CN105129762A - Belt-type atmosphere sintering furnace for continuous production of lithium iron phosphate cathode material - Google Patents
Belt-type atmosphere sintering furnace for continuous production of lithium iron phosphate cathode material Download PDFInfo
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- CN105129762A CN105129762A CN201510607178.7A CN201510607178A CN105129762A CN 105129762 A CN105129762 A CN 105129762A CN 201510607178 A CN201510607178 A CN 201510607178A CN 105129762 A CN105129762 A CN 105129762A
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Abstract
The invention belongs to the field of lithium iron phosphate cathode material preparation, and particularly relates to a belt-type atmosphere sintering furnace for continuous production of a lithium iron phosphate cathode material. The belt-type atmosphere sintering furnace comprises a furnace body and a support mechanism used for supporting the furnace body, and is characterized by further comprising a through hearth, a feed opening, a discharge opening, a roller-type sealing mechanism, a plate type conveying belt, a cooling discharge device, protective gas input and gas pressure control devices and a temperature control device, wherein the through hearth is arranged in the furnace body; the feed opening and the discharge opening are formed in side surfaces of the furnace body; the roller-type sealing mechanism is arranged on one side surface of the furnace body; the plate type conveying belt penetrates the through hearth and is provided with grooves; the cooling discharge device is arranged before the discharge opening; the protective gas input and gas pressure control devices and the temperature control device are connected with the through hearth; the through hearth is divided into four sections of working areas through three sealing walls. As an integral steel sheet with the grooves serves as the conveying belt, continuous production can be realized; a unique sealing mechanism is adopted, so as to not only seal the hearth, but also further reduce the oxygen content of a high-temperature working area by air pressure difference among different working areas, and improve the property of the material.
Description
Technical field
The invention belongs to lithium iron phosphate positive material preparation field, be specifically related to a kind of belt atmosphere sintering furnace of continuous seepage lithium iron phosphate positive material.
Background technology
The advantages such as safety performance is good, discharge-rate is high, cycle performance is excellent owing to having for LiFePO 4 material, use temperature wide ranges, life-span length, environmental protection, just got more and more people's extensive concerning since appearance, be expected to be widely used in electromobile and portable electric appts.In recent years, along with country more and more payes attention to environmental issue, especially since 2011 to reasons such as the regulations of lead-acid storage battery production, facilitate developing rapidly of power ferric phosphate lithium cell industry.But, due to LiFePO 4 material complicated process of preparation, production unit is immature, technical threshold is higher, therefore industrialization speed is comparatively slow, limits it and further applies.
At present, the preparation of LiFePO 4 material mainly adopts high-temperature solid phase reaction method, heat treated temperatures as high 600-800 DEG C.At this temperature, the as easy as rolling off a log oxidation of the ferrous ion in material, causes the degradation of material.Therefore, in order to prevent LiFePO 4 material oxidized in production process, domestic enterprise adopts step equipment for Heating Processing, as: atmosphere protection box-type furnace, atmosphere protection clock hood type furnace etc., significantly limit the production efficiency of material.In recent years, some domestic equipment manufacturers attempt pushed bat kiln, meshbeltfurnace, the rotary kiln that exploitation can be used for continuous seepage LiFePO 4 material, and try out in the enterprise that some produce LiFePO 4 material, achieve some results, but still differ greatly with step equipment for Heating Processing in the stability and consistence of material property.Meanwhile, also have some at present about the patent of the equipment of continuous seepage LiFePO 4 material, as the patent No. be CN201587859 patent describes the horizontal continuous producing apparatus of a kind of LiFePO 4 material microwave heating; The patent No. is that a kind of ferric lithium phosphate precursor sintering that patent describes of CN102092699 prepares iron lithium phosphate method and microwave sintering apparatus; The patent No. is that patent describes of CN201971642U a kind of highly leads lithium iron phosphate sintering device.But the various equipment involved by above-mentioned patent, still exist some defects, while being difficult to ensure production efficiency in actual production, take into account stability and the consistence of material.
