CN110885081A - Graphite carbonization method based on high-temperature gasification impurity removal - Google Patents

Graphite carbonization method based on high-temperature gasification impurity removal Download PDF

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Publication number
CN110885081A
CN110885081A CN201811044791.2A CN201811044791A CN110885081A CN 110885081 A CN110885081 A CN 110885081A CN 201811044791 A CN201811044791 A CN 201811044791A CN 110885081 A CN110885081 A CN 110885081A
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China
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pipe
carbonization
graphite
furnace
discharging
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胡顺虎
胡鹏程
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Shimen Chujing New Materials Co Ltd
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Shimen Chujing New Materials Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/20Graphite
    • C01B32/21After-treatment
    • C01B32/215Purification; Recovery or purification of graphite formed in iron making, e.g. kish graphite
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

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Abstract

The invention discloses a graphite carbonization method based on high-temperature gasification impurity removal, which comprises the following steps: step 1: a feeding step; pushing graphite powder into the carbonization furnace by adopting a pushing mechanism based on hydraulic pressure or motor drive; step 2: a carbonization purification step; keeping the temperature in the carbonization furnace at 2500-3200 ℃, and carbonizing and purifying the graphite powder in the carbonization furnace in a protective atmosphere; metal impurities in the graphite powder are gasified at high temperature; step 3, discharging; and discharging the waste gas and the carbonized and purified graphite powder through a discharging device. The graphite carbonization method based on high-temperature gasification impurity removal has the advantages of high production efficiency, energy consumption saving and easiness in implementation.

Description

Graphite carbonization method based on high-temperature gasification impurity removal
Technical Field
The invention relates to a graphite carbonization method based on high-temperature gasification impurity removal.
Background
The conventional graphite carbonization is realized by feeding graphite powder into a carbonization furnace through manual feeding, specifically, the graphite powder is firstly loaded into a carbon boat, then the carbon boat loaded with the graphite powder is fed into a carbon tube of a furnace body for heating by using a push rod by an operator, and after a period of time, the carbon boat is fed into the next carbon boat loaded with the graphite powder. See patent publication No. CN201882914U for details, entitled: a graphite cathode material high-temperature graphitizing carbon tube furnace for the lithium ion battery; the disadvantages of this carbonization method are:
(1) the production efficiency is low, and the efficiency is low due to the manual propulsion of the carbon boat.
(2) The feeding mechanism occupies a large space, so that the whole carbonization system occupies a large area and has high requirements on environmental factors such as factory buildings.
(3) The limited carbon boat loading also results in low production efficiency and low productivity.
(4) Because the carbon boat and the graphite powder are heated together during heating, the carbon boat consumes a large amount of heat, the energy consumption is high, and the production cost is high.
And because the existence of the carbon boat, the temperature environment inside and outside the carbon boat has difference, leads to the graphite powder heating homogeneity of different positions in the carbon boat to be relatively poor, leads to the graphite quality of final product relatively poor. Furthermore, the carbon boats occupy a large space, resulting in a small amount per one feeding, and thus the yield is limited.
In addition, in the prior art, a high-temperature ion replacement process is adopted, chlorine (or freon) is flushed into a furnace, the chlorine and metal impurities in the graphite form metal compounds (such as chloride or fluoride) in a high-temperature environment, and then the metal compounds are gasified and discharged and can be discharged along with high-temperature gas, so that the purification of the graphite is realized. The working temperature is about 2000 ℃. This process is also known as: removing impurities by high-temperature ion replacement.
And chlorine or freon are harmful to the environment.
The prior art has low productivity, and the prior yield is 120-; large investment and high energy consumption.
Therefore, it is necessary to design a new graphite carbonization method based on high-temperature gasification impurity removal.
Disclosure of Invention
The invention aims to solve the technical problem of providing a graphite carbonization method based on high-temperature gasification impurity removal, and the graphite carbonization method based on high-temperature gasification impurity removal has high production efficiency.
The technical solution of the invention is as follows:
a graphite carbonization method based on high-temperature gasification impurity removal comprises the following steps:
step 1: a feeding step;
pushing graphite powder into the carbonization furnace by adopting a pushing mechanism based on hydraulic pressure or motor drive;
step 2: a carbonization purification step;
keeping the temperature in the carbonization furnace at 2500-3200 ℃, and carbonizing and purifying the graphite powder in the carbonization furnace in a protective atmosphere; metal impurities in the graphite powder are gasified at high temperature;
step 3, discharging;
and discharging the waste gas and the carbonized and purified graphite powder through a discharging device.
The steps 1-3 are continuously and circularly implemented, and continuous production is realized.
The material pushing mechanism is used for intermittently pushing the raw material into the carbonization furnace; the pushing mechanism comprises a plunger (5) and a driving mechanism for driving the plunger to reciprocate in the feeding pipe; the plunger is positioned in the feeding pipe; the feeding pipe is communicated with the inlet of a carbonization furnace in the graphite carbonization system, and a hopper communicated with the feeding pipe is arranged above the feeding pipe; the driving mechanism is a hydraulic driving mechanism; the hydraulic driving mechanism comprises a hydraulic oil cylinder (22), a hydraulic station (23) and a valve for controlling the on-off of a liquid path; the valve is controlled by the controller; the hydraulic station is connected with the hydraulic oil cylinder through a hydraulic oil pipe; the piston of the hydraulic oil cylinder is connected with the plunger piston through a push rod, and the controller is an MCU, preferably a PLC.
The MCU is connected with a human-computer interface device; the human interface device includes a display screen and keys or a touch pad for inputting parameters.
Generally, the material is pushed once every 5 to 15 minutes, and the material is set according to the purity of the raw material, and the higher the purity, the shorter the time can be.
The discharging device is provided with a discharging pipe and a impurity discharging pipe, and the discharging device is also provided with a water cooling device.
