Horizontal-vertical cooperative continuous graphitization process and device

Abstract

The present application relates to a kind of lying and standing synergic continuous graphitization process and device, device includes self-heating graphite tube rotary drum, power receiving electrode stick, additional heating heat-resistant steel rotary drum, graphitization vertical furnace, self-heating graphite tube rotary drum is connected in series with the additional heating heat-resistant steel rotary drum, the inner cylinder of the self-heating graphite tube rotary drum is graphite tube, two ends of the graphite tube are connected electric slip ring, and are heated by power receiving electrode stick, the inner cylinder of the additional heating heat-resistant steel rotary drum is heat-resistant steel cylinder, the feed end of the heat-resistant steel cylinder is connected with loading fixed end, the discharge end of the self-heating graphite tube rotary drum is connected with discharge fixed end, the graphitization vertical furnace is arranged below the discharge fixed end, and is connected with the discharge port of discharge fixed end.The beneficial effects of the present application are: the coating of carbon material, low-temperature carbonization, high-temperature carbonization, graphitization are gathered in a set of device and carried out synergic continuous production, realize power saving, environmental protection, high yield, high quality.

Description

TECHNICAL FIELD

[0001] The present application relates to industrial furnace equipment, in particular to a horizontal-vertical cooperative continuous graphitization process and device. BACKGROUND

[0002] In the production process of battery graphite negative electrode material, multiple sets of equipment and production processes are required, and each process cannot be continuously carried out. At present, petroleum coke or pitch coke coating, low-temperature carbonization, high-temperature carbonization and graphitization are completed in different equipment, and multiple heating and cooling are required, which has high energy consumption and serious pollution.

[0003] The main technical difficulties of the prior art are: the coated petroleum coke or pitch coke contains a large amount of volatile matter, which cannot be graphitized in one step, otherwise the performance of the coating material will be damaged, secondly, the rapid release of a large amount of volatile matter will cause the furnace to be blown out, thirdly, it is very difficult to integrate low-temperature carbonization and high-temperature carbonization in one device, and fourthly, the material without high-temperature carbonization, especially the powder, limits continuous graphitization, which will cause the furnace to be blown out, blocked and blown out. SUMMARY

[0004] The purpose of the present application is to provide a horizontal-vertical cooperative continuous graphitization process and device, which integrates the coating, low-temperature carbonization, high-temperature carbonization and graphitization of carbon materials in one device for cooperative continuous production, achieving power saving, environmental protection, high yield and high quality.

[0005] In order to achieve the above purpose, the present application adopts the following technical scheme:

[0006] A horizontal-vertical cooperative continuous graphitization process, which uses a horizontal rotary heating furnace and a graphitization vertical furnace for cooperative production, the horizontal rotary heating furnace is connected in series with a low-temperature zone and a high-temperature zone, the material discharged from the high-temperature zone is sent to the graphitization vertical furnace, and specifically comprises:

[0007] 1) The low-temperature zone uses a heat-resistant steel drum for external heating, and completes the coating and low-temperature carbonization of carbon materials, and the heating temperature interval is adjustable from room temperature to 1000℃;

[0008] 2) The high-temperature zone uses a graphite tube rotary drum for self-heating, and the heating temperature interval is adjustable from 500℃ to 1700℃, and the carbon materials are subjected to high-temperature carbonization and graphitization, and the graphitized materials are subjected to high-temperature carbonization after secondary coating;

[0009] 3) The low-temperature zone and the high-temperature zone are inclined as a whole, the material is conveyed to the graphitization vertical furnace by the rotating conveying power, and the material falls into the graphitization vertical furnace by gravity;

[0010] 4) Anode and cathode of the graphitization vertical furnace are made of graphite material, an annular channel is formed between the anode and the cathode, carbon material pre-graphitized in high temperature zone is used as resistance material to realize continuous heating between the two poles, and the highest heating temperature is 3000 DEG C.

[0011] The overall inclination angle of the low temperature zone and the high temperature zone is 1-5 DEG, and the transmission device adopts frequency conversion speed regulation.

[0012] A device for horizontal and vertical cooperative continuous graphitization process, comprising a self-heating graphite tube rotary drum, a power receiving electrode rod, an external heating heat-resistant steel rotary drum and a graphitization vertical furnace, the self-heating graphite tube rotary drum is connected in series with the external heating heat-resistant steel rotary drum, the inner cylinder of the self-heating graphite tube rotary drum is a graphite tube, the two ends of the graphite tube are connected with an electric slip ring and are heated by the power receiving electrode rod, the inner cylinder of the external heating heat-resistant steel rotary drum is a heat-resistant steel cylinder, the feeding end of the heat-resistant steel cylinder is connected with a feeding fixed end, the discharging end of the self-heating graphite tube rotary drum is connected with a discharging fixed end, the graphitization vertical furnace is arranged below the discharging fixed end and is connected with a discharging port of the discharging fixed end.

