upper cover 2 is provided with a stirring fan blade 6 driven by a motor 9.

[0041] By setting the stirring fan blades 6 driven by the motor 9, the raw materials for the experiment can be thoroughly mixed.

[0042] The gas buffer assembly includes a buffer tank 10 and a counterweight rod 13. The inner cavity of the buffer tank 10 is connected to the inner cavity of the heating furnace 1. A T-shaped counterweight rod 13 is vertically installed at the upper end of the buffer tank 10. A piston block that is sealed and slidably installed on the inner wall of the buffer tank 10 is installed at the lower end of the counterweight rod 13. The lower base 3 is sealed and installed at the lower end of the heating furnace 1. An air inlet pipe is installed on the lower base 3. A gas flow meter 5 is installed on the air inlet pipe. A thermometer 4 is installed on the lower base 3.

[0043] By setting a buffer tank 10 to reduce the gas temperature and setting a counterweight rod 13 to make the gas quickly and completely rush into the U-shaped measuring tube 16, it is easier to control the variables of gas transportation and make the gas transported under the same extrusion pressure.

[0044] The measuring component includes multiple linearly distributed U-shaped measuring tubes 16, each filled with water. One end of each U-shaped measuring tube 16 has a vertically suspended float 17 suspended on the water surface, and a scale rod 19 is vertically mounted on the float 17. The other end of the U-shaped measuring tube 16 has a connecting block 15 that connects to the air intake adjustment component.

[0045] The amount of gas generated is detected by setting a U-shaped measuring tube 16. The pressure difference on both sides causes different liquid levels, and the amount of gas is clearly reflected by the scale rod 19.

[0046] The intake adjustment assembly includes an adjustment frame 14 and a strip 30. The adjustment frame 14 is provided with output interfaces 28 corresponding to the U-shaped measuring tubes 16. The strip 30 is slidably inserted into the adjustment frame 14. An electromagnetic control valve is provided inside the strip 30. The input end of the electromagnetic control valve is connected to the buffer tank 10. The output end of the battery control valve is provided with a connecting port 24. The connecting port 24 is connected to multiple sets of output interfaces 28 through the sliding insertion of the strip 30.

[0047] By setting up the electromagnetic control valve in conjunction with the insert 30, the connection position can be switched through the sliding insertion of the insert 30, thereby facilitating the comparison of gas generation at different temperatures.

[0048] Example 2:

[0049] Based on embodiment 1, the front end of the adjustment frame 14 is provided with a slot 20, the insert 30 is slidably inserted into the adjustment frame 14 along the slot 20, the front end of the adjustment frame 14 is provided with an extension frame 32, the front end of the insert 30 is provided with a telescopic rod 23 fixed on the extension frame 32, and the telescopic end of the telescopic rod 23 is fixed to the front end of the insert 30.

[0050] By setting up the extension frame 32 and the telescopic rod 23 in coordination, the automatic control of the sliding insertion of the insertion rod 30 is achieved.

[0051] Example 3:

[0052] Based on embodiment 2, the front end of the extension frame 32 is provided with a cross fixing rod 21, the middle of the cross fixing rod 21 is provided with a through hole, one end of the telescopic rod 23 is provided with a screw inserted into the through hole, and the end of the telescopic rod 23 is fixed to the cross fixing rod 21 by a bolt fastener 22 that is screwed and rotated on the screw.

[0053] By using the cross-shaped fixing rod 21 and the bolt fastener 22, the telescopic rod 23 can be fixed in position.

[0054] The front end of the insert 30 is provided with an air inlet pipe 27, which is connected to the lower inner cavity of the buffer tank 10.

[0055] The gas transport pipeline is connected by setting up an air inlet pipe 27.

[0056] Example 4:

[0057] Based on embodiment 3, the connecting port 24 is configured as an inwardly recessed groove, and an elastically compressed rubber sealing ring is provided on the inner wall of the connecting port 24. A pair of long strip-shaped sealing strips 25 located on both sides of the connecting port 24 are provided at the upper end of the insert 30, and the sealing strips 25 are slidably inserted into the slot 20.

[0058] The sealing performance at the connection port 24 is improved by setting a rubber sealing ring, and the sealing performance between the insert 30 and the output interface 28 is further improved by setting a pair of symmetrical sealing strips 25 to prevent gas leakage.

[0059] Example 5:

[0060] Based on embodiment 4, an exhaust port 26 is provided on the side wall of the insert 30. The exhaust port 26 is connected to the electromagnetic control valve. The adjustment frame 14 is provided with multiple sets of through holes 29 corresponding to the exhaust port 26. The multiple sets of through holes 29 are located between adjacent connecting ports 24.