The discharging device (3) comprises a main pipe (35), a discharging pipe (31) and an impurity discharging pipe (32); the main pipe is horizontally arranged, one end of the main pipe is butted with a discharge hole of the carbonization furnace, and the other end of the main pipe is provided with an end cover (34);
the impurity discharging pipe and the discharging pipe are respectively arranged above and below the main pipe; the impurity discharging pipe and the discharging pipe are communicated with the main pipe;
an outer pipe (36) is sleeved outside the main pipe, and a closed cavity is formed between the outer pipe and the inner pipe; the outer pipe is provided with a water inlet pipe (37) and a water outlet pipe (38); the water inlet pipe and the water outlet pipe are both communicated with the closed cavity; the closed cavity is only provided with a water inlet pipe.
The water inlet pipe is arranged below the outer pipe, and the water outlet pipe is arranged above the outer pipe; when the carbonization furnace works, cooling water is input from the water inlet pipe to carry out water cooling on the discharging device. Preferably, the water outlet pipe and the water inlet pipe are both arranged along the radial direction of the outer pipe.
The main pipes of the carbonization furnace, the feeding pipe and the discharging device are all horizontally arranged.
The carbonization furnace adopts a carbon tube furnace, a heating component of the carbon tube furnace is a carbon tube, and the inner wall of the carbon tube is provided with a reinforcing layer. The reinforcing layer may be a tungsten layer, and the thickness of the reinforcing layer is 0.5 to 5mm, further, 1.9 to 2.1mm, preferably 2 mm.
The inlet pipe is provided with an inlet pipe which is communicated with the inlet pipe; protective gas enters the furnace body of the carbonization furnace from the gas inlet pipe; the protective gas is inert gas or nitrogen. The inert gas is preferably helium or argon.
The graphite carbonization system corresponding to the method comprises a carbonization furnace, a material pushing mechanism, a discharging device and a gas supply device; the material pushing mechanism is positioned at the rear end of the carbonization furnace, and the discharging device is positioned at the front end of the carbonization furnace;
the carbonization furnace is used for heating the graphite powder pushed into the furnace body under the protective atmosphere so as to carbonize and purify the graphite powder;
the material pushing mechanism is used for intermittently pushing the raw material into the carbonization furnace; the pushing mechanism comprises a plunger (5) and a driving mechanism for driving the plunger to reciprocate in the feeding pipe; the plunger is positioned in the feeding pipe; the feeding pipe is communicated with the inlet of a carbonization furnace in the graphite carbonization system, and a hopper communicated with the feeding pipe is arranged above the feeding pipe;
the discharging device is used for discharging the carbonized finished product and waste gas;
the gas supply device is used for filling protective gas into the inner cavity of the carbonization furnace. The protective gas is inert gas or nitrogen.
The material pushing mechanism, the carbonization furnace and the discharging device are sequentially and horizontally arranged.
The driving mechanism is a hydraulic driving mechanism; the hydraulic driving mechanism comprises a hydraulic oil cylinder (22), a hydraulic station (23) and a valve for controlling the on-off of a liquid path; the valve is controlled by the controller;
the hydraulic station is connected with the hydraulic oil cylinder through a hydraulic oil pipe; the piston of the hydraulic oil cylinder is connected with the plunger piston through a push rod.
The driving mechanism is based on a motor and a transmission mechanism; the driving mechanism comprises a motor (25) and a transmission mechanism; the motor drives the plunger to move through a transmission mechanism, and the transmission mechanism is a lead screw transmission mechanism or a connecting rod reciprocating transmission mechanism.
The plunger is of a hollow structure. And a displacement sensor is arranged on the plunger and connected with the MCU.
The discharging device (3) comprises a main pipe (35), a discharging pipe (31) and an impurity discharging pipe (32); the main pipe is horizontally arranged, one end of the main pipe is butted with a discharge hole of the carbonization furnace, and the other end of the main pipe is provided with an end cover (34); the impurity discharging pipe is used for discharging flue gas.
The impurity discharging pipe and the discharging pipe are respectively arranged above and below the main pipe; the impurity discharging pipe and the discharging pipe are communicated with the main pipe, and the aperture of the impurity discharging pipe is smaller than that of the discharging pipe. Preferably, the end cap is hinged to the end of the main tube to facilitate opening of the end cap to clear the dredging conduit.
An outer pipe (36) is sleeved outside the main pipe, and a closed cavity is formed between the outer pipe and the inner pipe; the outer pipe is provided with a water inlet pipe (38) and a water outlet pipe (37); the water inlet pipe and the water outlet pipe are both communicated with the closed cavity; the closed cavity is only provided with openings at the water inlet pipe and the water outlet pipe, and the rest parts are sealed. One part of the flange plate is used as part of the inner wall of the closed space, and the cooling device based on the water inlet pipe, the water outlet pipe and the closed cavity is used for cooling the flange.
The water inlet pipe is arranged below the outer pipe, and the water outlet pipe is arranged above the outer pipe; when the carbonization furnace works, cooling water is input from the water inlet pipe to carry out water cooling on the discharging device. Preferably, the water outlet pipe and the water inlet pipe are both arranged along the radial direction of the outer pipe.
The carbonization furnace is a carbon tube furnace, the heating component in the carbon tube furnace is a carbon tube, and the inner wall of the carbon tube is provided with a reinforcing layer. The reinforcing layer may be a tungsten layer, and the thickness of the reinforcing layer is 0.5 to 5mm, further, 1.9 to 2.1mm, preferably 2 mm.
The graphite powder is sent to the carbon tube to be heated.
The material pushing mechanism is controlled by the MCU; the MCU is a PLC.
The air inlet pipe of the air supply device is arranged on the feeding pipe and communicated with the feeding pipe; protective gas is filled into the furnace body of the carbonization furnace from the gas inlet pipe; the protective gas is inert gas or nitrogen. The inert gas is preferably helium or argon.
The gas supply device comprises a shielding gas inlet pipe (24) arranged on the carbon feed pipe, one end of the shielding gas inlet pipe is communicated with the feed pipe, and the other end of the shielding gas inlet pipe is connected with a gas source; the feeding pipe is butted with a feeding hole at the rear end of the carbonization furnace.
The graphite carbonization system also comprises a cooling module, wherein the cooling module comprises a water pipe, a valve and a water receiving tank; the water pipe is arranged above the carbonization furnace, and water sprayed from the water pipe flows into the water receiving tank through the outer wall of the carbonization furnace; an electrically controlled valve is arranged on the water pipe, and the opening degree of the valve is controlled by the MCU.
