CN105129762B - 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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- CN105129762B CN105129762B CN201510607178.7A CN201510607178A CN105129762B CN 105129762 B CN105129762 B CN 105129762B CN 201510607178 A CN201510607178 A CN 201510607178A CN 105129762 B CN105129762 B CN 105129762B
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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, and in particular to a kind of continuous production iron phosphate lithium positive pole material
The belt atmosphere sintering furnace of material.
Background technology
LiFePO 4 material is as with having a safety feature, discharge-rate is high, cycle performance is excellent, use temperature range
The advantages of width, life-span length, environmental protection, since the advent of the world just gets more and more people's extensive concerning, and is expected in electric automobile and portable
It is widely used in formula electronic equipment.In recent years, as country increasingly payes attention to environmental issue, especially 2011 years with
Carry out the reasons such as the regulation to lead-acid storage battery production, promote developing rapidly for power ferric phosphate lithium cell industry.But, by
Complicated process of preparation, production equipment in LiFePO 4 material are immature, technical threshold is higher, therefore industrialization speed is slower,
Limit its further popularization and application.
At present, the preparation of LiFePO 4 material mainly adopts high-temperature solid phase reaction method, the temperature of heat treatment to be up to 600-800
℃.At this temperature, in material ferrous ion is easy to oxidation, causes the hydraulic performance decline of material.Therefore, in order to prevent phosphoric acid
Ferrum lithium material is oxidized in production process, and domestic enterprise is essentially all using step Equipment for Heating Processing, such as：Atmosphere protection
Batch-type furnace, atmosphere protection clock hood type furnace etc., significantly limit the production efficiency of material.In recent years, some domestic device fabrications
Business attempts exploitation and can be used to continuously produce the pushed bat kiln of LiFePO 4 material, meshbeltfurnace, rotary kiln, and in some production iron phosphate
The enterprise of lithium material is tried out, and achieves some results, but in terms of stability and the concordance of material property with interval
The Equipment for Heating Processing of formula still differs greatly.Meanwhile, also there are some equipment with regard to continuous production LiFePO 4 material at present
The patent of patent, such as Patent No. CN201587859 describes a kind of horizontal continuous production of LiFePO 4 material microwave heating and sets
It is standby；The patent of Patent No. CN102092699 describes a kind of ferric lithium phosphate precursor sintering and prepares LiFePO4 method and micro-
Ripple agglomerating plant；The patent of Patent No. CN201971642U describes a kind of height and leads lithium iron phosphate sintering device.But, it is above-mentioned
Various equipment involved by patent, however it remains some defects, it is difficult to ensure to take into account while production efficiency in actual production
The stability and concordance of material.
The content of the invention
The present invention cannot take into account the deficiency of production efficiency and properties of product for existing LiFePO 4 material production equipment, carry
For a kind of temperature control accurately, low oxygen content can be with the belt atmosphere sintering furnace of continuous way production lithium iron phosphate positive material.
In order to realize foregoing invention purpose, the present invention is adopted the following technical scheme that：A kind of continuous production iron phosphate lithium positive pole
The belt atmosphere sintering furnace of material, including：The supporting mechanism of body of heater and support body of heater；Characterized in that, also including positioned at body of heater
Interior through burner hearth, charging aperture and discharging opening positioned at body of heater side, the roller type sealing mechanism for being arranged at body of heater side, wear
Cross the slat conveyer with groove of through burner hearth, the cooling discharging device positioned at discharging opening front end and connect through burner hearth
Protective gas is input into and gas pressure control device and temperature control equipment, and charging aperture and discharging opening adopt roller type sealer
Structure is sealed；Wherein, through burner hearth is divided into four segment process interval, each interval operating temperature and shielding gas by three seals wall
The air pressure of body has differences, and narrow gap is left on each envelope wall, and described gap only allows slat conveyer and LiFePO4
Positive electrode passes through.
A kind of belt atmosphere sintering furnace of aforesaid continuous production lithium iron phosphate positive material, first paragraph technique length of an interval
Spend for 1.5-2 rice, temperature is 80-150 DEG C, protective gas pressure is P1；The interval length of second segment technique is 2.5-3 rice, warm
Spend for 300-450 DEG C, protective gas pressure is P2；3rd segment process length of an interval degree is 6-8 rice, and temperature is 600-700 DEG C, is protected
Shield gas pressure is P3；4th segment process is interval interval for cooling, is provided with circulating water cooling device, and length is 2.5-3.5 rice, is protected
Shield gas pressure is P4；Wherein, each interval protective gas pressure is slightly above normal atmosphere P0, and mutual between four
Relation is：P2=P3>P1>P4.
