WO2015139526A1 - 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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WO2015139526A1
WO2015139526A1 PCT/CN2015/070979 CN2015070979W WO2015139526A1 WO 2015139526 A1 WO2015139526 A1 WO 2015139526A1 CN 2015070979 W CN2015070979 W CN 2015070979W WO 2015139526 A1 WO2015139526 A1 WO 2015139526A1
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kettle
aging kettle
aging
iron phosphate
lithium iron
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PCT/CN2015/070979
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English (en)
French (fr)
Inventor
何向明
王莉
罗晶
李建军
徐程浩
张建利
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 WO2015139526A1 publication Critical patent/WO2015139526A1/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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B01J19/006—Baffles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • B01J19/245—Stationary reactors without moving elements inside placed in series
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00054—Controlling or regulating the heat exchange system
    • B01J2219/00056—Controlling or regulating the heat exchange system involving measured parameters
    • B01J2219/00058—Temperature measurement
    • B01J2219/00063—Temperature measurement of the reactants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00054—Controlling or regulating the heat exchange system
    • B01J2219/00056—Controlling or regulating the heat exchange system involving measured parameters
    • B01J2219/00065—Pressure measurement
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00054—Controlling or regulating the heat exchange system
    • B01J2219/00056—Controlling or regulating the heat exchange system involving measured parameters
    • B01J2219/00067—Liquid level measurement
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00094—Jackets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00162—Controlling or regulating processes controlling the pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00164—Controlling or regulating processes controlling the flow
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00182—Controlling or regulating processes controlling the level of reactants in the reactor vessel
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00189—Controlling or regulating processes controlling the stirring velocity

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 continuous preparation device for lithium iron phosphate comprising a raw material tank, a reaction kettle, a first aging kettle, a second aging kettle, a gas input device, a heating device, a stirrer and a product storage tank, wherein the reaction kettle is connected to the raw material tank, The first aging kettle is connected to the reaction kettle, and the second aging kettle is connected to the first aging kettle, the gas input device and the reaction kettle, the first aging kettle, the second aging kettle and the product respectively
  • the storage tanks are connected, and the heating devices are respectively disposed outside the reaction kettle, the first aging kettle and the second aging kettle, and the agitators are respectively disposed inside the reaction kettle, the first aging kettle and the second aging kettle.
  • 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 Raw material preheating device 14 Reactor 20 Back pressure valve twenty two Baffle twenty four The first Chenhua kettle 30 Second aging kettle 40 Heating jacket 50 Blender 52 Frequency converter 54 Discharge valve 56 Thermocouple 58 Level gauge 59 Gas input device 60 Pressure gas tank 62 filter 64 Pressure reducing valve 66 Needle valve 68 Check valve 69 Ball valve 70 Pressure detecting device 80 Product storage tank 90
  • 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 lithium iron phosphate continuous preparation device 1 may further include a raw material preheating device 14 disposed outside the closed conduit connecting the raw material tank 10 and the reaction kettle 20 to preheat the raw material solution flowing through the pipeline, which is helpful The reaction proceeds in the reaction vessel 20.
  • the raw material solution passes through the reaction vessel 20, the first aging kettle 30 and the second aging kettle 40 in sequence, and undergoes two reaction processes, namely, a preliminary reaction process in the reactor 20, and in the first aging kettle 30. And an aging reaction process in the second sinker 40.
  • a preliminary reaction process in the reactor 20 In the whole hydrothermal or solvothermal reaction process of lithium iron phosphate, lithium iron phosphate can be initially formed in the reaction for 4 hours, but the time node of lithium iron phosphate crystal form is more than 10 hours, that is, the electrochemical performance is optimal.
  • the reaction vessel 20 is used to thoroughly mix the raw material solution and complete a preliminary crystallization reaction having an average residence time of 4 hours at a predetermined temperature and pressure, and strong stirring is required in the reaction vessel 20.
  • the first aging kettle 30 and the second aging kettle 40 are used to complete the reaction time of the average crystallization of lithium iron phosphate crystals together with the mother liquor in a stable and stable reaction condition for 5 hours to 10 hours.
  • the iron-lithium crystal form is complete and the electrochemical performance is optimized.
  • the reaction time of all the materials is normally distributed, and the first aged kettle 30 and the second aged kettle 40 can make the normal distribution of the reaction time more. Focus on the average stay time.
  • the first aging kettle 30 is connected to the reactor 20 through a closed line
  • the second aging kettle 40 is connected to the first aging kettle 30 through a closed line.
  • the second aging kettle 40 is connected to the product storage tank 90 via a closed conduit.
  • the discharge port on the side wall of the reaction vessel 20 is connected to the feed port of the first aging kettle 30.