The MCU is connected with a touch display screen, or the MCU is connected with a display screen and a key. The MCU is also connected with a communication module. May be a wireless communication module for remote monitoring.
The MCU is PLC or DSP.
The carbonization furnace is provided with a temperature control module, and the temperature control module comprises an infrared temperature measurement unit for measuring the temperature in the carbonization furnace; the infrared temperature measuring unit comprises a main temperature measuring carbon tube (15) and a main infrared thermometer (16); the main temperature measuring carbon tube penetrates through a furnace wall (14) of the carbonization furnace and is inserted on the carbonization furnace along the radial direction of the carbonization furnace, and an axial carbon tube (11) is arranged in the carbonization furnace; the front end of the main temperature measurement carbon tube is abutted with the carbon tube, the outer end of the main temperature measurement carbon tube is positioned outside the furnace wall, the main infrared thermometer is arranged at the outer end of the main temperature measurement carbon tube, and the data output end of the main infrared thermometer is connected with the MCU;
the AC side of the rectifier is connected with an AC power supply, the AC side of the rectifier is connected with the DC side of the inverter, and the AC side of the inverter supplies power to the carbon tube; and the pulse output end of the MCU is connected with the control end of a power switch in the inverter.
And a displacement sensor is arranged on the plunger of the propeller and is connected with the MCU.
The propeller plunger is of a hollow structure.
The temperature control module comprises an infrared temperature measuring unit for measuring the temperature in the carbonization furnace; the infrared temperature measuring unit comprises a main temperature measuring carbon tube (15) and a main infrared thermometer (16); the main temperature measuring carbon tube penetrates through a furnace wall (14) of the carbonization furnace and is inserted on the carbonization furnace along the radial direction of the carbonization furnace, and an axial carbon tube (11) is arranged in the carbonization furnace; the front end of the main temperature measurement carbon tube is abutted with the carbon tube, the outer end of the main temperature measurement carbon tube is positioned outside the furnace wall, the main infrared thermometer is arranged at the outer end of the main temperature measurement carbon tube, and the data output end of the main infrared thermometer is connected with the MCU;
the AC side of the rectifier is connected with an AC power supply, the AC side of the rectifier is connected with the DC side of the inverter, and the AC side of the inverter supplies power to the carbon tube; and the pulse output end of the MCU is connected with the control end of a power switch in the inverter.
The motor is a stepping motor. The MCU is connected with a touch display screen, or the MCU is connected with a display screen and a key. The MCU is PLC or DSP.
The propeller plunger comprises a barrel column (41), a front end piece (42) and a connecting block (43); the cylinder column is a cylindrical part; the inner part of the cylinder is a cavity (48);
the front end piece is fixed at the front end of the cylinder column, the connecting block is fixed at the rear end of the cylinder column, and the connecting block is used for being connected with a piston rod of the hydraulic cylinder;
the front end piece is cylindrical, and the outer side wall of the front end piece is provided with at least one circumferential air ring groove (44);
the outer side wall of the rear end of the cylinder is provided with at least one circumferential gas ring groove (44). And a sealing ring is arranged in the gas ring groove.
A travel switch is arranged in the feeding pipe, a displacement sensor is arranged on the plunger, and the displacement sensor is connected with the MCU.
The connecting block is connected with the cylinder column through threads, or the connecting block is welded on the cylinder column.
The connecting block is a cylindrical component with steps, and the front end of the connecting block is inserted in the cavity of the cylinder. The annular step of the connecting block is used as a limiting component.
The rear end of the connecting block is provided with a circular depressed part (47) with internal threads. The piston rod is provided with an external thread which is matched with the internal thread, and the piston rod is connected with the concave part through a thread.
The front end of the cylinder is provided with a round front end plate (49); an axial through hole (46) is arranged at the center of the front end plate; the through hole is a threaded hole; the central part of the rear end of the front end piece is provided with a blind hole (45) along the axial direction; and the screw penetrates through the through hole and is screwed in the blind hole, so that the front end piece is connected with the cylinder column.
The front end piece is provided with 3 air ring grooves; the rear end of the cylinder is provided with 2 gas ring grooves. The rear end of connecting block is equipped with displacement sensor for detect the propulsive displacement volume of plunger, the plunger cartridge is equipped with proximity sensor in the inlet pipe, and proximity sensor is travel switch or photoelectric switch, and displacement sensor passes through amplifier circuit and links to each other with MCU, and proximity sensor links to each other with MCU.
The total length of the thruster plunger is 550-600mm, the outer diameter of the cylinder is 110-130mm, the length of the cylinder is 480-490mm, and the length of the connecting block is 40-45 mm; the length of the nose piece is 65-75 mm.
The total length of the propeller plunger is 570mm, the outer diameter of the cylinder is 120mm, the inner diameter of the cylinder is 101mm, the length of the cylinder is 485mm, and the length of the connecting block is 42 mm; the nose piece has a length of 70 mm.
The diameter of the front end piece is 120mm, and the depth of the blind hole is 35 mm;
the depth of the concave part of the connecting block is 18mm, the diameter of the front end of the connecting block is 103mm, and the step thickness is 15mm
Furthermore, the front end of the front end piece is provided with a heat-resistant layer, the heat-resistant layer is a tungsten layer, and the thickness of the heat-resistant layer is 1-5mm, and the thickness is contained in the total thickness of the front end piece.
The width of gas ring groove is 5mm, and the interval thickness of adjacent gas ring groove is 5mm, and the width of overhaul groove is 3 mm.
The diameters of the blind holes and the through holes are 16mm, and the blind holes and the through holes are both M16 threaded holes. The thickness of the front end plate is 12 mm.
The wall thickness of the cylinder was 9.5 mm.
The rear end of connecting block is equipped with displacement sensor for detect the propulsive displacement volume of plunger, and the plunger cartridge is equipped with proximity sensor in the inlet pipe, and proximity sensor is travel switch or photoelectric switch, and proximity sensor is triggered the back, and control motor or pneumatic cylinder make the plunger no longer act or move back, realizes process control. The proximity sensor is connected with the MCU; the displacement sensor is connected with an ADC port of the MCU through the amplifier. The MCU is also connected with a display screen, and the display screen is used for displaying real-time displacement and the like. The MCU controls the work of the hydraulic oil cylinder through the control device or controls the action of the plunger through the control motor.