Summary of the invention
The present invention is directed to the deficiency that existing LiFePO 4 material production unit cannot take into account production efficiency and product performance, provide a kind of temperature control accurately, low oxygen content continous way can produce the belt atmosphere sintering furnace of lithium iron phosphate positive material.
In order to realize foregoing invention object, the present invention adopts following technical scheme: a kind of belt atmosphere sintering furnace of continuous seepage lithium iron phosphate positive material, comprising: the supporting mechanism of body of heater and support body of heater; It is characterized in that, also comprise the through burner hearth being positioned at body of heater, the opening for feed being positioned at body of heater side and discharge port, the trolley type sealing mechanism being arranged at body of heater side, the shielding gas input being connected through burner hearth through the slat conveyer of the band groove of through burner hearth, the cooling discharging device that is positioned at discharge port front end and gas pressure control device and temperature-control device, opening for feed and discharge port all adopt trolley type sealing mechanism to seal; Wherein, it is interval that through burner hearth is divided into four segment process by three seals wall; the working temperature in each interval and the air pressure of shielding gas there are differences, and each sealed wall leaves narrow gap, and described gap only allows slat conveyer and lithium iron phosphate positive material to pass through.
The belt atmosphere sintering furnace of aforesaid a kind of continuous seepage lithium iron phosphate positive material, the length between first paragraph process island is 1.5-2 rice, and temperature is 80-150 DEG C, and shielding gas pressure is P1; Length between second segment process island is 2.5-3 rice, and temperature is 300-450 DEG C, and shielding gas pressure is P2; 3rd segment process length of an interval degree is 6-8 rice, and temperature is 600-700 DEG C, and shielding gas pressure is P3; 4th segment process interval is between cooling zone, and be provided with circulating water cooling device, length is 2.5-3.5 rice, and shielding gas pressure is P4; Wherein, the shielding gas pressure in each interval is all a little more than standard atmospheric pressure P0, and the mutual relationship between four is: P2=P3>P1>P4.
The belt atmosphere sintering furnace of aforesaid a kind of continuous seepage lithium iron phosphate positive material, described opening for feed and discharge port lay respectively at the both sides of body of heater, leave the narrow gap that slat conveyer and lithium iron phosphate positive material can be allowed to pass through in trolley type sealing mechanism, opening for feed and discharge port are each passed through the narrow gap in trolley type sealing mechanism.
The belt atmosphere sintering furnace of aforesaid a kind of continuous seepage lithium iron phosphate positive material, the roller of described trolley type sealing mechanism is made up of the rubbery outer cover of hollow copper roller and parcel hollow copper rod, and hollow copper roller inside is passed through for recirculated cooling water.
The belt atmosphere sintering furnace of aforesaid a kind of continuous seepage lithium iron phosphate positive material, trolley type sealing mechanism is made up of at least 2 rollers and the spring that is connected with upper roller, according to lithium iron phosphate positive material thickness regulating spring height to regulate the distance between the adjacent rollers below upper roller, upper roller, make described distance only allow slat conveyer and lithium iron phosphate positive material to pass through, keep furnace chamber to be in sealed state all the time.
The belt atmosphere sintering furnace of aforesaid a kind of continuous seepage lithium iron phosphate positive material, the slat conveyer of sintering oven is made up of the monoblock type steel sheet with groove, lithium iron phosphate positive material is positioned in groove, and conveying belt completes the transportation work of lithium iron phosphate positive material under the effect of power transmission.
The belt atmosphere sintering furnace of aforesaid a kind of continuous seepage lithium iron phosphate positive material, the slat conveyer of sintering oven only has one to be arranged in through burner hearth, and another is positioned at burner hearth outside.
The belt atmosphere sintering furnace of aforesaid a kind of continuous seepage lithium iron phosphate positive material, the monoblock type steel sheet thickness of composition slat conveyer is 10-50mm, and material is spring steel.
The belt atmosphere sintering furnace of aforesaid a kind of continuous seepage lithium iron phosphate positive material; the temperature-control device of sintering oven, shielding gas input and gas pressure control device adopts PLC to control; the temperature of each operation interval of real-time monitoring and gaseous tension, and can adjust the temperature of operation interval and pressure.
