WO2015139527A1 - 磷酸铁锂连续制备装置 - Google Patents

磷酸铁锂连续制备装置 Download PDF

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WO2015139527A1
WO2015139527A1 PCT/CN2015/070980 CN2015070980W WO2015139527A1 WO 2015139527 A1 WO2015139527 A1 WO 2015139527A1 CN 2015070980 W CN2015070980 W CN 2015070980W WO 2015139527 A1 WO2015139527 A1 WO 2015139527A1
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continuous
iron phosphate
lithium iron
reaction tube
reaction
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PCT/CN2015/070980
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English (en)
French (fr)
Inventor
何向明
王莉
罗晶
李建军
张建利
徐程浩
尚玉明
高剑
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江苏华东锂电技术研究院有限公司
清华大学
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Publication of WO2015139527A1 publication Critical patent/WO2015139527A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/16—Oxyacids of phosphorus; Salts thereof
    • C01B25/26—Phosphates
    • C01B25/45—Phosphates containing plural metal, or metal and ammonium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the utility model relates to a continuous preparation device of lithium iron phosphate.
  • lithium-ion batteries have been widely used in consumer electronic products such as notebook computers, mobile phones, and video cameras.
  • Lithium iron phosphate has been receiving great attention as a positive active material for lithium ion batteries with good safety, low cost and environmental friendliness.
  • the synthesis methods of lithium iron phosphate in the laboratory mainly include high temperature solid phase method, spray method, hydrothermal synthesis method, coprecipitation method, emulsion drying method and microwave synthesis method.
  • lithium iron phosphate is mainly synthesized on a large scale by a high temperature solid phase method.
  • the high-temperature solid-phase method requires sintering at a relatively high temperature, and the product has a large particle size and poor performance.
  • Hydrothermal synthesis and solvothermal synthesis are methods for synthesizing lithium iron phosphate of smaller size grains at lower temperatures.
  • a lithium iron phosphate preparation device comprises a continuous preparation device of lithium iron phosphate, comprising a raw material tank, a reaction kettle, an intermediate pump, a continuous reaction tube, a product storage tank and a gas input device, wherein the inlet of the reaction kettle is sealed a pipeline is connected to the raw material tank, and the intermediate pump is respectively connected to the discharge port of the reaction kettle and the continuous reaction tube through a closed pipeline, so that the material is continuously transported from the reactor to the continuous reaction tube, and Outputted to the product storage tank, one end of the continuous reaction tube is connected to the intermediate pump, and the other end is connected to the product storage tank through a closed pipeline, and the gas input device is respectively sealed with the reaction kettle and the product storage tank
  • the lines are connected to maintain a predetermined reaction pressure in the reaction vessel and the continuous reaction tube.
  • the utility model divides the original reaction kettle of the hydrothermal synthesis method into two parts, namely, a stirring reaction device and a constant temperature reaction device, and supplies the pressure required by the two devices through the gas input device, so that the raw materials continuously pass through the two
  • the device can realize the continuous reaction to produce lithium iron phosphate during the operation of the material, and can realize large-scale industrial continuous production of the product, and greatly improve the consistency of the lithium iron phosphate product.
  • FIG. 1 is a schematic view showing the structure of a continuous preparation device of lithium iron phosphate according to an embodiment of the present invention.
  • Lithium iron phosphate continuous preparation device 1 Raw material tank 10 Metering pumps 12 Reactor 20 Heating jacket twenty two Blender twenty four Frequency converter 26 Discharge valve 28 Thermocouple 30 Intermediate pump 40 Continuous reaction tube 50 Constant temperature oil bath 52 Heater 54 Gas input device 60 Pressure gas tank 62 filter 64 Pressure reducing valve 66 Check valve 68 Ball valve 70 Pressure detecting device 80 Product storage tank 90 Back pressure valve 92
  • the present invention provides a lithium iron phosphate continuous preparation device 1 for continuously preparing lithium iron phosphate by hydrothermal synthesis or solvothermal synthesis, and the lithium iron phosphate continuous preparation device 1 comprises a raw material tank 10 .
  • the mixing agitation device, the intermediate pump 40, the thermostatic reaction device, the product storage tank 90, and the gas input device 60 are used to continuously prepare lithium iron phosphate by hydrothermal synthesis or solvothermal synthesis.
  • the raw material tank 10 is used for storing a raw material solution of hydrothermal synthesis or solvothermal synthesis of lithium iron phosphate.
