WO2018076747A1 - System for preparing lithium hydroxide - Google Patents
System for preparing lithium hydroxide Download PDFInfo
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- WO2018076747A1 WO2018076747A1 PCT/CN2017/090661 CN2017090661W WO2018076747A1 WO 2018076747 A1 WO2018076747 A1 WO 2018076747A1 CN 2017090661 W CN2017090661 W CN 2017090661W WO 2018076747 A1 WO2018076747 A1 WO 2018076747A1
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- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/02—Oxides; Hydroxides
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- the lithium product is characterized in that it further comprises: a shielding gas supply subsystem for removing carbon dioxide from the air, thereby providing carbon dioxide-free air as a shielding gas for the preparation process of the lithium hydroxide, and protecting the gas supply subsystem
- the system includes: a filtering device having: an air inlet portion that introduces outside air, a filter portion that communicates with the air inlet portion, filters and removes particulate matter in the introduced outside air, and communicates with the filter portion to filter
- the air outlet port derived from the rear air the mother liquid storage device stores the lithium hydroxide mother liquor remaining after the crystal is precipitated in the concentrated crystallizing device;
- the absorption tower has a gas inlet portion connected to the gas outlet port to introduce the filtered air
- the absorbent inlet portion communicates with the mother liquid storage device, and the lithium hydroxide mother liquid is introduced as an absorbent;
- the tower body communicates with the gas inlet portion and communicates with the absorption liquid inlet portion, and the absorbent is used for the filtered
- the absorption tower can utilize the remaining lithium hydroxide mother liquor as the absorbent after the crystal is precipitated in the concentrated crystallization device.
- Figure 4 is a block diagram showing the structure of a cleaning member according to the present invention in an embodiment
- Figure 9 is a control flow chart of the drying control unit according to the present invention in the embodiment.
- the preparation subsystem uses a lithium salt such as crude lithium carbonate, industrial grade lithium carbonate, lithium chloride or lithium sulfate as a raw material to prepare a lithium hydroxide product, which comprises: a raw material removing device, a causticizing device, a concentrated crystallization device, and a crystal drying device. , crushing device and screening packaging device.
- a lithium salt such as crude lithium carbonate, industrial grade lithium carbonate, lithium chloride or lithium sulfate
- the filtering device 100 is for filtering out particulate matter in the air, and includes a housing 11, three filter members 12, and a cleaning member 13.
- the inside of the rotating plate 131a is further provided with a first water supply passage communicating with the first cleaning liquid distribution pipe 131c. (not shown), the inlet B of the first water supply passage extends from the inside of the rotating shaft 131a-2 to communicate with the water supply unit 135.
- the three ultrasonic vibrating members 136 are respectively mounted on the three fixing frames of the three filtering members 12, and in the cleaning state, the filtering member 12 is driven to vibrate by the ultrasonic vibrating member 136, and under the action of the ultrasonic waves, the dust on the filtering net is accelerated and disengaged. , which can improve the cleaning effect.
- the mother liquid storage device 200 stores the lithium hydroxide mother liquid remaining after the crystals are precipitated in the concentrated crystallizing device. Since the lithium hydroxide mother liquid has a very high hydroxide content, it is possible to efficiently absorb carbon dioxide in the air.
- the carbon dioxide in the air can be sufficiently absorbed, thereby achieving the purpose of effectively removing carbon dioxide, and further, the gas drying device
- the carbon dioxide-free gas is dried to obtain a shielding gas, and the supply device can supply the shielding gas to the preparation subsystem, so that an inexpensive gas such as air can be used as a shielding gas used in a large quantity in the preparation subsystem, thereby effectively reducing hydrogen.
- the cost of preparing lithium oxide is very high, the carbon dioxide in the air can be sufficiently absorbed, thereby achieving the purpose of effectively removing carbon dioxide, and further, the gas drying device The carbon dioxide-free gas is dried to obtain a shielding gas, and the supply device can supply the shielding gas to the preparation subsystem, so that an inexpensive gas such as air can be used as a shielding gas used in a large quantity in the preparation subsystem, thereby effectively reducing hydrogen.