The invention has the beneficial effects as follows: apparatus of the present invention are belt atmosphere sintering furnace, have employed the monoblock type steel sheet of band groove as conveying belt, can realize the production of continous way, not only efficiency is high, and can reduce the quantity of operator, saves labor cost; Present invention employs unique sealing mechanism, not only can realize the sealing of furnace chamber, and the oxygen level in hot operation interval can be reduced by the draught head in different operating interval further, improve the performance of material.Apparatus of the present invention, as a kind of continuous production equipment taking into account production efficiency and material property, are expected to be widely used in the large-scale production of lithium iron phosphate positive material.
Accompanying drawing explanation
Fig. 1 is the belt atmosphere sintering furnace structural representation of continuous seepage lithium iron phosphate positive material of the present invention.
Fig. 2 is the sectional view between cooling zone, and refrigerating unit is " returning " font watercooling jacket; Conveying belt is the plank frame of groove type.
Fig. 3 is the seal roll structural representation after amplifying.
Embodiment
Below in conjunction with accompanying drawing, the invention will be further described.
According to Fig. 1-Fig. 3, a kind of belt atmosphere sintering furnace of continuous seepage lithium iron phosphate positive material, comprising: the supporting mechanism 102 of body of heater 101 and support body of heater; It is characterized in that; also comprise the through burner hearth 103 being positioned at body of heater 101, the opening for feed 104 being positioned at body of heater side 106 and discharge port 105, the trolley type sealing mechanism 111 being arranged at body of heater side 106, the slat conveyer 107 through the band groove of through burner hearth 103, the cooling discharging device 109 being positioned at discharge port 105 front end, the shielding gas input being connected through burner hearth and gas pressure control device 108 and temperature-control device; opening for feed and discharge port all adopt trolley type sealing mechanism 111 to seal, and namely trolley type sealing mechanism is 2 groups.Temperature-control device comprises the structures such as temperature sensor, controller, heating unit.The opening for feed 104 of body of heater, discharge port 105 are arranged at the left and right sides of body of heater respectively.Leave the narrow gap that slat conveyer and lithium iron phosphate positive material can be allowed to pass through in trolley type sealing mechanism, opening for feed and discharge port are each passed through the narrow gap in trolley type sealing mechanism.
Belt atmosphere sintering furnace of the present invention, it is interval that its through burner hearth is divided into four segment process by three seals wall 110, temperature in each interval can control to adjust by PLC, and the heat treatment time of material then can realize controlling by the adjustment transfer rate of conveying belt and the length of each operation interval.In the present invention, the length between first paragraph process island is 1.5-2 rice, and temperature is 80-150 DEG C; Length between second segment process island is 2.5-3 rice, and temperature is 300-450 DEG C; 3rd segment process length of an interval degree is 6-8 rice, and temperature is 600-700 DEG C; 4th segment process interval is between cooling zone, and be provided with circulating water cooling device, length is 2.5-3.5 rice.
In order to prevent material oxidized in high-temperature zone, apparatus of the present invention should first vacuumize furnace chamber before work, and then pass into shielding gas, as highly purified nitrogen and argon gas.
In the present invention; because each operation interval of furnace chamber is separated by sealed wall; only leave the minimum gap allowing slat conveyer and lithium iron phosphate positive material to pass through; therefore operationally can be inputted by shielding gas and pressure control device adjusts the air pressure of each operation interval, to make it there are differences.Shielding gas pressure dependence in each interval of the furnace chamber of apparatus of the present invention is P2=P3>P1>P4>P0; namely the air pressure in hot operation district is greater than the air pressure in low-temperature working district, and the air pressure in burner hearth is greater than the air pressure outside burner hearth.Because the shielding gas in furnace chamber can only flow to low-pressure stage by high pressure section, burner hearth is interior, the shielding gas of cold zone enters high-temperature zone therefore just can effectively to prevent the air outside burner hearth from entering, thus reduces the oxidized probability of material.