The outer layer of the carbon tube is provided with a circle of reinforcing layer, specifically a tungsten layer, the thickness of the reinforcing layer is 6-15mm, and the reinforcing layer plays a role in reinforcing. The reinforcing layer of the inner wall can be eliminated, and only the reinforcing layer of the outer wall is arranged; or only the inner wall reinforcing layer is used, the outer wall is not provided with the reinforcing layer, or the inner wall and the outer wall are both provided with the reinforcing layer.
Has the advantages that:
the graphite carbonization method based on high-temperature gasification impurity removal adopts the unique automatic feeding module, and also comprises the temperature control module, the cooling module and the gas supply module to realize the carbonization of the graphite powder, thereby being capable of obviously improving the production efficiency.
Specifically, the invention has the following characteristics:
(1) adopt the automatic reciprocal circulation feeding module based on plunger and hydraulic pressure, can greatly improve feeding efficiency and compare with current feeding mode based on manual work and graphite boat, need not the manual work and push away the material, efficiency is showing and is improving. Practice shows that the yield can reach 350-.
(2) Energy consumption saving
Because this system has cancelled the carbon boat, then heating efficiency is higher, because the carbon boat not only has taken up heating space, has still absorbed very big heat, leads to the energy consumption to improve. By adopting the invention, the cost is saved by more than 60 percent after the carbon boat is cancelled.
(3) Small occupied space
The original feeding module occupies a large space, and because an operator can only feed the carbon boat into the furnace body by using a longer push rod, the production can be carried out in a larger field.
(4) Is environment-friendly and pollution-free
The prior art adopts chlorine or Freon, and waste gas also contains the gases, so that the environmental pollution is great, while the invention adopts inert gas (such as argon) or nitrogen as protective gas, so that the environment is not polluted, and the personal health of field workers is also facilitated.
(5) And the automatic control is adopted, so that unmanned production can be realized.
The feeding module adopts a motor or hydraulic material pushing, manual material pushing is not needed, the material pushing, heating and discharging are fully automated only by setting parameters by an operator, the operator only needs to monitor production on site and intervene when a fault occurs or the operator stops working, the labor intensity of the operator on site can be obviously reduced, and the automation degree is high.
(6) The system has low cost and economical efficiency.
The spiral feeding mechanism is made of heat-resistant tungsten metal, so that the cost is extremely high, one set of propelling mechanism is more than million RMB, and the spiral feeding mechanism is not suitable for popularization and use.
(7) High purity and high quality
Compared with replacement purification, the high-temperature gasification purification is adopted, and the purity of the product can be obviously improved. The molecular structure of the graphite powder is changed in a high-temperature environment, and the purity of the graphite powder is improved. And moreover, automatic air inlet is adopted, a one-way valve is arranged at the air inlet pipe, the air flow direction is guaranteed, and stable and orderly production is guaranteed. And because PLC control is adopted, automatic control and automatic production can be realized, the progress is controllable, the feeding is uniform and controllable, and the feeding time is controllable, so that the product consistency is good, and the stability is good.
In addition, the system adopts centralized control, can realize unmanned production and has high automation degree.
In addition, the plunger of the propeller consists of a barrel, a front end piece and a connecting block, and the propeller is compact in structure and easy to install.
In addition, the arrangement of the air ring groove improves the sealing performance of the whole plunger.
The barrel column is connected with the front end piece through the screw, and the connection is reliable.
The hydraulic rod is connected with the connecting block of the plunger through threads, and the connection is tight and reliable.
The plunger adopts a hollow structure, so that the weight is small, the propelling is flexible, and the energy consumption is small.
All the parts are reasonable in size design and can be coordinated and matched with the carbon tube furnace, so that the high yield of graphite carbonization is realized.
The invention is also provided with a displacement sensor, a proximity sensor and a display screen which are matched with the plunger, thereby being convenient for detection and control. The plunger of the propeller is compact in structure, tight in combination and easy to popularize and implement.
In conclusion, the system is a great improvement of the existing graphite carbonization method based on high-temperature gasification impurity removal, is particularly beneficial to improving the productivity, saving the energy consumption and reducing the production cost, and has remarkable economic and social benefits.
Drawings
Description of the drawings:
FIG. 1 is a schematic diagram of the overall structure of a control system;
FIG. 2 is a schematic diagram of the general structure of a graphite carbonization system based on a motor and a driving mechanism;
FIG. 3 is a schematic view of a plunger construction;
FIG. 4 is a block diagram of a detection system;
FIG. 5 is a schematic diagram of a signal amplification circuit;
FIG. 6 is a schematic diagram of a brightness adjusting circuit;
FIG. 7 is a schematic diagram of the general structure of a graphite carbonization system based on a hydraulic drive mechanism;
FIG. 8 is a schematic view of a temperature measuring mechanism;
FIG. 9 is a schematic view of a furnace tube structure;
FIG. 10 is a schematic view of a temperature module;
FIG. 11 is a schematic view of a gas supply module;
FIG. 12 is a schematic view of the structure of the discharging device.
Description of reference numerals: 1-a carbonization furnace, 2-a material pushing device, 3-a material discharging device and 4-a hopper; 5-pusher plunger;
11-carbon tube, 12-furnace inlet, 13-furnace outlet, 111-carbon tube body, 112-tungsten layer; 14-furnace wall, 15-main temperature measuring carbon tube, 16-main infrared thermometer, 17-standby carbon temperature measuring tube and 18-standby infrared thermometer.
21-a propeller, 22-a hydraulic oil cylinder and 23-a hydraulic station; 24-protective gas inlet pipe, 25-motor, 26-base, 27-screw rod, 28-inlet pipe; 31-a discharge pipe and 32-a impurity discharge pipe. 33-flange plate, 34-end cover, 35-main pipe, 36-outer pipe, 37-water inlet pipe and 38-water outlet pipe.
41-column, 42-front end piece, 43-connecting block, 44-gas ring groove, 45-blind hole, 46-through hole, 47-depressed part, 48-cavity, 49-front end plate and 40-maintenance groove.