- the cost of preparing lithium oxide is very high.
- the air filtering device has three filter members, and as the air filtering device of the present invention, it is also possible to provide only two filter members or have three or more filters depending on the actual filtering conditions.
- the member, and the filter particle size of the filter member can also be selected depending on the situation. The more the number of filter members, the finer the particle size and the better the filtration effect, but the filtration time will be longer and the cost will increase.
- the filter mesh located at the outermost layer of the first filter member and the second filter member is a magnetic filter mesh
- at least one filter member is provided At least one layer of the filter is a magnetic filter, and the magnetic foreign matter can be filtered.
- the more the number of the magnetic filter the better the effect of the magnetic difference, but the corresponding cost will increase, so it can be based on actual conditions. The need for the situation to determine the number of magnetic filters.
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Abstract
Description
本发明属于电池材料制备领域,具体涉及一种氢氧化锂制备系统。The invention belongs to the field of battery material preparation, and in particular relates to a lithium hydroxide preparation system.
随着锂离子电池在新能源汽车上的应用,高镍、高能量密度正极材料成为发展趋势。目前,高镍正极材料一般都是采用氢氧化锂作为原料,相比于碳酸锂,氢氧化锂因其在晶体结构、溶解性等方面的优势,或更能满足未来锂电材料“以安全性为前提、不断提升能量密度”的大趋势。With the application of lithium ion batteries in new energy vehicles, high nickel and high energy density cathode materials have become a development trend. At present, high-nickel cathode materials generally use lithium hydroxide as a raw material. Compared with lithium carbonate, lithium hydroxide has advantages in crystal structure, solubility, etc., or more suitable for future lithium-ion materials. The premise is to continuously increase the energy density.
现在,制备电池级的氢氧化锂产品一般都是采用如下工艺流程和装置:Now, the preparation of battery-grade lithium hydroxide products generally uses the following processes and devices:
1)原料除杂,采用原料除杂装置以粗碳酸锂、工业级碳酸锂、氯化锂、硫酸锂等作为原料,对其进行除杂提纯;1) removing impurities from raw materials, using raw material removing device to remove impurities and purifying with crude lithium carbonate, industrial grade lithium carbonate, lithium chloride, lithium sulfate, etc.
2)苛化,将提纯后的原料加入苛化装置中,与氢氧化钙溶液或氢氧化钠溶液进行苛化反应得到氢氧化锂溶液;2) causticizing, adding the purified raw material to a causticizing device, causticizing reaction with calcium hydroxide solution or sodium hydroxide solution to obtain a lithium hydroxide solution;
3)浓缩结晶,采用浓缩结晶装置对氢氧化锂溶液进行浓缩结晶得到氢氧化锂晶体和氢氧化锂母液;3) concentrated crystallization, concentrated crystallization of the lithium hydroxide solution using a concentrated crystallization device to obtain lithium hydroxide crystals and lithium hydroxide mother liquor;
4)晶体干燥,采用晶体干燥装置对氢氧化锂晶体进行动态干燥;4) crystal drying, using a crystal drying device to dynamically dry lithium hydroxide crystals;
5)破碎,采用破碎装置对干燥后的氢氧化锂进行破碎;5) crushing, crushing the dried lithium hydroxide by using a crushing device;
6)筛分包装,采用筛分包装装置对破碎后的氢氧化锂进行筛分和包装,制成成品。6) Screening and packaging, using the screening and packaging device to sieve and package the crushed lithium hydroxide to form a finished product.