[0061] By setting the exhaust port 26 and the through hole 29 to cooperate, when the insert 30 slides to switch positions, the through hole 29 and the exhaust port 26 are connected. Thus, under the premise of sealing the gas generated at the previous experimental temperature, the excess gas in the buffer tank 10 and the heating furnace 1 is released, achieving internal and external pressure balance and avoiding the cumulative impact of gas generation when switching temperatures.

[0062] Example 6:

[0063] Based on embodiment 5, the U-shaped measuring tube 16 is mounted on the fixed base 18, and the fixed base 18 is provided with multiple sets of linearly distributed slots 31, and the multiple sets of linearly distributed U-shaped measuring tubes 16 are fixedly mounted on the slots 31.

[0064] Multiple sets of U-shaped measuring tubes 16 are fixedly installed by setting the fixing seat 18 and the slot 31.

[0065] A preparation method based on the above-described apparatus for preparing high-performance carbon materials includes the following steps:

[0066] One or more of the following raw materials are used: catalytic cracking slurry, ethylene tar, vacuum residue, rubber asphalt, and coal tar pitch. The mass G0 is recorded. The raw materials are added to 50%-80% of the reactor volume. After the addition is completed, the stirring components are used to achieve full stirring. After completion, the stirring shaft is lifted and disassembled, and then reinstalled on the flange of the reactor. After the airtightness is checked and qualified, the heating is started.

[0067] The reaction temperature was rapidly increased to 460℃ and held at that temperature for 0.5-1 hour. The readings were recorded as the scale rod was raised to 19.

[0068] Switch the position of insert 30 to connect another set of U-shaped measuring tubes 16, rapidly raise the reaction temperature to 470℃, keep the temperature constant for 0.5-1h, and record the scale rod 19 rising to the scale.

[0069] Switch again, rapidly raise the reaction temperature to 480℃, hold the temperature for 0.5-1 hour, and record the increase in scale on scale rod 19;

[0070] Switch again, rapidly raise the reaction temperature to 490℃, hold the temperature for 0.5-1 hour, and record the increase in scale on the scale rod 19.

[0071] Switch again, rapidly raise the reaction temperature to 500℃, hold the temperature for 0.5-1 hour, and record the increase in scale on scale rod 19.

[0072] By comparing the height differences of multiple sets of scale rods 19, the amount of gas generated at the corresponding temperature can be determined.

[0073] The reactor, with its flat-bottomed flange structure, is easy to disassemble and clean, and simple to operate. It also features a stirring mechanism at the start of the reaction test to prevent uneven mixing and sedimentation. The U-shaped measuring tube 16 collects the gas produced by the cracking of the raw materials and measures the amount of gas produced by the reaction through the scale rod 19, avoiding calculation and weighing. The comparison is more obvious and can determine the degree of reaction at different temperature stages, thereby determining the critical reaction temperature for each batch of raw materials.

[0074] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. An apparatus for preparing high-performance carbon materials, characterized in that: The apparatus for preparing high-performance carbon materials includes: A heating furnace (1) is provided with a detachable upper end cover (2) and a lower base (3) at its upper and lower ends respectively. A stirring device driven by a motor (9) is provided in the heating furnace (1). A gas buffer assembly, comprising a buffer tank (10) and a counterweight rod (13), wherein the inner cavity of the buffer tank (10) is connected to the inner cavity of the heating furnace (1), and a T-shaped counterweight rod (13) is vertically arranged at the upper end of the buffer tank (10), and a piston block that is sealed and slidably installed on the inner wall of the buffer tank (10) is arranged at the lower end of the counterweight rod (13). The measuring component includes multiple linearly distributed U-shaped measuring tubes (16), each U-shaped measuring tube (16) is filled with water, and a float (17) is vertically mounted on one end of the U-shaped measuring tube (16) and suspended on the water surface. A scale rod (19) is vertically mounted on the float (17), and a connecting block (15) for connecting to the regulating air intake component is mounted on the other end of the U-shaped measuring tube (16). The intake adjustment assembly includes an adjustment frame (14) and a strip (30). The adjustment frame (14) is provided with output interfaces (28) corresponding to U-shaped measuring tubes (16). The strip (30) is slidably inserted into the adjustment frame (14). An electromagnetic control valve is provided inside the strip (30). The input end of the electromagnetic control valve is connected to the buffer tank (10). The output end of the battery control valve is provided with a connection port (24). The connection port (24) is connected to multiple sets of output interfaces (28) through the sliding insertion of the strip (30).