  • This embodiment includes two raw material tanks 10, wherein one raw material tank 10 stores a ferrous phosphate solution, and the other raw material tank 10 stores phosphoric acid and A solution after the lithium hydroxide reaction.
  • the mixing agitation device is used to mix the raw material solutions and uniformly mix them at a predetermined temperature and pressure.
  • the mixing and agitating device includes a reaction vessel 20, a heating jacket 22, and a stirrer 24.
  • the feed port of the reaction vessel 20 is connected to the raw material tank 10 through a closed line, and a metering pump 12 can be further disposed on the closed line between the raw material tank 10 and the reaction vessel 20 at a working pressure of 0 to 2 MPa.
  • the raw material solution is transferred to the reaction vessel 20 and the ratio between the raw material solutions delivered from the different raw material tanks 10 is controlled.
  • the agitator 24 is disposed inside the reaction vessel 20, and specifically may be a stirring rod with a stirring slurry.
  • the agitator 24 may be connected to an electric control device disposed outside the reaction vessel 20.
  • the electric control device may have a frequency converter 26 for The rotation speed of the agitator 24 is adjusted, and the rotation speed can be 0 to 200 rpm.
  • the heating jacket 22 is disposed outside the reactor 20 for heating and holding the reactor 20, and specifically may be disposed around the outer wall of the reactor 20.
  • the mixing and agitating device may further include a pyrometer, such as a thermocouple 30, for measuring the temperature inside the reactor 20.
  • the mixing and agitating device mainly performs uniform mixing of the raw material solution, and in the mixing and stirring device, the raw material solution may not undergo a chemical reaction.
  • the raw material solution may start to undergo a chemical reaction in the mixing and agitating device, that is, a reaction of hydrothermal or solvothermal synthesis of lithium iron phosphate.
  • the working temperature inside the reaction vessel 20 can be 25 to 250 ° C
  • the working pressure can be 0 to 1.6 MPa
  • the volume can be 10 L to 20 L.
  • the discharge port of the reaction vessel 20 may be located at the bottom or side wall of the reaction vessel 20. When located at the side wall of the reaction vessel 20, the centrifugal force generated by the agitation of the agitator 24 may cause the reacted material to exit the side wall.
  • the material overflows, and when it is located at the bottom of the reaction vessel 20, the material naturally flows out by gravity.
  • the reactor 20 may further include a discharge valve 28 disposed at the discharge port for controlling the discharge of materials inside the reaction vessel 20.
  • the reactor 20 can be further provided with an exhausting means such as a needle valve for controlling the internal pressure of the reactor 20 to be within a predetermined interval.
  • the thermostatic reaction apparatus includes a constant temperature oil bath 52 and a continuous reaction tube 50 disposed in the constant temperature oil bath 52.
  • the constant temperature reaction device is configured to heat the material passing through the continuous reaction tube 50 under a predetermined pressure, and the material is passed through the entire continuous reaction tube 50 in a constant temperature and constant pressure state, thereby performing a hydrothermal or solvothermal reaction.
  • the pressure in the continuous reaction tube 50 is regulated by the gas input device 60.
  • the continuous reaction tube 50 has a sufficient length to allow the material to stay in the continuous reaction tube 50 for a sufficiently long period of time. Specifically, the residence time of the material in the continuous reaction tube 50 may be 2 hours to 6 hours.
  • the length of the continuous reaction tube 50 may be 10 meters to 20 meters, and the inner diameter may be 5 mm to 20 mm.
  • the continuous reaction tube 50 can be flexibly disposed in the constant temperature oil bath 52 to save space.
  • the constant temperature oil bath 52 is heated by the heater 54 to make the internal oil temperature uniform and constant, and the operating temperature range of the constant temperature oil bath 52 can be 5 to 250 °C.
  • the thermostatic reaction apparatus may further include a thermometer, such as a thermocouple 30, for measuring the temperature of the oil inside the constant temperature oil bath 52 and the temperature of the heater 54.
  • the intermediate pump 40 is disposed between the reaction vessel 20 and the continuous reaction tube 50, and is connected to the discharge port of the reaction vessel 20 and the continuous reaction tube 50 through a closed line.
  • the intermediate pump 40 is used for continuously inputting the material in the reaction kettle 20 into the continuous reaction tube 50, and precisely adjusting the material flow rate, so that the time during which the material stays through the continuous reaction tube 50 is controllable, and finally passes through the continuous reaction tube. 50 output to the product storage tank.