在上述生产过程中,制备的氢氧化锂极易吸收空气中的二氧化碳,而重新生成碳酸锂,为了避免与二氧化碳反应,保证产品中的碳酸根含量≤0.7wt.%以达到纯度标准,在苛化装置、浓缩结晶装置、晶体干燥装置、破碎装置以及筛分包装装置中都会通入惰性气体,如氮气、氩气等,作为保护气体,以防止空气中的二氧化碳进入,但是上述制备过程时间长、使用装置多,惰性气体的消耗量非常大,大大增加了氢氧化锂的制备成本。In the above production process, the prepared lithium hydroxide is very easy to absorb carbon dioxide in the air, and re-generates lithium carbonate, in order to avoid reaction with carbon dioxide, to ensure that the carbonate content in the product is ≤0.7wt.% to achieve the purity standard, in the harsh Inertizers, concentrated crystallization devices, crystal drying devices, crushing devices, and screening and packaging devices are all supplied with an inert gas such as nitrogen or argon as a shielding gas to prevent carbon dioxide from entering the air, but the above preparation process takes a long time. The use of many devices, the consumption of inert gas is very large, greatly increasing the preparation cost of lithium hydroxide.
发明内容Summary of the invention
本发明是为了解决上述课题而进行的,目的在于提供一种低成本制备氢氧化锂的氢氧化锂制备系统。The present invention has been made to solve the above problems, and an object thereof is to provide a lithium hydroxide production system which can produce lithium hydroxide at low cost.
本发明为了实现上述目的,采用了以下结构。In order to achieve the above object, the present invention employs the following structure.
本发明所涉及的氢氧化锂制备系统,包括:制备子系统,采用锂盐作为原料经原料除杂装置、苛化装置、浓缩结晶装置、晶体干燥装置、破碎装置以及筛分包装装置制备氢氧化锂产品,其特征在于,还包括:保护气体供给子系统,除去空气中的二氧化碳,从而为氢氧化锂的制备工艺提供无二氧化碳的空气作为保护气体,保护气体供给子系 统,包括:过滤装置,具有:将外部空气引入的进气口部,与进气口部相连通、将引入的外部空气中的颗粒物过滤去除的过滤部,以及与过滤部相连通、将过滤后的空气导出的出气口部;母液储存装置,存储有浓缩结晶装置中析出晶体后余下的氢氧化锂母液;吸收塔,具有:气体入口部,与出气口部相连通,将过滤后空气引入;吸收剂入口部,与母液储存装置相连通,引入氢氧化锂母液作为吸收剂;塔体,与气体入口部相连通,并与吸收液入口部相连通,用吸收剂来对过滤后空气中的二氧化碳进行吸收以获得无二氧化碳气体;气体排出口部,与塔体相连通,将无二氧化碳气体排出;以及液体排出口部,与塔体相连通,将吸收了二氧化碳的吸收剂作为吸收溶液排出;气体干燥装置,与气体排出口部相连通,对无二氧化碳气体进行干燥,得到保护气体;以及供给装置,与气体干燥装置相连通,将保护气体提供给制备子系统,其中,过滤部包括至少一个过滤构件,每个过滤构件都包括多层过滤网,至少一个过滤构件中的至少一层过滤网为磁性过滤网。The lithium hydroxide preparation system according to the present invention comprises: a preparation subsystem, which uses a lithium salt as a raw material to prepare a hydroxide by a raw material removing device, a causticizing device, a concentrated crystallization device, a crystal drying device, a crushing device, and a screening packaging device. The lithium product is characterized in that it further comprises: a shielding gas supply subsystem for removing carbon dioxide from the air, thereby providing carbon dioxide-free air as a shielding gas for the preparation process of the lithium hydroxide, and protecting the gas supply subsystem The system includes: a filtering device having: an air inlet portion that introduces outside air, a filter portion that communicates with the air inlet portion, filters and removes particulate matter in the introduced outside air, and communicates with the filter portion to filter The air outlet port derived from the rear air; the mother liquid storage device stores the lithium hydroxide mother liquor remaining after the crystal is precipitated in the concentrated crystallizing device; the absorption tower has a gas inlet portion connected to the gas outlet port to introduce the filtered air The absorbent inlet portion communicates with the mother liquid storage device, and the lithium hydroxide mother liquid is introduced as an absorbent; the tower body communicates with the gas inlet portion and communicates with the absorption liquid inlet portion, and the absorbent is used for the filtered air. The carbon dioxide is absorbed to obtain a carbon dioxide-free gas; the gas discharge port portion communicates with the tower body to discharge the carbon dioxide-free gas; and the liquid discharge port portion communicates with the tower body, and the absorbent that absorbs the carbon dioxide is discharged as the absorption solution. a gas drying device that communicates with the gas discharge port to dry the carbon dioxide-free gas to obtain a shielding gas And a supply device in communication with the gas drying device to provide the shielding gas to the preparation subsystem, wherein the filter portion includes at least one filter member, each filter member including a multi-layer filter, at least one of the at least one filter member The filter is a magnetic filter.