[0013] The graphitization vertical furnace comprises an inner graphite column, an outer graphite cylinder and a material cooler, the inner graphite column and the outer graphite cylinder form an annular channel, the inner graphite column and the outer graphite cylinder are respectively connected with electrodes, the annular channel is connected with the discharging port of the discharging fixed end, the bottom of the annular channel is provided with a discharging pipe, the lower part of the discharging pipe is provided with a material cooler, and the outer part of the outer graphite cylinder is provided with a heat insulation layer and a supporting device.

[0014] The discharging fixed end comprises a steel structure shell, a refractory heat insulation material layer, a plug valve and a discharging chute, the steel structure shell is wrapped outside the refractory heat insulation material layer, the inside of the refractory heat insulation material layer is a discharging cavity, the discharging end of the self-heating graphite tube rotary drum is inserted into the discharging cavity, the plug valve and the discharging chute are arranged at the bottom of the discharging cavity, and the discharging port of the discharging chute is connected with the graphitization vertical furnace.

[0015] The feeding fixed end comprises a steel structure shell, a refractory heat insulation material layer and a spiral feeder, the steel structure shell is wrapped outside the refractory heat insulation material layer, the inside of the refractory heat insulation material layer is a feeding cavity, the feeding end of the heat-resistant steel cylinder is inserted into the feeding cavity, and the spiral feeder is connected with the feeding end of the heat-resistant steel cylinder.

[0016] Sealing devices are arranged between the heat-resistant steel cylinder and the feeding fixed end and between the self-heating graphite tube rotary drum and the discharging fixed end.

[0017] The sealing device comprises a flexible sealing ring, a graphite sealing ring, an outer fixed tube, an inner sealing tube, a sealing alignment device, the inner sealing tube is connected with the self-heating graphite tube rotary cylinder or the heat-resistant steel cylinder through the sealing alignment device, a plurality of flexible sealing rings are arranged between the inner sealing tube and the outer fixed tube in the axial direction, and the graphite sealing ring is arranged at the innermost side of the plurality of flexible sealing rings, and the outer fixed tube is connected with a discharging fixed end or a charging fixed end.

[0018] The sealing alignment device comprises a lead screw and a corrugated expander, the self-heating graphite tube rotary cylinder or the heat-resistant steel cylinder is connected with the inner sealing tube through the lead screw, and the corrugated expander is further arranged between the self-heating graphite tube rotary cylinder or the heat-resistant steel cylinder and the inner sealing tube for sealing.

[0019] The self-heating graphite tube rotary cylinder comprises a graphite tube, a layer of refractory insulation material wrapped outside the graphite tube, and a steel outer shell fixed outside the layer of refractory insulation material.

[0020] Compared with the prior art, the present application has the following beneficial effects:

[0021] The present application provides a horizontal-vertical cooperative continuous graphitization process and device, which integrates the coating of carbon material, low-temperature carbonization, high-temperature carbonization and graphitization in one device for cooperative continuous production, thereby achieving power saving, environmental protection, high yield and high quality. BRIEF DESCRIPTION OF DRAWINGS

[0022] Figure 1 is a schematic diagram of the overall structure of the present application;

[0023] In the figure: 1 - feeding system, 2 - charging fixed end, 3 - heat-resistant steel cylinder, 4 - transmission device, 5 - power receiving electrode rod, 6 - electric slip ring, 7 - graphite tube, 8 - discharging fixed end, 9 - discharging chute, 10 - inner graphite column, 11 - outer graphite cylinder, 12 - heat insulation layer and supporting device, 13 - material cooler, 14 - vertical furnace sealing rotary unloader, 15 - supporting roller, 16 - screw feeder, 17 - flexible sealing ring, 18 - graphite sealing ring, 19 - lead screw, 20 - corrugated expander, and 21 - electrode. DETAILED DESCRIPTION

[0024] The specific embodiments of the present application will be further described below in combination with the drawings:

[0025] See Figure 1 A horizontal-vertical cooperative continuous graphitization process, which adopts a horizontal rotary heating furnace and a graphitization vertical furnace for cooperative production, the horizontal rotary heating furnace is connected in series with a low-temperature zone and a high-temperature zone, the discharging material of the high-temperature zone is sent into the graphitization vertical furnace, and specifically comprises:

[0026] 1) Low temperature zone adopts heat-resistant steel material drum form to heat, complete carbon material coating, low temperature carbonization, heating temperature interval from room temperature to 1000℃ adjustable;

[0027] 2) High temperature zone adopts graphite tube rotary drum self-heating type, heating temperature interval from 500℃ to 1700℃ adjustable, high temperature carbonization, graphitization and high temperature carbonization of graphitized material after secondary coating of carbon material;

[0028] 3) Low temperature zone and high temperature zone are inclined as a whole, material is conveyed to the graphitization vertical furnace by the rotating conveying power, and the material falls into the graphitization vertical furnace by gravity;

[0029] 4) The anode and cathode of the graphitization vertical furnace are both made of graphite material, an annular channel is formed between the anode and the cathode, the carbon material carbonized and pre-graphitized in the high temperature zone is used as resistance material to realize continuous heating between the two poles, and the highest heating temperature is 3000℃.

[0030] The overall inclination angle of the low temperature zone and the high temperature zone is 1°-5°, and the transmission device 4 adopts frequency conversion speed regulation.

[0031] A device for a horizontal-vertical cooperative continuous graphitization process, comprising a self-heating graphite tube rotary drum, a power receiving electrode rod 5, an externally heated heat-resistant steel rotary drum and a graphitization vertical furnace, the self-heating graphite tube rotary drum is connected in series with the externally heated heat-resistant steel rotary drum, the inner cylinder of the self-heating graphite tube rotary drum is a graphite tube 7, both ends of the graphite tube 7 are connected with an electric slip ring 6 and are heated by the power receiving electrode rod 5, the inner cylinder of the externally heated heat-resistant steel rotary drum is a heat-resistant steel cylinder 3, the heat-resistant steel cylinder 3 is connected with the graphite tube 7 through an insulating flange, one end of the heat-resistant steel cylinder 3 for feeding is connected with a feeding fixing end 2, one end of the self-heating graphite tube rotary drum for discharging is connected with a discharging fixing end 8, and the graphitization vertical furnace is arranged below the discharging fixing end 8 and is connected with a discharging port of the discharging fixing end 8.

[0032] Both ends of the graphite tube 7 in the high temperature zone adopt the power receiving electrode rod 5 and the electric slip ring 6 to deliver electricity into the graphite tube 7, and the graphite tube 7 is heated by the current, and since the graphite can withstand a high temperature of more than 3000℃ in the case of air insulation, the graphite rotary drum of the present application can withstand a high temperature of more than 2000℃.

[0033] The graphitization vertical furnace comprises an inner graphite column 10, an outer graphite cylinder 11 and a material cooler 13, the inner graphite column 10 and the outer graphite cylinder 11 form an annular channel, the inner graphite column 10 and the outer graphite cylinder 11 are respectively connected with electrodes 21, the annular channel is connected with the discharging port of the discharging fixing end 8, the bottom of the annular channel is a discharging pipe, the lower part of the discharging pipe is provided with the material cooler 13, and the outer part of the outer graphite cylinder 11 is provided with a heat insulation layer and a supporting device 12.

[0034] The discharge fixed end 8 comprises a steel structure shell, a refractory insulation material layer, a plug valve, and a discharge chute 9. The steel structure shell is wrapped outside the refractory insulation material layer, the inside of the refractory insulation material layer is a discharge cavity, the discharge end of the self-heating graphite tube rotary drum is inserted into the discharge cavity, the plug valve and the discharge chute 9 are arranged at the bottom of the discharge cavity, and the discharge port of the discharge chute 9 is connected with the graphitization vertical furnace.

[0035] The charging fixed end 2 comprises a steel structure shell, a refractory insulation material layer, and a screw feeder 16. The steel structure shell is wrapped outside the refractory insulation material layer, the inside of the refractory insulation material layer is a feeding cavity, the feeding end of the heat-resistant steel cylinder 3 is inserted into the feeding cavity, and the screw feeder 16 is connected with the feeding end of the heat-resistant steel cylinder 3.

[0036] The screw feeder 16 extends into the feeding cavity from the side of the charging fixed end 2 and is connected with the heat-resistant steel cylinder 3. A corrugated compensator is arranged between the part of the screw feeder 16 outside the charging fixed end 2 and the charging fixed end 2 for sealing during feeding. The feeding port of the screw feeder 16 is connected with the feeding system 1.

[0037] Sealing devices are arranged between the heat-resistant steel cylinder 3 and the charging fixed end 2 and between the self-heating graphite tube rotary drum and the discharge fixed end 8.