Detailed Description
The invention will be described in further detail below with reference to the following figures and specific examples:
example 1:
referring to fig. 1,2 and 7, a graphite carbonization system comprises a carbonization furnace, a material pushing mechanism, a discharging device and a gas supply device; the material pushing mechanism is positioned at the rear end of the carbonization furnace, and the discharging device is positioned at the front end of the carbonization furnace;
the carbonization furnace is used for heating the graphite powder pushed into the furnace body under the protective atmosphere so as to carbonize and purify the graphite powder;
the material pushing mechanism is used for intermittently pushing the raw material into the carbonization furnace; the pushing mechanism comprises a plunger (5) and a driving mechanism for driving the plunger to reciprocate in the feeding pipe; the plunger is positioned in the feeding pipe; the feeding pipe is communicated with the inlet of a carbonization furnace in the graphite carbonization system, and a hopper communicated with the feeding pipe is arranged above the feeding pipe;
the discharging device is used for discharging the carbonized finished product and waste gas;
the gas supply device is used for filling protective gas into the inner cavity of the carbonization furnace. The protective gas is inert gas or nitrogen.
The material pushing mechanism, the carbonization furnace and the discharging device are sequentially and horizontally arranged.
The plunger is of a hollow structure. And a displacement sensor is arranged on the plunger and connected with the MCU.
The carbonization furnace is a carbon tube furnace, the heating component in the carbon tube furnace is a carbon tube, and the inner wall of the carbon tube is provided with a reinforcing layer. The reinforcing layer can be a tungsten layer or a carbon steel layer, and the thickness of the reinforcing layer is 0.5-5mm, further, the thickness is 1.9-2.1mm, and preferably 2 mm.
The graphite powder is sent to the carbon tube to be heated.
The material pushing mechanism is controlled by the MCU; the MCU is a PLC.
The air inlet pipe of the air supply device is arranged on the feeding pipe and communicated with the feeding pipe; protective gas is filled into the furnace body of the carbonization furnace from the gas inlet pipe; the protective gas is inert gas or nitrogen. The inert gas is preferably helium or argon.
A graphite carbonization method based on high-temperature gasification impurity removal comprises the following steps:
step 1: a feeding step;
pushing graphite powder into the carbonization furnace by adopting a pushing mechanism based on hydraulic pressure or motor drive;
step 2: a carbonization purification step;
keeping the temperature in the carbonization furnace at 2500-3200 ℃, and carbonizing and purifying the graphite powder in the carbonization furnace in a protective atmosphere; metal impurities in the graphite powder are gasified at high temperature;
step 3, discharging;
and discharging the waste gas and the carbonized and purified graphite powder through a discharging device.
The steps 1-3 are continuously and circularly implemented, and continuous production is realized.
The MCU is connected with a human-computer interface device; the human interface device includes a display screen and keys or a touch pad for inputting parameters.
Generally, the material is pushed once every 5 to 15 minutes, and the material is set according to the purity of the raw material, and the higher the purity, the shorter the time can be.
The discharging device is provided with a discharging pipe and a impurity discharging pipe, and the discharging device is also provided with a water cooling device.
The main pipes of the carbonization furnace, the feeding pipe and the discharging device are all horizontally arranged.
The carbonization furnace adopts a carbon tube furnace, a heating component of the carbon tube furnace is a carbon tube, and the inner wall of the carbon tube is provided with a reinforcing layer.
The inlet pipe is provided with an inlet pipe which is communicated with the inlet pipe; protective gas enters the furnace body of the carbonization furnace from the gas inlet pipe; the protective gas is inert gas or nitrogen. The inert gas is preferably helium or argon
Referring to fig. 1, a control module of a graphite carbonization system comprises a controller, a feeding module, a temperature control module and a gas supply module; the feeding module is used for intermittently pushing the raw materials into the carbonization furnace; the temperature control module is used for heating the carbon tube in the carbonization furnace and controlling the temperature in the carbonization furnace to be stable in a set range; the gas supply module is used for charging protective gas into the carbonization furnace; the feeding module, the temperature control module and the gas supply module are all controlled by a controller; the controller is an MCU. The control system also comprises a cooling module, wherein the cooling module comprises a water pipe, a valve and a water receiving tank; the water pipe is arranged above the carbonization furnace, and water sprayed from the water pipe flows into the water receiving tank through the outer wall of the carbonization furnace; an electrically controlled valve is arranged on the water pipe, and the opening degree of the valve is controlled by the MCU.
The following detailed description of each part:
description of the carbonization furnace:
as shown in fig. 2,7 and 9, the carbonization furnace comprises a furnace body and a carbon tube 11 transversely arranged in the furnace body; the front end of the furnace body is a furnace body inlet 12, the rear end of the furnace body is a furnace body outlet 13, and the carbon tube, the furnace body inlet and the furnace body outlet are coaxial;
the inner wall of the carbon tube is provided with a tungsten layer 112.
The thickness of the tungsten layer is preferably 2 mm.
The furnace body is cylindrical, and the inner diameter of the furnace body is 860 mm.
The outer diameter of the carbon tube is 175 mm; the inner diameter of the carbon tube was 125 mm.
A water cooling device is arranged outside the furnace body, and comprises a spray pipe arranged at the top of the furnace body and a water collecting container arranged at the bottom of the furnace body; the water spray pipe is used for spraying water to the outer wall of the furnace body; the water collecting container is used for collecting water which flows to the bottom of the furnace body along the outer wall of the furnace body.
The AC side of the rectifier is connected with an AC power supply, the AC side of the rectifier is connected with the DC side of the inverter, and the AC side of the inverter supplies power to the carbon tube; the pulse output end of the MCU is connected with the control end (such as the G pole of the IGBT) of the power switch in the inverter. The inverter outputs currents with different sizes to control the heating of the carbon tube, so that the temperature in the furnace is controlled, and the specific control process is the existing mature technology.
The MCU is also connected with a touch display screen.