A kind of belt atmosphere sintering furnace of aforesaid continuous production lithium iron phosphate positive material, the charging aperture and discharging opening
Respectively positioned at the both sides of body of heater, leave in roller type sealing mechanism and slat conveyer and lithium iron phosphate positive material can be allowed to pass through
Narrow gap, charging aperture and discharging opening are each passed through the narrow gap in roller type sealing mechanism.
A kind of belt atmosphere sintering furnace of aforesaid continuous production lithium iron phosphate positive material, described roller type sealer
The roller of structure is made up of the rubbery outer cover of hollow copper roller and parcel hollow copper rod, is passed through for recirculated cooling water inside hollow copper roller.
A kind of belt atmosphere sintering furnace of aforesaid continuous production lithium iron phosphate positive material, roller type sealing mechanism is by extremely
Few 2 rollers and spring composition be connected with upper roller, according to lithium iron phosphate positive material thickness adjusted spring heights with
Adjust the distance between upper roller, adjacent rollers below upper roller, make described distance only allow slat conveyer and
Lithium iron phosphate positive material passes through, and keeps furnace chamber to be in sealing state all the time.
A kind of belt atmosphere sintering furnace of aforesaid continuous production lithium iron phosphate positive material, the slat conveyer of sintering furnace
It is made up of monoblock type sheet metal with groove, lithium iron phosphate positive material is positioned in groove, and conveyer belt is in power transmission
In the presence of complete the transportation work of lithium iron phosphate positive material.
A kind of belt atmosphere sintering furnace of aforesaid continuous production lithium iron phosphate positive material, the slat conveyer of sintering furnace
Only one is located in through burner hearth, and another is located at outside burner hearth.
A kind of belt atmosphere sintering furnace of aforesaid continuous production lithium iron phosphate positive material, constitutes the whole of slat conveyer
Body formula sheet metal thickness is 10-50mm, and material is spring steel.
A kind of belt atmosphere sintering furnace of aforesaid continuous production lithium iron phosphate positive material, the temperature control dress of sintering furnace
Put, protective gas input and gas pressure control device are controlled using PLC, the temperature and gas pressure of each operation interval of monitor in real time
Power, it is possible to which the temperature and pressure of operation interval are adjusted.
The invention has the beneficial effects as follows：Apparatus of the present invention are belt atmosphere sintering furnace, employ monoblock type with groove thin
Steel plate is used as conveyer belt, it is possible to achieve the production of continuous way, not only efficiency high, and can reduce the quantity of operator, section
About labor cost；The sealing mechanism of uniqueness is present invention employs, the sealing of furnace chamber not only can be realized, and can be by not
The interval oxygen content of hot operation is further reduced with the draught head of operation interval, improves the performance of material.Apparatus of the present invention are made
For a kind of continuous production equipment for taking into account production efficiency and material property, the scale metaplasia in lithium iron phosphate positive material is expected to
It is widely used in product.
Description of the drawings
Fig. 1 is the belt atmosphere sintering furnace structural representation of the continuous production lithium iron phosphate positive material of the present invention.
Fig. 2 is the interval profile of cooling, and chiller is " returning " font cooling jacket；Conveyer belt is board-like for groove type
Structure.
Fig. 3 is the seal roll structural representation after amplifying.
Specific embodiment
The invention will be further described below in conjunction with the accompanying drawings.
According to Fig. 1-Fig. 3, a kind of belt atmosphere sintering furnace of continuous production lithium iron phosphate positive material, including：Body of heater 101
And support the supporting mechanism 102 of body of heater；Characterized in that, also include the through burner hearth 103 in body of heater 101, positioned at stove
The charging aperture 104 and discharging opening 105 of body side surface 106, be arranged at the roller type sealing mechanism 111 of body of heater side 106, through insertion
The slat conveyer with groove 107 of formula burner hearth 103, the cooling discharging device 109 positioned at 105 front end of discharging opening, connection insertion
The protective gas input of formula burner hearth and gas pressure control device 108 and temperature control equipment, charging aperture and discharging opening are adopted
Roller type sealing mechanism 111 is sealed, i.e., roller type sealing mechanism is 2 groups.Temperature control equipment includes temperature sensor, control
The structures such as device, heater.The charging aperture 104 of body of heater, discharging opening 105 are respectively arranged at the left and right sides of body of heater.Roller type is close
The narrow gap that slat conveyer and lithium iron phosphate positive material can be allowed to pass through, charging aperture and discharging opening point are left in sealing mechanism
Narrow gap that Chuan Guo be in roller type sealing mechanism.