2. The apparatus for preparing high-performance carbon materials according to claim 1, characterized in that: The upper end cover (2) is provided with a feed inlet (7) for adding raw materials, a vent (8) for balancing internal and external pressure and an air hole (12). The air hole (12) is connected to the lower end cavity of the buffer tank (10) through a connecting pipe (11). The upper end cover (2) is provided with a stirring fan blade (6) driven by a motor (9).

3. The apparatus for preparing high-performance carbon materials according to claim 1, characterized in that: The lower base (3) is sealed and installed at the lower end of the heating furnace (1). An air inlet pipe is provided on the lower base (3), a gas flow meter (5) is provided on the air inlet pipe, and a thermometer (4) is provided on the lower base (3).

4. The apparatus for preparing high-performance carbon materials according to claim 1, characterized in that: The front end of the adjustment frame (14) is provided with a slot (20), and the insert (30) slides into the adjustment frame (14) along the slot (20). The front end of the adjustment frame (14) is provided with an extension frame (32), and the front end of the insert (30) is provided with a telescopic rod (23) fixed on the extension frame (32). The telescopic end of the telescopic rod (23) is fixed to the front end of the insert (30).

5. The apparatus for preparing high-performance carbon materials according to claim 1, characterized in that: The front end of the extension frame (32) is provided with a cross fixing rod (21), the middle of the cross fixing rod (21) is provided with a through hole, one end of the telescopic rod (23) is provided with a screw inserted into the through hole, and the end of the telescopic rod (23) is fixed to the cross fixing rod (21) by a bolt fastener (22) installed on the screw through a threaded rotation.

6. The apparatus for preparing high-performance carbon materials according to claim 1, characterized in that: The connecting port (24) is configured as an inwardly recessed groove. An elastically compressed rubber sealing ring is provided on the inner wall of the connecting port (24). A pair of long strip-shaped sealing strips (25) located on both sides of the connecting port (24) are provided at the upper end of the insert (30). The sealing strips (25) are slidably inserted into the slot (20).

7. The apparatus for preparing high-performance carbon materials according to claim 1, characterized in that: The insert (30) has an exhaust port (26) on its side wall. The exhaust port (26) is connected to the electromagnetic control valve. The adjustment frame (14) has multiple sets of through holes (29) corresponding to the exhaust port (26). The multiple sets of through holes (29) are located between adjacent connecting ports (24).

8. The apparatus for preparing high-performance carbon materials according to claim 1, characterized in that: The front end of the insert (30) is provided with an air inlet pipe (27), which is connected to the lower end cavity of the buffer tank (10).

9. The apparatus for preparing high-performance carbon materials according to claim 1, characterized in that: The U-shaped measuring tube (16) is installed on the fixed base (18), and the fixed base (18) is provided with multiple sets of linearly distributed slots (31), and the multiple sets of linearly distributed U-shaped measuring tubes (16) are fixedly installed on the slots (31).

10. A method for preparing high-performance carbon materials using an apparatus according to any one of claims 1-9, characterized in that: The preparation method includes the following steps: One or more of the following raw materials are used: catalytic cracking slurry, ethylene tar, vacuum residue, rubber asphalt, and coal tar pitch. The mass G0 is recorded. The raw materials are added to 50%-80% of the volume of the reactor. After the addition is completed, the mixture is stirred thoroughly by a stirring device. The upper cover (2) of the heating furnace (1) is then reinstalled. After the airtightness is checked, the heating begins. The reaction temperature was rapidly increased to 460℃ and held at that temperature for 0.5-1h. The scale rod (19) was then raised to the next level. Switch the position of the insert (30), connect another set of U-shaped measuring tubes (16), rapidly raise the reaction temperature to 470℃, keep the temperature constant for 0.5-1h, and record the scale rod (19) to increase the scale. Switch again, rapidly raise the reaction temperature to 480℃, hold the temperature for 0.5-1h, and record the scale rod (19) as it increases in value; Switch again, rapidly raise the reaction temperature to 490℃, hold the temperature for 0.5-1h, and record the scale rod (19) as it increases in value; Switch again, rapidly raise the reaction temperature to 500℃, hold the temperature for 0.5-1h, and record the scale rod (19) as it increases in value; By comparing the height differences of multiple sets of scale rods (19), the amount of gas generated at the corresponding temperature can be determined.

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