  • the intermediate pump 40 can be a diaphragm pump, the rated flow rate can be 0 ⁇ 2 liters/hour, and the flow rate can be adjusted by the frequency converter, and the outlet pressure can be 0 ⁇ 2 MPa.
  • One end of the continuous reaction tube 50 is connected to the reaction vessel 20 through an intermediate pump 40, and the other end is connected to a product storage tank 90.
  • the pressure in the reaction vessel 20 and the continuous reaction tube 50 can be adjusted by the gas input device 60, respectively, so that they can be the same or different.
  • the gas input device 60 is connected to the reaction vessel 20 and the product storage tank 90 through a closed pipeline for continuously inputting a high pressure shielding gas into the reaction vessel 20 and the product storage tank 90, so that the continuous reaction process
  • the predetermined reaction pressure is maintained in the reaction vessel 20 and the continuous reaction tube 50.
  • the shielding gas can be hydrogen or nitrogen.
  • the gas protection device 60 may include a pressurized gas tank 62, a filter 64, and a pressure reducing valve 66 connected by a closed line.
  • the high pressure gas in the pressurized gas tank 62 is filtered by the filter 64, and then depressurized to a suitable reaction pressure by a pressure reducing valve 66, and sent to the reaction vessel 20 and the product storage tank 90 through a closed line.
  • a check valve 68 may be provided at the outlet of the gas input device 60 to protect the gas input device 60.
  • the product storage tank 90 can be coupled to a back pressure valve 92 such that the internal pressure of the product storage tank 90 does not exceed a predetermined pressure during the reaction.
  • the product storage tank 90 may have a volume of 10L to 20L, an internal working temperature range of 0 to 250 ° C, and a working pressure range of 0 to 1.6 MPa.
  • the connecting gas input device 60 and the reaction vessel 20 and the product storage tank 90 may be provided with a valve, such as a ball valve, to adjust the pressure of the output gas, and the connection between the product storage tank 90 and the continuous reaction tube 50.
  • the pipeline can also be provided with a ball valve.
  • the pressure detecting device 80 may be separately disposed at different positions of the lithium iron phosphate continuous preparation device 1 to monitor the pressure inside the devices, for example, inside and outside the gas input device 60, the inlet of the continuous reaction tube 50, and the product.
  • a pressure detecting device 80 is disposed inside the tank.
  • the different positions of the lithium iron phosphate continuous preparation device 1 may be respectively provided with valves, such as a ball valve 70, to facilitate segmentation control and maintenance of the preparation device 1.
  • the raw material solutions are respectively taken out from the respective raw material tanks 10 through the metering pump 12, and are input to the reaction vessel 20.
  • the heating jacket 22 heats the reaction vessel 20, the agitator 24 agitates the raw material solution, and the gas input device 60 introduces a gas into the reaction vessel 20 to raise the pressure of the reaction vessel 20 to a predetermined pressure range to make the raw material solution uniform.
  • lithium iron phosphate product crystals are crystallized under the conditions of temperature and pressure.
  • the residence time of the material in the reactor 20 is determined by the difference between the feed rate and the discharge speed, and can be adjusted by adjusting the flow rate of the metering pump and the intermediate pump to allow the material to stay in the reactor 20 for a sufficient period of time.
  • the pre-reacted material is sent from the intermediate pump 40 to the continuous reaction tube 50, through which the temperature of the continuous reaction tube 50 is maintained at a predetermined temperature interval of the reaction, and the inside of the continuous reaction tube 50 remains the predetermined temperature.
  • the reaction pressure so the hydrothermal or solvothermal reaction can continue, so that the crystal grains of the lithium iron phosphate product are continuously increased, and the length of the continuous reaction tube 50 can make the reaction long enough for the material to advance from the inlet to the outlet.
  • the product produced after the reaction is completed is input to the product storage tank 90.
  • the gas input device 60 causes the product storage tank 90 to have the same pressure as the reaction vessel 20, so that the inside of the continuous reaction tube 50 in communication between the two can have the same pressure.