Belt atmosphere sintering furnace of the present invention, its through burner hearth are divided into four segment process by three seals wall 110
Interval, the temperature in each interval can be adjusted by PLC controls, and the heat treatment time of material then can be defeated by adjusting
The length of transfer rate and each operation interval of band is sent realizing control.In the present invention, the interval length of first paragraph technique is
1.5-2 rice, temperature are 80-150 DEG C；The interval length of second segment technique is 2.5-3 rice, and temperature is 300-450 DEG C；3rd section of work
Skill length of an interval degree is 6-8 rice, and temperature is 600-700 DEG C；4th segment process is interval interval for cooling, is provided with circulating water dress
Put, length is 2.5-3.5 rice.
In order to prevent material to be oxidized in high-temperature region, apparatus of the present invention should first to furnace chamber evacuation, Ran Houzai before work
Protective gas is passed through, such as highly purified nitrogen and argon.
In the present invention, as each operation interval of furnace chamber is separated by envelope wall, permission slat conveyer and phosphoric acid are only left
The minimum gap that ferrum lithium anode material passes through, therefore operationally can be adjusted by protective gas input and pressure control device
The air pressure of whole each operation interval, is allowed to have differences.Protective gas pressure in each interval of furnace chamber of apparatus of the present invention is closed
It is for P2=P3>P1>P4>The air pressure of P0, the i.e. air pressure in hot operation area more than low-temperature working area, the air pressure in burner hearth are more than stove
Air pressure outside thorax.As the protective gas in furnace chamber can only flow to low pressure stage by high pressure section, therefore just effectively can prevent
Air outside burner hearth is entered in burner hearth, the protective gas of low-temperature space enters high-temperature region, so as to reduce the probability that material is oxidized.
The protective gas input of apparatus of the present invention and gas pressure control device are by aerating pipe, pump-line, electromagnetic valve
Door and pressure transducer are constituted, wherein being respectively arranged with an electromagnetic valve on every aerating pipe and pump-line, and utilize threeway
Joint links together, and pump-line is linked together by three way cock with aerating pipe, closes exhaust tube during inflation operation
The electromagnetic valve in road, then cuts out the electromagnetic valve of aerating pipe when being evacuated operation.In production, the air pressure of each operation interval is by pressure
Sensor detects, and by PLC control system electromagnetic valve for adjusting door being evacuated or be inflated, the gas of each operation interval of precise control
Pressure.
Roller type sealing mechanism 111 is provided with the charging aperture 104 of body of heater, discharging opening 105, the seal roll in the mechanism exists
Can be rotated with conveyer belt together during work, promote lithium iron phosphate positive material to enter sintering furnace inside cavity.Seal roll
It is made up of hollow copper roller 112 and rubbery outer cover 113（Fig. 3）, wherein circulating water cooling system is provided with hollow copper roller, can prevent
Rubbery outer cover is destroyed at high temperature.The upper roller of sealing mechanism is connected with spring, can be according to the change of material thickness during work
Change to adjust height, make furnace chamber be in sealing state all the time.The two ends of roller type sealing mechanism are sealed in body of heater lateral inner, by
At least 2 rollers and and upper roller（Refer to above conveyer belt and material and with conveyer belt close to that roller）Even
The spring for connecing is constituted, and according to lithium iron phosphate positive material thickness adjusted spring heights to adjust the height of upper roller, and then is adjusted
Saved the distance between adjacent rollers below upper roller and upper roller, make described distance only allow slat conveyer and
Lithium iron phosphate positive material passes through, and keeps furnace chamber to be in sealing state all the time.Upper roller and the adjacent rolling below upper roller
Wheel, is fitted with conveyer belt part, operationally, can be rotated with conveyer belt together, promotes lithium iron phosphate positive material to enter
Enter sintering furnace inside cavity or discharged by sintering furnace inside cavity.