本发明所涉及的氢氧化锂制备系统,还可以具有这样的特征:过滤装置具有:壳体,包括:壳本体,位于壳本体的一侧的进气口部,和位于壳本体的一侧的出气口部;过滤部,包括:至少两个过滤构件,安装在壳体内,位于进气口部和出气口部之间,对从进气口部进来的空气进行过滤;以及清洗构件,对过滤构件进行清洁,并将清洁出的颗粒物清洗后排出。The lithium hydroxide preparation system according to the present invention may further have a feature that the filter device has a casing, including: a casing body, an air inlet portion on one side of the casing body, and a side of the casing body. The air outlet portion includes: at least two filter members installed in the casing between the air inlet portion and the air outlet portion to filter air entering from the air inlet portion; and a cleaning member for filtering The components are cleaned and the cleaned particles are washed and discharged.
本发明所涉及的氢氧化锂制备系统,还可以具有这样的特征:清洗构件包括:至少一个清洗板单元,安装在壳体内,每个清洗板单元都位于相邻两个过滤构件之间,具有:转动板,可转动地安装在壳体内;多个喷气嘴,安装在转动板的正面上,能够向过滤构件喷气,将颗粒物从过滤构件喷出;以及第一清洗液分布管,安装在转动板的背面上,沿着该背面喷淋清洗液;吹气板单元,安装在壳体内,位于出气口部与最靠近该出气口部的过滤构件之间,具有:转动板和多个喷气嘴;第二清洗液分布管,安装在壳本体的内壁上,沿着与过滤构件的另一侧相对向的壳本体的内侧壁喷淋清洗液;清洗控制单元,与所有的转动板相连,控制每个转动板在过滤状态时都转动至与过滤构件相垂直,在清洗状态时都转动至使正面朝向过滤构件;以及清洗液排出单元,安装在壳本体底部,将附着有颗粒物的清洗液从壳本体内排出。The lithium hydroxide preparation system according to the present invention may further have the following feature: the cleaning member comprises: at least one cleaning plate unit installed in the casing, each cleaning plate unit being located between the adjacent two filtering members, a rotating plate rotatably mounted in the housing; a plurality of air nozzles mounted on the front surface of the rotating plate, capable of jetting air to the filtering member to eject particulate matter from the filtering member; and a first cleaning liquid distribution tube mounted on the rotation a cleaning liquid is sprayed along the back surface of the plate; the air blowing plate unit is installed in the casing, between the air outlet portion and the filter member closest to the air outlet portion, and has a rotating plate and a plurality of air nozzles a second cleaning liquid distribution pipe, mounted on the inner wall of the casing body, spraying the cleaning liquid along the inner side wall of the casing body opposite to the other side of the filtering member; the cleaning control unit is connected to all the rotating plates, and is controlled Each rotating plate is rotated to be perpendicular to the filtering member in the filtering state, and is rotated to the front side toward the filtering member in the cleaning state; and the cleaning liquid discharge unit, At the bottom of the housing body, the cleaning liquid adhered particulate matter discharged from the housing body.