  • the utility model divides the original reaction kettle of the hydrothermal synthesis method into two parts, namely, a stirring reaction device and a constant temperature reaction device, and supplies the pressure required by the two devices through the gas input device, so that the raw materials continuously pass through the two
  • the device can continuously react to form lithium iron phosphate during the operation of the material, and can obtain a better crystal form, and can realize large-scale industrial continuous production of the product, and greatly improve the consistency of the lithium iron phosphate product.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

提供一种磷酸铁锂制备装置，属于连续制备装置，包括原料罐（10）、反应釜（20）、中间泵（40）、连续反应管（50）、产品储罐（90）和气体输入装置（60），反应釜（20）的进料口通过密闭的管路与原料罐（10）相连接，中间泵（40）分别与反应釜（20）的出料口及连续反应管（50）通过密闭的管路连接，使物料连续不断的从该反应釜（20）输送至连续反应管（50），并输出至产品储罐（90），连续反应管（50）的一端与中间泵（40）相连，另一端与产品储罐（90）通过密闭的管路连接，气体输入装置（60）分别与反应釜（20）及产品储罐（90）通过密闭的管路相连，使反应釜（20）及连续反应管（50）中维持预定的反应压力。

Description

磷酸铁锂连续制备装置 技术领域
本实用新型涉及一种磷酸铁锂连续制备装置。
背景技术
能源问题一直是人类社会与科学技术发展的一个重大问题。锂离子电池作为能量密度较高的绿色二次电池，已广泛应用于笔记本电脑、手机、摄影机等消费性电子产品。
磷酸铁锂作为一种具有较好安全性，价格低廉且对环境友好的锂离子电池正极活性材料一直受到人们极大关注。目前磷酸铁锂在实验室中的合成方法主要有高温固相法、喷雾法、水热合成法、共沉淀法、乳剂干燥法和微波合成法等。在工业上磷酸铁锂主要通过高温固相法大规模合成。然而，高温固相法需要在较高温度下进行烧结，产物粒度较大，性能较差。水热合成及溶剂热合成是能够在较低温度下合成较小尺寸晶粒的磷酸铁锂的方法。然而这两种合成方法需要将原料放置于密封的高压釜中加压加热，每次合成的产量受高压釜容积的限制，难以应用于工业化大规模生产。并且分批次合成的磷酸铁锂容易受反应条件差异的影响，不同批次生产的磷酸铁锂产品性能不一致。
发明内容
有鉴于此，确有必要提供一种磷酸铁锂连续制备装置，通过该装置能够实现磷酸铁锂水热合成法的连续制备，满足工业化产品性一致性需要。
一种磷酸铁锂制备装置，包括一种磷酸铁锂连续制备装置，包括原料罐、反应釜、中间泵、连续反应管、产品储罐和气体输入装置，该反应釜的进料口通过密闭的管路与该原料罐相连接，该中间泵分别与该反应釜的出料口及该连续反应管通过密闭的管路连接，使物料连续不断的从该反应釜输送至该连续反应管，并输出至该产品储罐，该连续反应管的一端与该中间泵相连，另一端与该产品储罐通过密闭的管路连接，该气体输入装置分别与该反应釜及该产品储罐通过密闭的管路相连，使反应釜及连续反应管中维持预定的反应压力。
本实用新型将水热合成法原有的反应釜分为两个部分，即搅拌反应装置与恒温反应装置，并通过气体输入装置提供该两个装置所需的压力，使原料连续的经过该两个装置，可以实现在物料运行过程中不断反应生成磷酸铁锂，可以实现产品大规模工业化连续生产，大大提高磷酸铁锂产品的一致性。
 附图说明
图1为本实用新型实施例磷酸铁锂连续制备装置的结构示意图。
主要元件符号说明
磷酸铁锂连续制备装置 1
原料罐 10
计量泵 12
反应釜 20
加热套 22