The slat conveyer of apparatus of the present invention is made up of monoblock type sheet metal with groove, during work, iron phosphate lithium positive pole
Material is directly transported in monoblock type steel-sheet groove by blanking system, is not required to install the container for holding material on conveyer belt,
So can leave behind on roller type sealing mechanism and three seals door and only hold slat conveyer and lithium iron phosphate positive material is logical
Small gaps are crossed, the sealing property of furnace chamber is improve.As during work, conveyer belt will bend to certain shape and be wrapped in dynamic
On power apparatus, therefore the steel plate of composition conveyer belt must have good intensity and toughness, such as steel spring plate, and steel plate is most
Good thickness is 10-50mm.
In order to prevent lithium iron phosphate positive material to be oxidized in atmosphere, it is necessary to cooling treatment is carried out before discharging.This
Bright chiller is " returning " font cooling jacket（Fig. 2）, water jacket is welded by the good copper coin of heat conductivity.It is during work, cold
But water is passed through by low side in the presence of circulating pump, high-end outflow, effectively reduces the drop temperature of material.
Embodiment 1
The present embodiment prepares ferric lithium phosphate precursor initially with technology well known in the art, then by before LiFePO4
Drive body material to be sintered under the protection of nitrogen using belt atmosphere sintering furnace of the present invention.
（1）The pretreatment of persursor material：The speed that ferric lithium phosphate precursor material presses 50kg/h is added in feed appliance,
It it is 100 DEG C by the temperature control of the first operation interval, protection air pressure P1 is controlled to 1.05 normal atmospheres, the time of heat treatment
For 3 hours；
（2）The presintering of persursor material：Pretreated ferric lithium phosphate precursor material enters in the presence of conveyer belt
Enter the second operation interval, the interval pre-sintering temperature is 350 DEG C, protection air pressure P1 is controlled to 1.1 normal atmospheres, pre-burning
The knot time is 5 hours；
（3）The sintering of persursor material：The ferric lithium phosphate precursor material of presintering is entered in the presence of conveyer belt
3rd operation interval, the interval sintering temperature are 700 DEG C, and protection air pressure P1 is controlled to 1.1 normal atmospheres, sintering time
For 12 hours；
（4）The cooling and discharging of LiFePO 4 material：Sintered LiFePO 4 material is entered in the presence of conveyer belt
4th operation interval, is sufficiently cooled and discharges, and the interval shielding gas is voltage-controlled to be made as 1.02 normal atmospheres, slightly higher
In outside air pressure.
Products obtained therefrom is size-reduced, sieve, sample preparation test, and battery capacity reaches 158mA/h（0.2C）.
Embodiment 2
The present embodiment other operation with embodiment 1, difference is：The sintering temperature of the 3rd operation interval is 600 DEG C.
The present embodiment products obtained therefrom is size-reduced, sieve, sample preparation test, and battery capacity reaches 155mA/h（0.2C）.
Comparative example 1
The pretreatment of this comparative example, presintering and sintering process parameter（Temperature, air pressure, process time）It is same as Example 1,
Difference is：The equipment for adopting is atmosphere protection clock hood type furnace, and processing mode is batch (-type) process.
This comparative example products obtained therefrom is size-reduced, sieve, sample preparation test, and battery capacity reaches 157mA/h（0.2C）.
The result explanation of above-described embodiment and comparative example, the LiFePO4 material of continuous sintering furnace production of the present invention
The performance of material is not weaker than the atmosphere protection clock hood type furnace of batch (-type) process, but its production efficiency is apparently higher than atmosphere protection bell jar
Stove, with very strong practicality.
Ultimate principle, principal character and the advantage of the present invention has been shown and described above.The technical staff of the industry should
Understand, the present invention is not restricted to the described embodiments, the original for simply illustrating the present invention described in above-described embodiment and description
Reason, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, these changes and improvements
Both fall within scope of the claimed invention.The claimed scope of the invention is by appending claims and its equivalent circle.
It is fixed.