II, performing secondary filtration; description of the feeding Module
(1) Hydraulic-based feeding module
The driving mechanism is a hydraulic driving mechanism; the hydraulic driving mechanism comprises a hydraulic oil cylinder 22, a hydraulic station 23 and a valve for controlling the on-off of a liquid path; the valve is controlled by the controller;
the hydraulic station is connected with the hydraulic oil cylinder through a hydraulic oil pipe; the piston of the hydraulic oil cylinder is connected with the plunger piston through a push rod.
A feeding module adopts a propeller; the propeller is controlled by the controller; the propeller comprises a propeller plunger 5 and a driving mechanism for driving the propeller plunger to reciprocate in the feeding pipe; the feeding pipe is horizontally arranged; the inlet pipe is communicated with the inlet of a carbonization furnace in the graphite carbonization system, and a hopper is arranged above the inlet pipe. The driving mechanism is a hydraulic driving mechanism. The hydraulic driving mechanism comprises a hydraulic oil cylinder 22, a hydraulic station 23 and a valve for controlling the on-off of a liquid path; the valve is controlled by the controller; the hydraulic station is connected with the hydraulic oil cylinder through a hydraulic oil pipe; the piston of the hydraulic oil cylinder is connected with the plunger of the propeller through a push rod. The control device is an MCU. The MCU is PLC or DSP.
The MCU is connected with a touch display screen.
(2) Feeding module based on motor and driving mechanism
The driving mechanism is based on a motor and a transmission mechanism; the driving mechanism comprises a motor (25) and a transmission mechanism; the motor drives the plunger to move through a transmission mechanism, and the transmission mechanism is a lead screw transmission mechanism or a connecting rod reciprocating transmission mechanism.
As shown in fig. 3 and 7, the graphite carbonization system includes a controller and an impeller;
the propeller is controlled by the controller; the propeller comprises a propeller plunger 5 and a driving mechanism for driving the propeller plunger to reciprocate in the feeding pipe; the feeding pipe is horizontally arranged; the inlet pipe is communicated with the inlet of a carbonization furnace in the graphite carbonization system, and a hopper is arranged above the inlet pipe. The driving mechanism is based on a motor and a transmission mechanism.
The driving mechanism comprises a motor 25 and a transmission mechanism; the transmission mechanism is a screw rod transmission mechanism, the motor drives the screw rod to rotate through a gear or a synchronous belt, and the screw rod drives the plunger of the propeller to reciprocate.
Or the transmission mechanism is a connecting rod reciprocating transmission mechanism. The output shaft of the motor is connected with the propeller plunger through the link mechanism, and the motor rotates to drive the propeller plunger to reciprocate.
The motor is a stepping motor.
The controller is an MCU; the MCU is PLC or DSP.
In addition, the propeller plunger is of a hollow structure.
The pusher plunger comprises a barrel 41, a nose piece 42 and a connecting block 43; the cylinder column is a cylindrical part; the interior of the cylinder is a cavity 48;
the front end piece is fixed at the front end of the cylinder column, the connecting block is fixed at the rear end of the cylinder column, and the connecting block is used for being connected with a piston rod of the hydraulic cylinder;
the front end piece is cylindrical, and the outer side wall of the front end piece is provided with at least one circumferential air ring groove 44;
at least one circumferential gas ring groove 44 is provided on the outer side wall of the rear end of the column. And a sealing ring is arranged in the gas ring groove.
A travel switch is arranged in the feeding pipe, a displacement sensor is arranged on the plunger, and the displacement sensor is connected with the MCU.
The connecting block is connected with the cylinder column through threads, or the connecting block is welded on the cylinder column.
The connecting block is a cylindrical component with steps, and the front end of the connecting block is inserted in the cavity of the cylinder. The annular step of the connecting block is used as a limiting component.
The rear end of the connecting block is provided with a circular depressed part 47 with internal threads. The piston rod is provided with an external thread which is matched with the internal thread, and the piston rod is connected with the concave part through a thread.
The front end of the cylinder is provided with a round front end plate 49; the center of the front end plate is provided with an axial through hole 46; the through hole is a threaded hole; the central part of the rear end of the front end piece is provided with a blind hole 45 along the axial direction; and the screw penetrates through the through hole and is screwed in the blind hole, so that the front end piece is connected with the cylinder column.
The front end piece is provided with 3 air ring grooves; the rear end of the cylinder is provided with 2 gas ring grooves.
The total length of the thruster plunger is 550-600mm, the outer diameter of the cylinder is 110-130mm, the length of the cylinder is 480-490mm, and the length of the connecting block is 40-45 mm; the length of the nose piece is 65-75 mm.
The total length of the propeller plunger is 570mm, the outer diameter of the cylinder is 120mm, the inner diameter of the cylinder is 101mm, the length of the cylinder is 485mm, and the length of the connecting block is 42 mm; the nose piece has a length of 70 mm.
The diameter of the front end piece is 120mm, and the depth of the blind hole is 35 mm;
the depth of the concave part of the connecting block is 18mm, the diameter of the front end of the connecting block is 103mm, and the step thickness is 15mm
Furthermore, the front end of the front end piece is provided with a heat-resistant layer, the heat-resistant layer is a tungsten layer, and the thickness of the heat-resistant layer is 1-5mm, and the thickness is contained in the total thickness of the front end piece.
The width of gas ring groove is 5mm, and the interval thickness of adjacent gas ring groove is 5mm, and the width of overhaul groove is 3 mm.
The diameters of the blind holes and the through holes are 16mm, and the blind holes and the through holes are both M16 threaded holes. The thickness of the front end plate is 12 mm.
The wall thickness of the cylinder was 9.5 mm.
The rear end of connecting block is equipped with displacement sensor for detect the propulsive displacement volume of plunger, and the plunger cartridge is equipped with proximity sensor in the inlet pipe, and proximity sensor is travel switch or photoelectric switch, and proximity sensor is triggered the back, and control pneumatic cylinder or motor make the plunger no longer move or retreat, realize process control. The proximity sensor is connected with the MCU; the displacement sensor is connected with an ADC port of the MCU through the amplifier. The MCU is also connected with a display screen, and the display screen is used for displaying real-time displacement and the like. The circuit block diagram is shown in fig. 3.