搅拌器 24
变频器 26
放料阀 28
热电偶 30
中间泵 40
连续反应管 50
恒温油浴箱 52
加热器 54
气体输入装置 60
压力气罐 62
过滤器 64
减压阀 66
单向阀 68
球阀 70
压力检测装置 80
产品储罐 90
背压阀 92
如下具体实施方式将结合上述附图进一步说明本实用新型。
具体实施方式
下面将结合附图及具体实施例对本实用新型提供的磷酸铁锂连续制备装置作进一步的详细说明。
请参阅图1，本实用新型提供一种磷酸铁锂连续制备装置1，用于通过水热合成法或溶剂热合成法连续制备磷酸铁锂，该磷酸铁锂连续制备装置1包括原料罐10、混合搅拌装置、中间泵40、恒温反应装置、产品储罐90和气体输入装置60。
该原料罐10用于储存水热合成或溶剂热合成磷酸铁锂的原料溶液，本实施例包括两个原料罐10，其中一个原料罐10储存磷酸亚铁溶液，另一个原料罐10储存磷酸与氢氧化锂反应后的溶液。
该混合搅拌装置用于使原料溶液混合并在预定的温度及压力下进行均匀混合。该混合搅拌装置包括反应釜20、加热套22及搅拌器24。该反应釜20的进料口通过密闭的管路与原料罐10相连接，在原料罐10与反应釜20之间的密闭的管路上可以进一步设置计量泵12，工作压力为0~2MPa，用于将原料溶液输送到反应釜20并控制从不同原料罐10输送的原料溶液之间的比例。该搅拌器24设置在反应釜20内部，具体可以是具有搅拌浆的搅拌杆，该搅拌器24可以与设置在反应釜20外部电控装置连接，该电控装置可以具有变频器26，用于调整搅拌器24的转速，该转速可以为0~200转/分钟。该加热套22设置在该反应釜20外部，用于对该反应釜20进行加热和保温，具体可以围绕该反应釜20外壁设置。该混合搅拌装置可进一步包括一测温仪，如热电偶30，对该反应釜20内部的温度进行测量。该混合搅拌装置主要是要将原料溶液进行均匀混合，在该混合搅拌装置中，原料溶液可以不发生化学反应。为提高生产效率，也可以使原料溶液在该混合搅拌装置中即开始发生化学反应，即进行水热或溶剂热合成磷酸铁锂的反应。该反应釜20内部的工作温度可以在25~250℃，工作压力可以在0~1.6MPa，容积可以为10L至20L。该反应釜20的出料口可以位于反应釜20的底部或侧壁上，当位于反应釜20的侧壁时，由于搅拌器24的搅拌产生的离心力可以使反应后的物料从侧壁的出料口外溢，当位于反应釜20的底部时，物料通过重力作用自然流出。该反应釜20可进一步包括一放料阀28，设置在出料口处，用于控制反应釜20内部物料的排放。该反应釜20可进一部具有排气装置，如针形阀，用于控制反应釜20内部压力在预定区间。
该恒温反应装置包括恒温油浴箱52及设置在该恒温油浴箱52中的连续反应管50。该恒温反应装置用于对经过该连续反应管50的物料在预定的压力下进行加热，并使物料通过整个连续反应管50的过程均处于恒温恒压状态，从而进行水热或溶剂热反应。该连续反应管50内的压力由气体输入装置60进行调节。该连续反应管50具有足够的长度使物料在连续反应管50中停留的时间足够长。具体地，物料在该连续反应管50的停留时间可以为2小时~6小时，对应的，该连续反应管50的长度可以为10米~20米，内径可以为5毫米~20毫米。该连续反应管50可以弯曲的设置在该恒温油浴箱52中以节省空间。该恒温油浴箱52通过加热器54进行加热，使内部油温均匀恒定，该恒温油浴箱52的工作温度范围可以为5~250℃。该恒温反应装置可进一步包括测温仪，如热电偶30，对恒温油浴箱52内部的油温及加热器54的温度进行测量。
该中间泵40设置在该反应釜20与该连续反应管50之间，分别与该反应釜20的出料口及该连续反应管50通过密闭的管路连接。该中间泵40用于将反应釜20中的物料连续不断的输入到连续反应管50中，并精确调节物料流量，使物料经过连续反应管50所停留的时间可控，最终通过该连续反应管50输出至该产品储罐。该中间泵40可以采用隔膜泵，额定流量可以在0~2升/小时，并可通过变频器对流量进行调整，出口压力可以为0~2MPa。该连续反应管50的一端与该反应釜20通过中间泵40相连，另一端与产品储罐90相连。该反应釜20与该连续反应管50中的压力可以通过气体输入装置60分别进行调节，从而可以相同或不同。