[0038] The sealing device comprises a flexible sealing ring 17, a graphite sealing ring 18, an outer fixed tube, an inner sealing tube, and a sealing alignment device. The inner sealing tube is connected with the self-heating graphite tube rotary drum or the heat-resistant steel cylinder 3 through the sealing alignment device. A plurality of flexible sealing rings 17 are arranged in the axial direction between the inner sealing tube and the outer fixed tube. The graphite sealing ring 18 is arranged at the innermost side of the plurality of flexible sealing rings 17. The outer fixed tube is connected with the discharge fixed end 8 or the charging fixed end 2.

[0039] The sealing alignment device comprises a lead screw 19 and a corrugated expander 20. The self-heating graphite tube rotary drum or the heat-resistant steel cylinder 3 is connected with the inner sealing tube through the lead screw 19. The corrugated expander 20 is further arranged between the self-heating graphite tube rotary drum or the heat-resistant steel cylinder 3 and the inner sealing tube for sealing.

[0040] The sealing device adjusts the concentricity with the self-heating graphite tube rotary drum or the heat-resistant steel cylinder 3 through the sealing alignment device.

[0041] The lead screw 19 is composed of a nut in the middle and screw rods with positive and reverse threads at both ends. The length of the lead screw is adjusted by screwing the nut, so as to adjust the radial distance between the inner sealing tube and the self-heating graphite tube rotary drum or the outer heated heat-resistant steel rotary drum. In the circumferential direction, the adjustment of the screw rod achieves the concentricity of the sealing surface cylinder and the rotary kiln. The corrugated expander 20 plays a sealing role between the inside and outside of the kiln and can provide position compensation during debugging.

[0042] After the self-heating graphite tube rotary drum or the externally heated heat-resistant steel rotary drum is installed in place, the sealing surface is manually aligned, that is, the concentricity of the sealing device and the rotary drum is adjusted, and several distance adjusting lead screws 19 play a role in adjusting the concentricity and supporting the sealing device, so that the purpose of adjusting the center can be achieved during construction and debugging. After adjustment is completed, the outer fixed tube is fixedly connected with the charging fixed end 2 or the discharging fixed end 8 through bolts.

[0043] The self-heating graphite tube rotary drum comprises a graphite tube 7, a layer of refractory insulation material wrapped outside the graphite tube 7, and a steel shell fixed outside the layer of refractory insulation material.

[0044] The horizontal rotary heating furnace part of the present application adopts two parts of low-temperature zone and high-temperature zone in series, integrated into a set of rotary heating treatment furnace, with a downward inclination angle from the charging end to the discharging end, generally 1°-5°, and the transmission device 4 adopts frequency conversion speed regulation, which can automatically adjust the amount of material passing through the furnace. The low-temperature zone adopts a heat-resistant steel drum for external heating, which can complete the coating of carbon materials, low-temperature carbonization, and the heating temperature interval is adjustable from room temperature to 1000℃. The high-temperature zone adopts a graphite tube rotary drum with electric heating, and the heating temperature interval is adjustable from 500℃ to 1700℃, which can perform high-temperature carbonization and graphitization of carbon materials after secondary coating. The graphitization furnace adopts a vertical furnace, and the material is transported by gravity, connected to the lower part of the rotary heating furnace discharge port and working cooperatively with the horizontal rotary furnace. The high-temperature material after high-temperature carbonization in the horizontal rotary furnace is directly added to the vertical graphitization furnace through the discharge chute, and the anode and cathode of the vertical graphitization furnace are both made of graphite material, forming an annular channel between the anode and the cathode. The carbon material after high-temperature carbonization and pre-graphitization is heated continuously as a resistance material between the two poles, and the material temperature can be heated to 2800℃-3000℃ and kept for 10-30 minutes to realize the graphitization of the carbon material. The amount of material in the vertical furnace is adjusted by the vertical furnace sealing rotary discharger 14 to realize cooperation with the horizontal rotary furnace. The lower discharge pipe of the vertical graphitization furnace is provided with a partition type cooler, and the material after graphitization is discharged outside the furnace through the rotary vertical furnace sealing rotary discharger 14 after cooling, completing the continuous production process of coating, low-temperature carbonization, high-temperature carbonization, and graphitization.