本发明所涉及的氢氧化锂制备系统,还可以具有这样的特征:吸收塔为降膜吸收塔,吸收塔还具有:换向阀,安装在液体排出口部上,具有一个入口和两个出口,入口与液体排出口部相连通,一个出口作为第一出口与母液储存装置相连通,另一个出口作为第二出口与苛化装置相连通。The lithium hydroxide preparation system according to the present invention may further have the following feature: the absorption tower is a falling film absorption tower, and the absorption tower further has: a reversing valve installed on the liquid discharge port portion, having one inlet and two outlets The inlet is in communication with the liquid discharge port, one outlet is connected to the mother liquor storage device as a first outlet, and the other outlet is in communication with the causticizing device as a second outlet.
本发明所涉及的氢氧化锂制备系统,还可以具有这样的特征:吸收塔还具有:pH值检测控制器,与液体排出口部和换向阀都相连,检测位于液体排出口部中的吸收溶液的pH值,并在检测结果为pH值≤13时,控制换向阀转向至第二出口,使吸收溶液排向苛化装置;否则,控制换向阀转向至第一出口,使吸收溶液排向母液储存装置。 The lithium hydroxide preparation system according to the present invention may further have the following feature: the absorption tower further has: a pH value detecting controller connected to the liquid discharge port portion and the reversing valve to detect absorption in the liquid discharge port portion The pH value of the solution, and when the detection result is pH value ≤ 13, the control reversing valve is turned to the second outlet to discharge the absorption solution to the causticizing device; otherwise, the control reversing valve is turned to the first outlet to make the absorption solution Discharge to the mother liquor storage device.
本发明所涉及的氢氧化锂制备系统,还可以具有这样的特征:从吸收剂入口部进入的吸收剂的流量为0.5~1m3/min,从气体入口部进入的过滤后空气的流量为1~20m3/min。The lithium hydroxide production system according to the present invention may further have a feature that the flow rate of the absorbent entering from the inlet portion of the absorbent is 0.5 to 1 m 3 /min, and the flow rate of the filtered air entering from the gas inlet portion is 1 ~20m 3 /min.
本发明所涉及的氢氧化锂制备系统,还可以具有这样的特征:气体干燥装置包括:气液旋风分离器,具有:气液入口部,与气体排出口部相连通,让无二氧化碳气体进入;分离部,与气液入口部相连通,对进入的无二氧化碳气体进行气液分离;以及出口部,与分离部相连通,将分离后的低含水量气体排出;和干燥器,与出口部相连通,对低含水量气体进行干燥。The lithium hydroxide preparation system according to the present invention may further have the following feature: the gas drying device comprises: a gas-liquid cyclone separator having a gas-liquid inlet portion communicating with the gas discharge port portion to allow carbon dioxide-free gas to enter; a separating portion communicating with the gas-liquid inlet portion to perform gas-liquid separation of the entering carbon dioxide-free gas; and an outlet portion communicating with the separating portion to discharge the separated low-moisture gas; and a dryer connected to the outlet portion Pass, dry the low water content gas.
本发明所涉及的氢氧化锂制备系统,还可以具有这样的特征:出口部包括第一出口单元和第二出口单元,第一出口单元与苛化装置、浓缩结晶装置和晶体干燥装置相连通,用于供给一部分的低含水量气体,第二出口单元与干燥器相连通,将另一部分的低含水量气体送往干燥器。The lithium hydroxide preparation system according to the present invention may further have the feature that the outlet portion includes a first outlet unit and a second outlet unit, and the first outlet unit is connected to the causticizing device, the concentrated crystallization device, and the crystal drying device. For supplying a portion of the low moisture gas, the second outlet unit is in communication with the dryer and another portion of the low moisture gas is sent to the dryer.