该气体输入装置60分别与该反应釜20及该产品储罐90通过密闭的管路相连，用于将高压保护气体不断输入至该反应釜20及该产品储罐90中，使连续反应过程中反应釜20及连续反应管50中维持预定的反应压力。该保护气体可以是氢气或氮气。该气体保护装置60可以包括通过密闭管路连接的压力气罐62、过滤器64及减压阀66。该压力气罐62中的高压气体通过过滤器64过滤后，经减压阀66减压至合适的反应压力，通过密闭管路分别输送至该反应釜20及该产品储罐90。进一步地，可在该气体输入装置60的出口处设置一单向阀68，以保护该气体输入装置60。该产品储罐90可连接有背压阀92，使反应过程中产品储罐90内部压力不超过预定压力。该产品储罐90的容积可以为10L~20L，内部的工作温度范围可以为0~250℃，工作压力范围可以为0~1.6MPa。该连接气体输入装置60与反应釜20及产品储罐90的管路上可以设置有阀门，如球阀，从而对输出的气体压力进行调节，该产品储罐90与该连续反应管50之间的连接管路也可设置有球阀。
该磷酸铁锂连续制备装置1的不同位置可分别设置有压力检测装置80，以对各装置内部的压力进行监测，例如在该气体输入装置60的内部及出口、连续反应管50的入口及产品储罐内部均设置有压力检测装置80。该磷酸铁锂连续制备装置1的不同位置可分别设置有阀门，如球阀70，以便于对制备装置1进行分段控制及检修。
在该磷酸铁锂的连续制备过程中，原料溶液分别从各自的原料罐10中通过计量泵12抽出，输入到反应釜20中。该加热套22对反应釜20加热，搅拌器24对原料溶液进行搅拌，气体输入装置60向反应釜20中通入气体，使反应釜20的压力升高至预定的压力范围，使原料溶液均匀混合并在预定的压力及温度条件下进行初步的预反应。根据水热或溶剂热反应原理，磷酸铁锂产物晶粒在该温度和压力条件下结晶生成。物料在该反应釜20中的停留时间由进料速度及出料速度之间的差值决定，可通过调整计量泵与中间泵的流量进行调整，使物料在该反应釜20中停留足够时间，以达到预反应的目的。经过预反应后的物料由中间泵40输送到连续反应管50，通过该恒温油浴箱52使连续反应管50的温度保持在反应的预定温度区间，并且该连续反应管50内部仍保持该预定的反应压力，因此该水热或溶剂热反应可继续进行，使磷酸铁锂产物晶粒不断增多，该连续反应管50的长度可以使物料从入口至出口前进的过程中可以停留足够长的反应时间，反应完毕后生成的产物输入至该产品储罐90。该气体输入装置60使产品储罐90与反应釜20的压力相同，从而可以使在两者之间联通的连续反应管50内部具有相同的压力。
本实用新型将水热合成法原有的反应釜分为两个部分，即搅拌反应装置与恒温反应装置，并通过气体输入装置提供该两个装置所需的压力，使原料连续的经过该两个装置，可以实现在物料的运行过程中不断反应生成磷酸铁锂，且可以得到较好的结晶形态，并且可以实现产品大规模工业化连续生产，大大提高磷酸铁锂产品的一致性。
另外，本领域技术人员还可在本实用新型精神内做其他变化，当然，这些依据本实用新型精神所做的变化，都应包含在本实用新型所要求保护的范围之内。

Claims (10)

  1. 一种磷酸铁锂连续制备装置，其特征在于，包括原料罐、反应釜、中间泵、连续反应管、产品储罐和气体输入装置，该反应釜的进料口通过密闭的管路与该原料罐相连接，该中间泵分别与该反应釜的出料口及该连续反应管通过管路连接，该连续反应管的一端与该中间泵相连，另一端与该产品储罐通过管路连接，该气体输入装置分别与该反应釜及该产品储罐通过管路相连。
  2. 如权利要求1所述的磷酸铁锂连续制备装置，其特征在于，进一步包括设置在原料罐与反应釜之间的密闭的管路上的计量泵。
  3. 如权利要求1所述的磷酸铁锂连续制备装置，其特征在于，进一步包括对该反应釜进行加热的加热套及在该反应釜内部的搅拌器。
  4. 如权利要求1所述的磷酸铁锂连续制备装置，其特征在于，进一步包括对该连续反应管进行加热的恒温油浴箱，该连续反应管设置在该恒温油浴箱中。
  5. 如权利要求1所述的磷酸铁锂连续制备装置，其特征在于，该连续反应管的长度为10米~20米，内径为5毫米~20毫米。
  6. 如权利要求1所述的磷酸铁锂连续制备装置，其特征在于，该连续反应管弯曲的设置在该恒温油浴箱中。
  7. 如权利要求1所述的磷酸铁锂连续制备装置，其特征在于，该中间泵的额定流量为0~2升/小时。
  8. 如权利要求1所述的磷酸铁锂连续制备装置，其特征在于，该气体保护装置包括通过密闭管路连接的压力气罐、过滤器及减压阀。
  9. 如权利要求1所述的磷酸铁锂连续制备装置，其特征在于，进一步包括设置在该气体输入装置出口处的单向阀。
  10. 如权利要求1所述的磷酸铁锂连续制备装置，其特征在于，进一步包括与该产品储罐连接的背压阀。
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