  • the discharge port on the side wall of the first aging kettle 30 is connected to the feed port of the second aging kettle 40, and the discharge port on the side wall of the second aging kettle 40 is connected to the product storage tank 90.
  • the reactor 20, the first aging kettle 30 and the second aging kettle 40 are all required to operate at a constant temperature and pressure, and the pressure and temperature of the three kettles can be the same.
  • the working temperature of the three kettles can be between 25 and 250 ° C
  • the working pressure can be from 0 to 1.6 MPa
  • the volume of each kettle can be from 10 L to 20 L.
  • the preparation device 1 further includes three heating devices, such as a heating jacket 50, which are respectively disposed outside the reaction vessel 20, the first aging kettle 30 and the second aging kettle 40, for the reactor 20, the first Chen The kettle 30 and the second aging kettle 40 are separately heated and insulated.
  • the preparation apparatus 1 may further include three thermometers, such as a thermocouple 58, for measuring the temperatures inside the reactor 20, the first aging kettle 30, and the second aging kettle 40, respectively.
  • the preparation apparatus 1 may include three level gauges 59 disposed inside the reaction vessel 20, the first aging kettle 30, and the second aging kettle 40, respectively, for measuring the height of the internal material.
  • the reactor 20 may further include one or more baffles 24 disposed on the inner wall of the reaction vessel 20 for increasing the stirring resistance to sufficiently uniformly mix the raw material solution.
  • the reactor 20, the first aging kettle 30 and the second aging kettle 40 may each have a discharge valve 56 at the bottom of the tank for discharging the residual material in the kettle during shutdown.
  • the gas input device 60 is connected to the reaction kettle 20, the first aging kettle 30, the second aging kettle 40, and the product storage tank 90 through a closed pipeline for inputting a high pressure shielding gas for continuous reaction. Maintain a predetermined reaction pressure.
  • the connecting gas input device 60 and the reaction kettle 20, the first aging kettle 30, the second aging kettle 40, and the product storage tank 90 may be respectively provided with a pressure regulating valve, such as a ball valve 70, so as to The pressure of the product storage tank 90 is adjusted.
  • the reaction vessel 20, the first aging kettle 30, and the second aging kettle 40 may each have an exhausting device, such as a back pressure valve 22, for controlling the internal pressure of each of the kettles to be within a predetermined interval.
  • the shielding gas can be hydrogen or nitrogen.
  • the gas input 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.
  • the gas input device 60 can further include a needle valve 68 coupled to the pressure relief valve 66. Further, a check valve 69 may be provided at the outlet of the gas input device 60 to protect the gas input device 60.
  • the product storage tank 90 may have a volume of 10L ⁇ 20L, an operating temperature range of 0 ⁇ 250°C, and a working pressure range of 0 ⁇ 1.6MPa.
  • 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 reaction kettle 20, and the first aging A pressure detecting device 80 is provided inside the kettle 30 and the second aging kettle 40.
  • the different positions of the lithium iron phosphate continuous preparation device 1 may be respectively provided with a switching valve, such as a ball valve 70, to facilitate segmentation control and maintenance of the preparation device 1.
  • the gas input device 60 introduces gas into the reaction vessel 20, the first aging kettle 30, the second aging kettle 40, and the product storage tank 90, so that the pressure of the three kettles
  • the pressure is raised to a predetermined pressure range that is adjusted by a back pressure valve 22 and a pressure reducing valve 66 that heats the three kettles to a predetermined temperature range.
  • the raw material solutions are respectively withdrawn from the respective raw material tanks 10 through the metering pump 12, continuously injected into the reaction vessel 20, uniformly mixed by stirring, and subjected to preliminary pre-reaction under predetermined pressure and temperature conditions, according to hydrothermal or solvent heat.
  • lithium iron phosphate is crystallized under the conditions of temperature and pressure, and is continuously grown and fully reacted in the second-stage reaction and the third-stage reaction.
  • the discharge ports of the reaction vessel 20, the first aging kettle 30 and the second aging kettle 40 are all located on the side walls, and the centrifugal force generated by the stirring of the material of the reactor 20 under the agitator 52 is from the side wall.
  • the port overflows continuously to enter the first aging kettle 30.
  • the discharge port from the side wall continuously enters the second aging kettle 40, and under the agitation of the agitator 52 of the second aging kettle 40.
  • the product outlet tank 90 is continuously introduced from the discharge port of the side wall.
  • the process is a continuous process in which a raw material solution is continuously fed from the raw material tank 10 into the reaction vessel 20, and products are continuously output from the second aging kettle 40 to achieve dynamic equilibrium.
  • the utility model divides the hydrothermal synthesis method into three steps, corresponding to the reaction kettle, the first aging kettle and the second aging kettle, respectively, and provides the pressure required in the three kettles through the gas input device, so that the raw materials are continuously passed.