The shielding gas input of apparatus of the present invention and gas pressure control device are made up of gas ducting, pump-line, electromagnetic valve and pressure transmitter; a magnetic valve is all equipped with wherein every bar gas ducting and pump-line; and utilize Y-junction to link together; pump-line and gas ducting are linked together by Y-junction; close the magnetic valve of pump-line during inflation operation, during operation of bleeding, then close the magnetic valve of gas ducting.When producing, the air pressure of each operation interval is detected by pressure transmitter, and is undertaken bleeding or inflating by PLC control system electromagnetic valve for adjusting door, accurately controls the air pressure of each operation interval.
Opening for feed 104, discharge port 105 place of body of heater are provided with trolley type sealing mechanism 111, and the seal roll in this mechanism operationally can be rotated along with travelling belt together, promote lithium iron phosphate positive material and enter sintering oven inside cavity.Seal roll is made up of (Fig. 3) hollow copper roller 112 and rubbery outer cover 113, is wherein provided with circulating water cooling system in hollow copper roller, and rubbery outer cover can be prevented at high temperature to be destroyed.The upper roller of sealing mechanism is connected with spring, can regulate height, make furnace chamber be in sealed state all the time during work according to the change of material thickness.The two ends of trolley type sealing mechanism are sealed in body of heater lateral inner, be made up of at least 2 rollers and the spring that is connected with upper roller (refer to and to be positioned at above conveying belt and material and that roller be close to conveying belt), according to lithium iron phosphate positive material thickness regulating spring height to regulate the height of upper roller, and then the distance between the adjacent rollers that have adjusted below upper roller and upper roller, make described distance only allow slat conveyer and lithium iron phosphate positive material to pass through, keep furnace chamber to be in sealed state all the time.Adjacent rollers below upper roller and upper roller, all fits with conveying belt part, operationally, can rotate together along with travelling belt, promotes lithium iron phosphate positive material and enters sintering oven inside cavity or by the discharging of sintering oven inside cavity.
The slat conveyer of apparatus of the present invention is made up of the monoblock type steel sheet with groove, during work, lithium iron phosphate positive material is directly transported in monoblock type steel-sheet groove by blanking system, conveying belt does not need the container holding material is installed, such trolley type sealing mechanism and three seals door only can stay and only hold slat conveyer and lithium iron phosphate positive material by small gaps, improve the sealing property of furnace chamber.Because conveying belt during work will bend to certain shape and be wrapped in power set, the steel plate therefore forming conveying belt must have good intensity and toughness, such as Steel Spring Plate, and the optimum thickness of steel plate is 10-50mm.
In order to prevent lithium iron phosphate positive material oxidized in atmosphere, cooling process must be carried out before discharging.Refrigerating unit of the present invention is " returning " font watercooling jacket (Fig. 2), and water jacket is welded by the copper coin that thermal conductivity is good.During work, water coolant is passed into by low side under the effect of recycle pump, high-end outflow, effectively reduces the drop temperature of material.
Embodiment 1
First the present embodiment adopts technology well known in the art to prepare ferric lithium phosphate precursor, is then adopted by ferric lithium phosphate precursor material belt atmosphere sintering furnace of the present invention to sinter under the protection of nitrogen.
(1) pre-treatment of persursor material: add in feed appliance by the speed of 50kg/h by ferric lithium phosphate precursor material, controls to be 100 DEG C by the temperature of the first operation interval, and protection air pressure P1 controls to be 1.05 standard atmospheric pressures, and the heat treated time is 3 hours;
(2) presintering of persursor material: pretreated ferric lithium phosphate precursor material is under the effect of conveying belt, enter the second operation interval, the pre-sintering temperature in this interval is 350 DEG C, and protection air pressure P1 controls to be 1.1 standard atmospheric pressures, and the presintering time is 5 hours;
(3) sintering of persursor material: the ferric lithium phosphate precursor material of presintering, under the effect of conveying belt, enters the 3rd operation interval, the sintering temperature in this interval is 700 DEG C, and protection air pressure P1 controls to be 1.1 standard atmospheric pressures, and sintering time is 12 hours;
(4) cooling of LiFePO 4 material and discharging: sintered LiFePO 4 material is under the effect of conveying belt; enter the 4th operation interval; carry out cooling fully and discharging, the protection air pressure in this interval controls to be 1.02 standard atmospheric pressures, a little more than the air pressure of outside.