本发明所涉及的氢氧化锂制备系统,还可以具有这样的特征:干燥器具有:至少两个干燥塔和第一转向阀,每个干燥塔都具有:导入部,与出口部相连通,将低含水量气体导入;干燥部,与导入部相连通,填装有干燥剂,吸收低含水量气体中的水分;导出部,与干燥部相连通,将干燥后得到的保护气体导出;以及加热部,安装在干燥部上,对干燥剂进行加热,除去吸附的水分,第一转向阀安装在所有的干燥塔与出口部之间,具有:一个第一进入口和至少两个第一排出口,第一进入口与出口部相连通,至少两个第一排出口分别与至少两个干燥塔的导入部相连通,气体干燥装置还包括干燥控制单元,干燥控制单元与第一转向阀和两个加热部相连,能够在至少一个干燥塔吸水达到饱和时,控制第一转向阀转向至与另外的至少一个干燥塔的导入部相连通,并控制达到饱和的至少一个干燥塔的加热部进行加热。The lithium hydroxide preparation system according to the present invention may further have the following features: the dryer has: at least two drying towers and a first steering valve, each drying tower having: an introduction portion communicating with the outlet portion, a low-moisture gas is introduced; the drying portion is connected to the introduction portion, and is filled with a desiccant to absorb moisture in the low-moisture gas; the lead-out portion is connected to the drying portion, and the protective gas obtained after drying is discharged; and heating a portion installed on the drying portion to heat the desiccant to remove the adsorbed moisture. The first steering valve is installed between all the drying towers and the outlet portion, and has a first inlet port and at least two first discharge ports. The first inlet port is in communication with the outlet portion, and the at least two first outlet ports are respectively in communication with the introduction portions of the at least two drying towers, the gas drying device further comprising a drying control unit, the drying control unit and the first steering valve and two The heating portions are connected to control the first steering valve to be steered to communicate with the introduction portion of the other at least one drying tower when the water absorption of the at least one drying tower reaches saturation. Saturation control to achieve at least one heating unit for heating the drying tower.
本发明所涉及的氢氧化锂制备系统,还可以还包括:储气装置,与两个干燥塔的导出部都相连通,存储保护气体,干燥器还具有第二转向阀,该第二转向阀安装在两个干燥塔与储气装置之间,具有:两个第二进入口和一个第二排出口,两个第二进入口分别与两个干燥塔的导出部相连通,第二进入口与储气装置相连通,干燥控制单元还与第二转向阀相连,在一个干燥塔吸水达到饱和时,还控制第二转向阀转向至与另一个干燥塔的导出部相连通。The lithium hydroxide preparation system according to the present invention may further include: a gas storage device communicating with the lead-out portions of the two drying towers to store the shielding gas, the dryer further having a second steering valve, the second steering valve Installed between two drying towers and a gas storage device, having two second inlet ports and one second outlet port, the two second inlet ports respectively communicating with the outlet portions of the two drying towers, the second inlet port In communication with the gas storage device, the drying control unit is further coupled to the second steering valve to control the second steering valve to be in communication with the outlet portion of the other drying tower when the water absorption of one of the drying towers is saturated.
发明的作用与效果The role and effect of the invention
根据本发明的氢氧化锂制备系统,因为保护气体供给子系统中,过滤装置能够滤除空气中的颗粒物,吸收塔能够利用浓缩结晶装置中析出晶体后余下的氢氧化锂母液作为吸收剂来对过滤后空气中的二氧化碳进行吸收,由于氢氧化锂母液中氢氧根浓度非常高,因此能够充分吸收空气中的二氧化碳,从而达到有效地去除二氧化碳的目的,进一步,再由气体干燥装置来对无二氧化碳气体进行干燥得到保护气体,并且供给装置能够将这些保护气体提供给制备子系统,从而能够采用空气这种廉价的气体作为制备子系统中大量使用的保护气体,有效地降低了氢氧化锂的制备成本。 According to the lithium hydroxide preparation system of the present invention, since the filtering device is capable of filtering out particulate matter in the air in the protective gas supply subsystem, the absorption tower can utilize the remaining lithium hydroxide mother liquor as the absorbent after the crystal is precipitated in the concentrated crystallization device. After the filtered carbon dioxide in the air is absorbed, since the concentration of hydroxide in the lithium hydroxide mother liquor is very high, the carbon dioxide in the air can be sufficiently absorbed, thereby achieving the purpose of effectively removing carbon dioxide, and further, the gas drying device is used to The carbon dioxide gas is dried to obtain a shielding gas, and the supply device can supply the shielding gas to the preparation subsystem, so that an inexpensive gas such as air can be used as a shielding gas used in a large quantity in the preparation subsystem, thereby effectively reducing lithium hydroxide. Preparation costs.