  • the three kettles 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)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

提供一种磷酸铁锂连续制备装置，包括原料罐（10）、反应釜（20）、第一陈化釜（30）、第二陈化釜（40）、气体输入装置（60）、加热装置（50）、搅拌器（52）及产品储罐（90），其中反应釜（20）与原料罐（10）相连，第一陈化釜（30）与反应釜（20）相连，第二陈化釜（40）与第一陈化釜（30）相连，气体输入装置（60）分别与反应釜（20）、第一陈化釜（30）、第二陈化釜（40）及产品储罐相（90）连，加热装置（50）分别设置在反应釜（20）、第一陈化釜（30）及第二陈化釜（40）外部，搅拌器（52）分别设置在反应釜（20）、第一陈化釜（30）及第二陈化釜（40）内部。

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。
一种磷酸铁锂连续制备装置，包括原料罐、反应釜、第一陈化釜、第二陈化釜、气体输入装置、加热装置、搅拌器及产品储罐，该反应釜与原料罐相连，该第一陈化釜与该反应釜相连，该第二陈化釜与第一陈化釜相连，该气体输入装置分别与该反应釜、第一陈化釜、第二陈化釜及该产品储罐相连，该加热装置分别设置在该反应釜、第一陈化釜及第二陈化釜外部，该搅拌器分别设置在该反应釜、第一陈化釜及第二陈化釜内部。
本实用新型通过该磷酸铁锂连续制备装置使水热合成法可以分三个阶段进行，分别对应反应釜、第一陈化釜及第二陈化釜，通过气体输入装置提供三个釜中所需的压力，使原料连续的经过该三个釜，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。
 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
原料预热装置 14
反应釜 20
背压阀 22
挡板 24
第一陈化釜 30
第二陈化釜 40
加热套 50
搅拌器 52
变频器 54
放料阀 56
热电偶 58
液位计 59
气体输入装置 60
压力气罐 62
过滤器 64
减压阀 66
针形阀 68
单向阀 69
球阀 70
压力检测装置 80
产品储罐 90
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、反应釜20、第一陈化釜30、第二陈化釜40、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。该原料罐10通过密闭的管路与反应釜20的进料口相连接，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，用于将原料溶液输送到反应釜20。该磷酸铁锂连续制备装置1可进一步包括一原料预热装置14，设置在连接该原料罐10与该反应釜20的密闭管路外，使流过该管路的原料溶液预加热，有助于反应釜20中反应的进行。
该原料溶液依次经过该反应釜20、第一陈化釜30及第二陈化釜40，分别经历两个反应过程，即在反应釜20中的初步反应过程，以及在第一陈化釜30及第二沉化釜40中的陈化反应过程。在磷酸铁锂的整个水热或溶剂热反应过程中，反应4个小时即可初步生成磷酸铁锂，但10个小时以上为磷酸铁锂晶型完备的时间节点，即电化性能为最优。该反应釜20用于使原料溶液充分混合并在预定的温度及压力下完成平均停留时间为4小时的初步结晶反应，该反应釜20中需要进行强搅拌。该第一陈化釜30及第二陈化釜40用于使初步结晶的磷酸铁锂晶与母液一起在反应条件较稳稳定的环境下完成平均停留5小时~10小时的反应时间，使磷酸铁锂晶型完备，达到电化学性能的最优化。另外，由于原料溶液在全混流反应釜20中连续进出，所有物料的反应时间为正态分布，该第一陈化釜30及第二陈化釜40可以使该反应时间的正态分布更加的集中于平均停留时间。
该第一陈化釜30与该反应釜20通过密闭的管路相连，该第二陈化釜40与第一陈化釜30通过密闭的管路相连。该第二陈化釜40与该产品储罐90通过密闭管路连接。具体地，该反应釜20侧壁上的出料口与该第一陈化釜30的进料口相连。该第一陈化釜30侧壁上的出料口与第二陈化釜40的进料口相连，该第二陈化釜40侧壁上的出料口与产品储罐90相连。
该反应釜20、第一陈化釜30及第二陈化釜40均需要在恒定的温度及压力下工作，该三个釜的压力及温度可相同。优选地，该三个釜内部的工作温度均可以在25~250℃，工作压力均可以在0~1.6MPa，每个釜的容积可以为10L至20L。
该制备装置1还包括三个加热装置，如加热套50，分别设置在该反应釜20、第一陈化釜30及第二陈化釜40的外部，用于对反应釜20、第一陈化釜30及第二陈化釜40分别进行加热和保温。另外，该制备装置1可进一步包括三个测温仪，如热电偶58，分别对该反应釜20、第一陈化釜30及第二陈化釜40内部的温度进行测量。
该制备装置1还包括三个搅拌器52，分别设置在该反应釜20、第一陈化釜30及第二陈化釜40的内部，具体可以是具有搅拌浆的搅拌杆，该搅拌器52可以与设置在釜外的电控装置连接，该电控装置可以具有变频器54，用于调整搅拌器52的转速，该转速可以为0~200转/分钟。
该制备装置1可包括三个液位计59，分别设置在该反应釜20、第一陈化釜30及第二陈化釜40的内部，用于测量内部物料的高度。