Products obtained therefrom through pulverizing, sieving, sample preparation testing, cell container reaches 158mA/h(0.2C).
Embodiment 2
Other operations of the present embodiment are with embodiment 1, and difference is: the sintering temperature of the 3rd operation interval is 600 DEG C.
The present embodiment products obtained therefrom through pulverizing, sieving, sample preparation testing, cell container reaches 155mA/h(0.2C).
Comparative example 1
The pre-treatment of this comparative example, presintering and sintering process parameter (temperature, air pressure, treatment time) are identical with embodiment 1, and difference is: the equipment of employing is atmosphere protection clock hood type furnace, and processing mode is intermittent type process.
This comparative example products obtained therefrom through pulverizing, sieving, sample preparation testing, cell container reaches 157mA/h(0.2C).
The result explanation of above-described embodiment and comparative example; the performance of the LiFePO 4 material that continuous sintering furnace of the present invention is produced is not weaker than the atmosphere protection clock hood type furnace of intermittent type process; but its production efficiency is apparently higher than atmosphere protection clock hood type furnace, there is very strong practicality.
More than show and describe ultimate principle of the present invention, principal character and advantage.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (9)
1. a belt atmosphere sintering furnace for continuous seepage lithium iron phosphate positive material, comprising: the supporting mechanism (102) of body of heater (101) and support body of heater, it is characterized in that, also comprise the through burner hearth (103) being positioned at body of heater (101), be positioned at opening for feed (104) and the discharge port (105) of body of heater side (106), be arranged at the trolley type sealing mechanism (111) of body of heater side (106), through the slat conveyer (107) of the band groove of through burner hearth (103), be positioned at the cooling discharging device (109) of discharge port (105) front end, connect shielding gas input and gas pressure control device (108) and the temperature-control device of through burner hearth, opening for feed and discharge port all adopt trolley type sealing mechanism (111) to seal, wherein, it is interval that through burner hearth is divided into four segment process by three seals wall (110), the working temperature in each interval and the air pressure of shielding gas there are differences, and each sealed wall leaves narrow gap, and described gap only allows slat conveyer and lithium iron phosphate positive material to pass through.
2. the belt atmosphere sintering furnace of a kind of continuous seepage lithium iron phosphate positive material according to claim 1, it is characterized in that: the length between first paragraph process island is 1.5-2 rice, temperature is 80-150 DEG C, and shielding gas pressure is P1; Length between second segment process island is 2.5-3 rice, and temperature is 300-450 DEG C, and shielding gas pressure is P2; 3rd segment process length of an interval degree is 6-8 rice, and temperature is 600-700 DEG C, and shielding gas pressure is P3; 4th segment process interval is between cooling zone, and be provided with circulating water cooling device, length is 2.5-3.5 rice, and shielding gas pressure is P4; Wherein, the shielding gas pressure in each interval is all a little more than standard atmospheric pressure P0, and the mutual relationship between four is: P2=P3>P1>P4.
3. the belt atmosphere sintering furnace of a kind of continuous seepage lithium iron phosphate positive material according to claim 1, it is characterized in that: described opening for feed and discharge port lay respectively at the both sides of body of heater, leave the narrow gap that slat conveyer and lithium iron phosphate positive material can be allowed to pass through in trolley type sealing mechanism, opening for feed and discharge port are each passed through the narrow gap in trolley type sealing mechanism.
4. the belt atmosphere sintering furnace of a kind of continuous seepage lithium iron phosphate positive material according to claim 3, it is characterized in that: the roller of described trolley type sealing mechanism is made up of the rubbery outer cover (113) of hollow copper roller (112) and parcel hollow copper rod, and hollow copper roller inside is passed through for recirculated cooling water.
5. the belt atmosphere sintering furnace of a kind of continuous seepage lithium iron phosphate positive material according to claim 1 or 3 or 4, it is characterized in that: trolley type sealing mechanism is made up of at least 2 rollers and the spring that is connected with upper roller, according to lithium iron phosphate positive material thickness regulating spring height to regulate the distance between the adjacent rollers below upper roller, upper roller, make described distance only allow slat conveyer and lithium iron phosphate positive material to pass through, keep furnace chamber to be in sealed state all the time.