并且,由于至少一个过滤构件中的至少一层过滤网为磁性过滤网,所以能够对磁性异物进行吸附,从而有效地除去磁性异物。Further, since at least one of the at least one filter member is a magnetic filter, the magnetic foreign matter can be adsorbed, thereby effectively removing the magnetic foreign matter.
图1是本发明涉及的保护气体供给子系统在实施例中的结构示意图;1 is a schematic structural view of a shielding gas supply subsystem according to an embodiment of the present invention;
图2是本发明涉及的保护气体供给子系统实施例中的结构框图;2 is a structural block diagram of an embodiment of a shielding gas supply subsystem according to the present invention;
图3是本发明涉及的过滤装置在实施例中的结构示意图;3 is a schematic structural view of a filter device according to an embodiment of the present invention;
图4是本发明的涉及的清洗构件在实施例中的结构框图;Figure 4 is a block diagram showing the structure of a cleaning member according to the present invention in an embodiment;
图5(a)是本发明的涉及的清洗板单元在实施例中从正面看的结构示意图;Figure 5 (a) is a schematic structural view of the cleaning plate unit according to the present invention as seen from the front in the embodiment;
图5(b)是本发明的涉及的清洗板单元在实施例中从背面看的结构示意图;Figure 5 (b) is a schematic view showing the structure of the cleaning plate unit according to the present invention as seen from the back in the embodiment;
图6是本发明涉及的清洗控制单元在实施例中的控制流程图;Figure 6 is a control flow chart of the cleaning control unit according to the present invention in an embodiment;
图7是本发明涉及的pH值检测控制器在实施例中的控制流程图;Figure 7 is a control flow chart of the pH detecting controller according to the present invention in the embodiment;
图8是本发明涉及的气液旋风分离器在实施例中的结构示意图;以及Figure 8 is a schematic structural view of a gas-liquid cyclone separator according to the present invention in an embodiment;
图9是本发明涉及的干燥控制单元在实施例中的控制流程图。Figure 9 is a control flow chart of the drying control unit according to the present invention in the embodiment.
以下参照附图对本发明所涉及的氢氧化锂制备系统作详细阐述。Hereinafter, the lithium hydroxide production system according to the present invention will be described in detail with reference to the accompanying drawings.
<实施例><Example>
本实施例中,氢氧化锂制备系统用于制备电池级的氢氧化锂产品,它包括制备子系统和保护气体供给子系统。In this embodiment, a lithium hydroxide preparation system is used to prepare a battery-grade lithium hydroxide product, which includes a preparation subsystem and a shielding gas supply subsystem.
制备子系统采用粗碳酸锂、工业级碳酸锂、氯化锂、硫酸锂等锂盐作为原料来制备氢氧化锂产品,它包括:原料除杂装置、苛化装置、浓缩结晶装置、晶体干燥装置、破碎装置以及筛分包装装置。The preparation subsystem uses a lithium salt such as crude lithium carbonate, industrial grade lithium carbonate, lithium chloride or lithium sulfate as a raw material to prepare a lithium hydroxide product, which comprises: a raw material removing device, a causticizing device, a concentrated crystallization device, and a crystal drying device. , crushing device and screening packaging device.