该反应釜20可进一步包括一个或多个挡板24，设置在反应釜20的内壁上，用于增加搅拌阻力，使原料溶液充分均匀的混合。
该反应釜20、第一陈化釜30及第二陈化釜40可分别在釜底具有放料阀56，用于在停机时排放釜内残留物料。
该气体输入装置60分别与该反应釜20、第一陈化釜30、第二陈化釜40及该产品储罐90通过密闭的管路相连，用于输入高压保护气体，使连续反应过程中维持预定的反应压力。该连接气体输入装置60与反应釜20、第一陈化釜30、第二陈化釜40及产品储罐90的管路上可以分别设置有压力调节阀门，如球阀70，从而对三个釜及产品储罐90的压力进行调节。该反应釜20、第一陈化釜30及第二陈化釜40可分别具有一排气装置，如背压阀22，用于分别控制各个釜内部压力在预定区间。该保护气体可以是氢气或氮气。该气体输入装置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。该气体输入装置60可进一步包括一针形阀68，与该减压阀66连接。进一步地，可在该气体输入装置60的出口处设置一单向阀69，以保护该气体输入装置60。该产品储罐90的容积可以为10L~20L，工作温度范围可以为0~250℃，工作压力范围可以为0~1.6MPa。
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，反应釜20、第一陈化釜30及第二陈化釜40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开关阀门，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，气体输入装置60向反应釜20、第一陈化釜30、第二陈化釜40及该产品储罐90中通入气体，使三个釜的压力升高至预定的压力范围，该压力范围通过背压阀22及减压阀66调整，加热套50对三个釜进行加热至预定的温度范围。原料溶液分别从各自的原料罐10中通过计量泵12抽出，不断的注入到反应釜20中，通过搅拌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，磷酸铁锂在该温度和压力条件下结晶生成，并在第二级反应及第三级反应中不断长大并反应充分。该反应釜20、第一陈化釜30及第二陈化釜40的出料口均位于侧壁上，在反应釜20的物料在搅拌器52的搅拌下产生的离心力，从侧壁的出料口不断溢出，从而进入该第一陈化釜30。相似地，在第一陈化釜30的搅拌器52的搅拌下从侧壁的出料口不断的进入到第二陈化釜40，以及在第二陈化釜40的搅拌器52的搅拌下从侧壁的出料口不断的进入到产品储罐90。该过程为一连续过程，不断有原料溶液从原料罐10输入反应釜20中，并不断有产物从第二陈化釜40输出，从而达到动态平衡。
本实用新型将水热合成法分三个步骤进行，分别对应反应釜、第一陈化釜及第二陈化釜，通过气体输入装置提供三个釜中所需的压力，使原料连续的经过该三个釜，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、第一陈化釜、第二陈化釜、气体输入装置、加热装置、搅拌器及产品储罐，该反应釜与原料罐相连，该第一陈化釜的进料口与该反应釜侧壁上的出料口相连，该第二陈化釜的进料口与第一陈化釜侧壁上的出料口相连，该产品储罐与该第二沉化釜侧壁上的出料口相连，该气体输入装置分别与该反应釜、第一陈化釜、第二陈化釜及该产品储罐相连，该加热装置分别设置在该反应釜、第一陈化釜及第二陈化釜外部，该搅拌器分别设置在该反应釜、第一陈化釜及第二陈化釜内部。
  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，该反应釜、第一陈化釜及第二陈化釜均具有背压阀。
  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，该反应釜与原料罐通过密闭管路相连接，该磷酸铁锂连续制备装置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。
  4. 如权利要求3所述的磷酸铁锂连续制备装置，其特征在于，进一步包括原料预热装置设置在连接该原料罐与该反应釜的密闭管路外。
  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，该气体输入装置包括通过密闭管路连接的压力气罐、过滤器及减压阀。
  6. 如权利要求5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。
  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，进一步包括压力调节阀门，分别设置在该气体输入装置与反应釜、第一陈化釜、第二陈化釜及产品储罐连接的管路上。
  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，进一步包括液位计，分别设置在该反应釜、第一陈化釜及第二陈化釜的内部。
  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，该反应釜进一步包括一个或多个挡板，设置在反应釜的侧壁上。
  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，该反应釜、第一陈化釜及第二陈化釜分别在釜底具有放料阀。
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