6. the belt atmosphere sintering furnace of a kind of continuous seepage lithium iron phosphate positive material according to claim 1, it is characterized in that: the slat conveyer of sintering oven is made up of the monoblock type steel sheet with groove, lithium iron phosphate positive material is positioned in groove, and conveying belt completes the transportation work of lithium iron phosphate positive material under the effect of power transmission.
7. the belt atmosphere sintering furnace of a kind of continuous seepage lithium iron phosphate positive material according to claim 1, is characterized in that: the slat conveyer of sintering oven only has one to be arranged in through burner hearth, and another is positioned at burner hearth outside.
8. the belt atmosphere sintering furnace of a kind of continuous seepage lithium iron phosphate positive material according to claim 1, is characterized in that: the monoblock type steel sheet thickness of composition slat conveyer is 10-50mm, and material is spring steel.
9. the belt atmosphere sintering furnace of a kind of continuous seepage lithium iron phosphate positive material according to claim 1; it is characterized in that: the temperature-control device of sintering oven, shielding gas input and gas pressure control device adopts PLC to control; the temperature of each operation interval of real-time monitoring and gaseous tension, and can adjust the temperature of operation interval and pressure.
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| CN201510607178.7A CN105129762B (en) | 2015-09-22 | 2015-09-22 | Belt-type atmosphere sintering furnace for continuous production of lithium iron phosphate cathode material |
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| CN201510607178.7A CN105129762B (en) | 2015-09-22 | 2015-09-22 | Belt-type atmosphere sintering furnace for continuous production of lithium iron phosphate cathode material |
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| CN105129762B CN105129762B (en) | 2017-04-19 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107146908A (en) * | 2016-12-08 | 2017-09-08 | 芜湖恒尼动力电池材料科技有限公司 | A kind of li-ion electrode materials carbon coating continuous apparatus |
| CN109579517A (en) * | 2019-01-21 | 2019-04-05 | 南京工程学院 | A kind of screw propulsion atmosphere sintering furnace producing ternary lithium electric material |
| CN110057193A (en) * | 2019-05-06 | 2019-07-26 | 株洲瑞德尔冶金设备制造有限公司 | A kind of integrated sintering furnace of continous way |
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| CN1474926A (en) * | 2000-11-17 | 2004-02-11 | ���п�ķ�����Ϲɷݹ�˾ | Device for continuously operated belt sintering |
| CN202057166U (en) * | 2010-12-07 | 2011-11-30 | 邹少华 | Pushing-in device of high-conductivity lithium iron phosphate sintering furnace |
| CN204958405U (en) * | 2015-09-22 | 2016-01-13 | 南京工程学院 | Continuous production lithium iron phosphate cathode material's belt atmosphere sintering stove |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1474926A (en) * | 2000-11-17 | 2004-02-11 | ���п�ķ�����Ϲɷݹ�˾ | Device for continuously operated belt sintering |
| CN202057166U (en) * | 2010-12-07 | 2011-11-30 | 邹少华 | Pushing-in device of high-conductivity lithium iron phosphate sintering furnace |
| CN204958405U (en) * | 2015-09-22 | 2016-01-13 | 南京工程学院 | Continuous production lithium iron phosphate cathode material's belt atmosphere sintering stove |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107146908A (en) * | 2016-12-08 | 2017-09-08 | 芜湖恒尼动力电池材料科技有限公司 | A kind of li-ion electrode materials carbon coating continuous apparatus |
| CN109579517A (en) * | 2019-01-21 | 2019-04-05 | 南京工程学院 | A kind of screw propulsion atmosphere sintering furnace producing ternary lithium electric material |
| CN109579517B (en) * | 2019-01-21 | 2023-11-21 | 南京工程学院 | Spiral propelling atmosphere sintering furnace for producing ternary lithium battery material |
| CN110057193A (en) * | 2019-05-06 | 2019-07-26 | 株洲瑞德尔冶金设备制造有限公司 | A kind of integrated sintering furnace of continous way |
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| CN105129762B (en) | 2017-04-19 |
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