Claims

1. A horizontal-vertical synergic continuous graphitization process, characterized by, The horizontal rotary heating furnace and the graphitization vertical furnace are used in cooperation to produce, the horizontal rotary heating furnace is two parts in series of low temperature area and high temperature area, the high temperature area discharges into the graphitization vertical furnace, specifically includes: 1) The low temperature area uses the heat-resistant steel material quality roller form to carry out the external heating, the heating temperature interval is from room temperature to 1000℃; 2) The high temperature area adopts the graphite pipe rotary drum self-heating type, the heating temperature interval is from 500℃ to 1700℃; 3) The low temperature area and the high temperature area are overall inclined, the material is transmitted to the graphitization vertical furnace by the transmission power of rotation, and the material falls into the graphitization vertical furnace by gravity; 4) The anode and the cathode of the graphitization vertical furnace all adopt the graphite material, an annular channel is formed between the anode and the cathode, the carbon material carbonized and pre-graphitized in the high temperature area is used as the resistance material to realize continuous heating between the two poles, and the highest heating temperature is 3000℃; The device used in the horizontal-vertical cooperation continuous graphitization process includes the self-heating graphite pipe rotary drum, the power receiving electrode rod, the external heating heat-resistant steel rotary drum and the graphitization vertical furnace, the self-heating graphite pipe rotary drum is connected with the external heating heat-resistant steel rotary drum in series, the inner cylinder of the self-heating graphite pipe rotary drum is a graphite pipe, the two ends of the graphite pipe are connected with the electric slip ring and are heated by the power receiving electrode rod, the inner cylinder of the external heating heat-resistant steel rotary drum is a heat-resistant steel cylinder, the feeding end of the heat-resistant steel cylinder is connected with the loading fixed end, the discharging end of the self-heating graphite pipe rotary drum is connected with the discharging fixed end, and the graphitization vertical furnace is arranged below the discharging fixed end and is connected with the discharging port of the discharging fixed end; Sealing devices are arranged between the heat-resistant steel cylinder and the loading fixed end and between the self-heating graphite pipe rotary drum and the discharging fixed end; The sealing device includes the flexible sealing ring, the graphite sealing ring, the outer fixed tube, the inner sealing tube and the sealing aligning device, the inner sealing tube is connected with the self-heating graphite pipe rotary drum or the heat-resistant steel cylinder through the sealing aligning device, a plurality of flexible sealing rings are arranged in the axial direction between the inner sealing tube and the outer fixed tube, the graphite sealing ring is arranged at the innermost side of the plurality of flexible sealing rings, and the outer fixed tube is connected with the discharging fixed end or the loading fixed end; The sealing aligning device includes the distance adjusting lead screw and the corrugated expander, the self-heating graphite pipe rotary drum or the heat-resistant steel cylinder is connected with the inner sealing tube through the distance adjusting lead screw, and the corrugated expander is further arranged between the self-heating graphite pipe rotary drum or the heat-resistant steel cylinder and the inner sealing tube for sealing.

2. A synergistic continuous graphitization process for horizontal and vertical standing according to claim 1, characterized in that, The overall inclination angle of the low temperature area and the high temperature area is 1°-5°, and the transmission device adopts variable frequency speed regulation.

3. A synergistic continuous graphitization process for horizontal and vertical standing according to claim 1, characterized in that, The graphitization vertical furnace includes the inner graphite column, the outer graphite cylinder and the material cooler, the inner graphite column and the outer graphite cylinder form an annular channel, the inner graphite column and the outer graphite cylinder are respectively connected with electrodes, the annular channel is connected with the discharging port of the discharging fixed end, the bottom of the annular channel is a discharging pipe, the lower part of the discharging pipe is provided with the material cooler, and the outer graphite cylinder is externally provided with a heat insulation layer and a supporting device.

4. A synergistic continuous graphitization process for horizontal and vertical standing according to claim 1, characterized in that, The discharge fixed end comprises a steel structure shell, a refractory insulation material layer, a plug valve and a discharge chute, the steel structure shell is wrapped outside the refractory insulation material layer, the inside of the refractory insulation material layer is a discharge cavity, the discharge end of the self-heating graphite tube rotary drum is inserted into the discharge cavity, the plug valve and the discharge chute are arranged at the bottom of the discharge cavity, and the discharge port of the discharge chute is connected with the graphitization vertical furnace.

5. A synergistic continuous graphitization process for horizontal and vertical standing according to claim 1, characterized in that, The charging fixed end comprises a steel structure shell, a refractory insulation material layer and a screw feeder, the steel structure shell is wrapped outside the refractory insulation material layer, the inside of the refractory insulation material layer is a feeding cavity, the feeding end of the heat-resistant steel cylinder is inserted into the feeding cavity, and the screw feeder is connected with the feeding end of the heat-resistant steel cylinder.

6. A synergistic continuous graphitization process for horizontal and vertical standing according to claim 1, characterized in that, The self-heating graphite tube rotary drum comprises a graphite tube, a refractory insulation material layer wrapped outside the graphite tube and a steel shell fixed outside the refractory insulation material layer.

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