As shown in fig. 5, the displacement detection module includes a displacement sensor and an amplifier with adjustable amplification factor;
the amplifier with adjustable amplification factor comprises an operational amplifier U1 and a multi-way switch U2; the multi-way switch U2 is a one-out-of-four selector;
the output end Vin of the displacement sensor is connected with the inverting input end of the operational amplifier U1 through a resistor R0; the non-inverting input end of the operational amplifier U1 is grounded through a resistor R06, the non-inverting input end of the operational amplifier U1 is also connected with 4 input channels of a four-in-one selector through 4 resistors R01-R04 respectively, the output channel of the four-in-one selector is connected with the output end Vout of the operational amplifier U1, and the Vout is connected with the ADC end of the MCU;
2 output ports of the MCU are respectively connected with channel selection ends A and B of the one-out-of-four selector;
the operational amplifier U1 employs an LM393 device.
Calculation formula of Vout and Vin:
vout ═ Vin, (Rx + R0)/R0; wherein Rx ═ R01, R02, R03, or R04; determining which resistance to select based on the gate terminal AB; and R01, R02, R03 and R04 are each different; preferred R04-5-R03-25-R02-100-R01; r01-5 × R0. can conveniently achieve span and precision switching.
As shown in fig. 6, the display screen is connected to the MCU, and the brightness adjusting circuit of the display screen includes LED string, triode, potentiometer Rx and a/D converter; the triode is an NPN type triode; a knob switch is also arranged on the fixing frame of the display screen and is coaxially connected with the potentiometer Rx;
the potentiometer Rx and the first resistor R1 are connected in series to form a voltage division branch, one end of the voltage division branch is connected with the positive electrode Vcc of the power supply, and the other end of the voltage division branch is grounded; the connection point of the potentiometer Rx and the first resistor R1 is connected with the input end of the A/D converter; the output end of the A/D converter is connected with the data input port of the MCU;
the LED lamp string comprises a plurality of LED lamps which are connected in series; the anode of the LED lamp string is connected with the anode Vcc of the power supply; the negative electrode of the LED lamp string is connected with the C electrode of the triode, and the E electrode of the triode is grounded through a second resistor R2; the B pole of the triode is connected with the output end of the MCU. The power supply positive pole Vcc is 5V, and the A/D converter is an 8-bit serial output type converter.
Temperature control module
As shown in fig. 8-10, the temperature control module includes a temperature detection module, a wireless communication module, a rectifier, and an inverter;
the temperature detection module comprises an infrared temperature measurement unit for measuring the temperature in the carbonization furnace; the infrared temperature measuring unit comprises a main temperature measuring carbon tube 15 and a main infrared thermometer 16; the main temperature measuring carbon tube penetrates through the wall 14 of the carbonization furnace and is inserted on the carbonization furnace along the radial direction of the carbonization furnace, and the carbonization furnace is internally provided with an axial carbon tube 11; the front end of the main temperature measurement carbon tube is abutted with the carbon tube, the outer end of the main temperature measurement carbon tube is positioned outside the furnace wall, the main infrared thermometer is arranged at the outer end of the main temperature measurement carbon tube, and the data output end of the main infrared thermometer is connected with the MCU;
the AC side of the rectifier is connected with an AC power supply, the AC side of the rectifier is connected with the DC side of the inverter, and the AC side of the inverter supplies power to the carbon tube; and the pulse output end of the MCU is connected with the control end of a power switch in the inverter. The carbon tube is internally provided with a tungsten layer to increase the strength of the carbon tube.
The infrared temperature measuring unit comprises a standby temperature measuring carbon tube 17 and a standby infrared thermometer 18; the main temperature measurement carbon tube penetrates through the furnace wall 14 of the carbonization furnace and is inserted on the carbonization furnace along the radial direction of the carbonization furnace, the front end of the standby temperature measurement carbon tube is abutted with the carbon tube, the outer end of the standby temperature measurement carbon tube is positioned outside the furnace wall, the standby infrared thermometer is arranged at the outer end of the standby temperature measurement carbon tube, and the data output end of the standby infrared thermometer is connected with the MCU. The spare temperature measuring carbon tube 17 and the spare infrared thermometer 18 have the functions of spare and temperature correction.
The main temperature measuring carbon tube and the standby temperature measuring carbon tube are arranged in a straight line. I.e. symmetrical with respect to the carbon tube.
The temperature detection module also comprises a temperature sensor for measuring the temperature of the outer wall of the carbonization furnace, the output end of the temperature sensor is connected with the A/D conversion port of the MCU through an amplifier, and the outer wall of the carbonization furnace is provided with a water cooling device. The control to the water cooling device is realized based on the detection of the temperature of the outer wall, the rapid cooling of the outer wall of the furnace body is realized, and when the temperature is too high, the flow and the flow speed of cold water are increased, so that the purpose of cooling is achieved. The MCU is connected with a display screen and a key or a touch pad for setting temperature. The MCU is connected with a communication module. The communication module is a wireless communication module (such as GPRS, 3G, 4G, 5G modules and the like, or a remote control module, so that the temperature can be remotely controlled, an operator does not need to control the temperature on site, and the safety is high).
Fourth, air supply module
As shown in fig. 7 and 11, a shielding gas inlet pipe 24 is arranged on the inlet pipe, one end of the shielding gas inlet pipe is communicated with the inlet pipe, and the other end of the shielding gas inlet pipe is connected with a gas source; the feeding pipe is butted with a feeding hole at the rear end of the carbon tube furnace; the front end of the carbon tube furnace is provided with a discharging device; the discharging device is provided with an upward impurity discharging pipe 32 and a downward discharging pipe 31; the impurity discharging pipe is used for discharging flue gas. Preferably, a filter screen is arranged in the impurity discharging pipe to prevent carbon powder from being discharged along with the flue gas. The protective gas inlet pipe is provided with a one-way valve. The gas supply module of the graphite carbonization system further comprises an opening valve arranged on the gas inlet pipe, and the opening valve is controlled by the MCU. The air inlet pipe is provided with an air pressure sensor; the air pressure sensor is connected with the MCU.
Fifth, discharging device
The discharging device 3 comprises a main pipe 35, a discharging pipe 31 and an impurity discharging pipe 32; the main pipe is horizontally arranged, one end of the main pipe is butted with a discharge port of the carbonization furnace, and the other end of the main pipe is provided with an end cover 34; the impurity discharging pipe is used for discharging flue gas.