Claims (8)
1. it is a kind of it is continuous production lithium iron phosphate positive material belt atmosphere sintering furnace, including：Body of heater（101）And support body of heater
Supporting mechanism（102）；Characterized in that, also including positioned at body of heater（101）Interior through burner hearth（103）, positioned at body of heater side
（106）Charging aperture（104）And discharging opening（105）, be arranged at body of heater side（106）Roller type sealing mechanism（111）, pass through
Through burner hearth（103）Slat conveyer with groove（107）, positioned at discharging opening（105）The cooling discharging device of front end
（109）, connect protective gas input and the gas pressure control device of through burner hearth（108）And temperature control equipment, charging
Mouth and discharging opening adopt roller type sealing mechanism（111）Sealing；Wherein, through burner hearth is by three seals wall（110）Divide
Interval for four segment process, the air pressure of each interval operating temperature and protective gas has differences, and narrow seam is left on each envelope wall
Gap, described gap only allow slat conveyer and lithium iron phosphate positive material to pass through；The interval length of first paragraph technique is
1.5-2 rice, temperature are 80-150 DEG C, and protective gas pressure is P1；The interval length of second segment technique is 2.5-3 rice, and temperature is
300-450 DEG C, protective gas pressure is P2；3rd segment process length of an interval degree is 6-8 rice, and temperature is 600-700 DEG C, shielding gas
Body pressure is P3；4th segment process is interval interval for cooling, is provided with circulating water cooling device, and length is 2.5-3.5 rice, shielding gas
Body pressure is P4；Wherein, each interval protective gas pressure is slightly above normal atmosphere P0, and the mutual relation between four
For：P2=P3>P1>P4.
2. it is according to claim 1 it is a kind of it is continuous production lithium iron phosphate positive material belt atmosphere sintering furnace, its feature
It is：The charging aperture and discharging opening are left in roller type sealing mechanism and can allow board-like conveying respectively positioned at the both sides of body of heater
The narrow gap that band and lithium iron phosphate positive material pass through, charging aperture and discharging opening are each passed through narrow in roller type sealing mechanism
Narrow slot.
3. it is according to claim 2 it is a kind of it is continuous production lithium iron phosphate positive material belt atmosphere sintering furnace, its feature
It is：The roller of described roller type sealing mechanism is by hollow copper roller（112）And the rubbery outer cover of parcel hollow copper rod（113）Group
Into passing through for recirculated cooling water inside hollow copper roller.
4. according to claim 1 or 2 or 3 it is a kind of continuous production lithium iron phosphate positive material belt atmosphere sintering furnace,
It is characterized in that：The spring that roller type sealing mechanism is connected by least 2 rollers and with upper roller is constituted, according to iron phosphate
Lithium anode material thickness adjusted spring heights are made with adjusting the distance between adjacent rollers below upper roller, upper roller
Described distance only allows slat conveyer and lithium iron phosphate positive material to pass through, and keeps furnace chamber to be in sealing state all the time.
5. it is according to claim 1 it is a kind of it is continuous production lithium iron phosphate positive material belt atmosphere sintering furnace, its feature
It is：The slat conveyer of sintering furnace is made up of monoblock type sheet metal with groove, and lithium iron phosphate positive material is positioned over groove
Interior, conveyer belt completes the transportation work of lithium iron phosphate positive material in the presence of power transmission.
6. it is according to claim 1 it is a kind of it is continuous production lithium iron phosphate positive material belt atmosphere sintering furnace, its feature
It is：The slat conveyer of sintering furnace only has one to be located in through burner hearth, and another is located at outside burner hearth.
7. it is according to claim 1 it is a kind of it is continuous production lithium iron phosphate positive material belt atmosphere sintering furnace, its feature
It is：The monoblock type sheet metal thickness of composition slat conveyer is 10-50mm, and material is spring steel.
8. it is according to claim 1 it is a kind of it is continuous production lithium iron phosphate positive material belt atmosphere sintering furnace, its feature
It is：The temperature control equipment of sintering furnace, protective gas are input into and gas pressure control device is controlled using PLC, monitor in real time
The temperature and gas pressure of each operation interval, it is possible to which the temperature and pressure of operation interval are adjusted.
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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 true CN105129762B (en) | 2017-04-19 |
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Families Citing this family (3)
| 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 |
| 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 |
| CN110057193B (en) * | 2019-05-06 | 2019-12-27 | 株洲瑞德尔冶金设备制造有限公司 | Continuous integrated sintering furnace |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2015
- 2015-09-22 CN CN201510607178.7A patent/CN105129762B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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