The impurity discharging pipe and the discharging pipe are respectively arranged above and below the main pipe; the impurity discharging pipe and the discharging pipe are communicated with the main pipe, and the aperture of the impurity discharging pipe is smaller than that of the discharging pipe. Preferably, the end cap is hinged to the end of the main tube to facilitate opening of the end cap to clear the dredging conduit.
An outer pipe 36 is sleeved outside the main pipe, and a closed cavity is formed between the outer pipe and the inner pipe; the outer pipe is provided with a water inlet pipe 37 and a water outlet pipe 38; the water inlet pipe and the water outlet pipe are both communicated with the closed cavity; the closed cavity is only provided with openings at the water inlet pipe and the water outlet pipe, and the rest parts are sealed. One part of the flange plate is used as part of the inner wall of the closed space, and the cooling device based on the water inlet pipe, the water outlet pipe and the closed cavity is used for cooling the flange.
The water inlet pipe is arranged below the outer pipe, and the water outlet pipe is arranged above the outer pipe; when the carbonization furnace works, cooling water is input from the water inlet pipe to carry out water cooling on the discharging device. Preferably, the water outlet pipe and the water inlet pipe are both arranged along the radial direction of the outer pipe.

Claims (10)

1. A graphite carbonization method based on high-temperature gasification impurity removal is characterized by comprising the following steps:
step 1: a feeding step;
pushing graphite powder into the carbonization furnace by adopting a pushing mechanism based on hydraulic pressure or motor drive;
step 2: a carbonization purification step;
keeping the temperature in the carbonization furnace at 2500-3200 ℃, and carbonizing and purifying the graphite powder in the carbonization furnace in a protective atmosphere; metal impurities in the graphite powder are gasified at high temperature;
step 3, discharging;
and discharging the waste gas and the carbonized and purified graphite powder through a discharging device.
2. The graphite carbonization method based on high-temperature gasification impurity removal according to claim 1, wherein the steps 1-3 are continuously and circularly performed to realize continuous production.
3. The graphite carbonization method based on high-temperature gasification impurity removal according to claim 1, characterized in that a material pushing mechanism is used for intermittently pushing the raw material into the carbonization furnace; the pushing mechanism comprises a plunger (5) and a driving mechanism for driving the plunger to reciprocate in the feeding pipe; the plunger is positioned in the feeding pipe; the feeding pipe is communicated with the inlet of a carbonization furnace in the graphite carbonization system, and a hopper communicated with the feeding pipe is arranged above the feeding pipe; the driving mechanism is a hydraulic driving mechanism; the hydraulic driving mechanism comprises a hydraulic oil cylinder (22), a hydraulic station (23) and a valve for controlling the on-off of a liquid path; the valve is controlled by the controller; the hydraulic station is connected with the hydraulic oil cylinder through a hydraulic oil pipe; the piston of the hydraulic oil cylinder is connected with the plunger piston through a push rod, and the controller is an MCU.
4. The graphite carbonization method based on high-temperature gasification impurity removal according to claim 3, wherein the MCU is connected with a human-computer interface device; the human interface device includes a display screen and keys or a touch pad for inputting parameters.
5. A graphite carbonization method based on high-temperature gasification impurity removal as claimed in claim 4, characterized in that the material is pushed once every 5-15 minutes.
6. The graphite carbonization method based on high-temperature gasification impurity removal as defined in claim 1, wherein a discharge pipe and an impurity removal pipe are arranged on the discharge device, and a water cooling device is further arranged on the discharge device.
7. The graphite carbonization method based on high-temperature gasification impurity removal according to claim 6, characterized in that the discharge device (3) comprises a main pipe (35), a discharge pipe (31) and an impurity removal pipe (32); the main pipe is horizontally arranged, one end of the main pipe is butted with a discharge hole of the carbonization furnace, and the other end of the main pipe is provided with an end cover (34);
the impurity discharging pipe and the discharging pipe are respectively arranged above and below the main pipe; the impurity discharging pipe and the discharging pipe are communicated with the main pipe;
an outer pipe (36) is sleeved outside the main pipe, and a closed cavity is formed between the outer pipe and the inner pipe; the outer pipe is provided with a water inlet pipe (37) and a water outlet pipe (38); the water inlet pipe and the water outlet pipe are both communicated with the closed cavity;
the water inlet pipe is arranged below the outer pipe, and the water outlet pipe is arranged above the outer pipe; when the carbonization furnace works, cooling water is input from the water inlet pipe to carry out water cooling on the discharging device.
8. The graphite carbonization method based on high-temperature gasification impurity removal according to claim 1, wherein the carbonization furnace, the feeding pipe and the main pipe of the discharging device are all horizontally arranged.
9. A graphite carbonization method based on high-temperature gasification impurity removal as claimed in claim 1, characterized in that the carbonization furnace is a carbon tube furnace, the heat generating components of the carbon tube furnace are carbon tubes, and the inner walls of the carbon tubes are provided with a reinforcing layer.
10. The graphite carbonization method based on high-temperature gasification impurity removal according to any one of claims 1 to 9, wherein an air inlet pipe is arranged on the feed pipe, and the air inlet pipe is communicated with the feed pipe; protective gas enters the furnace body of the carbonization furnace from the gas inlet pipe; the protective gas is inert gas or nitrogen.
CN201811044791.2A 2018-09-07 2018-09-07 Graphite carbonization method based on high-temperature gasification impurity removal Pending CN110885081A (en)

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CN111960413A (en) * 2020-08-17 2020-11-20 内蒙古恒胜新能源科技有限公司 Modification method of natural graphite negative electrode material
CN112320795A (en) * 2020-12-03 2021-02-05 长沙修恒信息科技有限公司 Full-process automatic graphite purification method
CN113341862A (en) * 2021-06-03 2021-09-03 自贡硬质合金有限责任公司 Remote control timing propulsion device and control method

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CN113341862A (en) * 2021-06-03 2021-09-03 自贡硬质合金有限责任公司 Remote control timing propulsion device and control method

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