保护气体供给子系统用于除去空气中的二氧化碳,从而为氢氧化锂的制备工艺提供无二氧化碳的空气作为保护气体。The shielding gas supply subsystem is used to remove carbon dioxide from the air to provide carbon dioxide-free air as a shielding gas for the lithium hydroxide preparation process.
图1是本发明涉及的保护气体供给子系统在实施例中的结构示意图;图2是本发明涉及的保护气体供给子系统实施例中的结构框图。1 is a schematic structural view of a protective gas supply subsystem according to an embodiment of the present invention; and FIG. 2 is a structural block diagram of an embodiment of a protective gas supply subsystem according to the present invention.
如图1和2所示,保护气体供给子系统1000包括过滤装置100、母液储存装置200、吸收塔300、气体干燥装置400、供给装置500以及储气装置600。As shown in FIGS. 1 and 2, the shielding
图3是本发明涉及的过滤装置在实施例中的结构示意图。Fig. 3 is a schematic view showing the structure of a filtering device according to the present invention in an embodiment.
如图1和3所示,过滤装置100用于滤除空气中的颗粒物,它包括:壳体11、三个过滤构件12和清洗构件13。As shown in FIGS. 1 and 3, the
壳体11用不锈钢(表面喷四氟材质)或塑料材料制成,并且不具有磁性。它包括壳本体111、进气口部112和出气口部113。壳本体111为中空结构。The
进气口部112位于壳本体111的右侧,它包括进气口112a和密封盖(图中未显示)。
进气口112a用于让空气进入壳体11,密封盖与进气口112a相匹配,用于在清洗状态时将进气口112a盖合封闭。The
出气口部113位于壳本体111的左侧,它包括风机113a和出口部分113b。风机113a的进风端朝向过滤构件12,风机113a的出风端朝向出口部分113b送风,即、在图1中,空气从右向左进入壳体11进行过滤。出口部分113b具有一个空气出口113b-1,让过滤后的空气排出。本实施例中,风机113a的进气量为15-20m3/min,过滤构件12的透气量为20-30m3/min。The
三个过滤构件12都安装在壳本体111内,位于进气口部112和出气口部113之间,对从进气口部112进来的空气进行过滤。每个过滤构件12都包括数层过滤网和固定这些过滤网的固定框。将这三个过滤构件12沿着从右至左的空气进入方向,依次记为:第一过滤构件121、第二过滤构件122和第三过滤构件123。第一过滤构件121过滤颗粒较大的杂物和粉尘;第二过滤构件122过滤较细的花粉等小颗粒物;第三过滤构件123过滤0.1微米至0.5微米的微小颗粒物。The three
本实施例中,第一过滤构件121和第二过滤构件122的位于最外层的过滤网都为磁性过滤网,即、一共设有四层磁性过滤网。该磁性过滤网为电磁铁过滤网,通电后具有吸磁性,磁能10000高斯,能够吸附空气中的磁性异物。In this embodiment, the filter screens of the
图4是本发明的涉及的清洗构件在实施例中的结构框图。Fig. 4 is a block diagram showing the structure of a cleaning member according to the present invention in an embodiment.
如图3和4所示,清洗构件13用于对三个过滤构件12进行清洁,并将清洁出的颗粒物清洗出壳体11,它包括:两个清洗板单元131、吹气板单元132、第二清洗液分布管133、供气单元134、供水单元135、三个超声振动件136、清洗液排出单元137、以及清洗控制单元138。As shown in FIGS. 3 and 4, the cleaning
两个清洗板单元131都安装在壳本体111内,每个清洗板单元131都位于相邻两个过滤构件12之间,如图1所示,一个清洗板单元131位于第一过滤构件121和第二过滤构件122之间,另一个清洗板单元131位于第二过滤构件122和第三过滤构件123之间。Two
图5(a)是本发明的涉及的清洗板单元在实施例中从正面看的结构示意图;图5(b)是本发明的涉及的清洗板单元在实施例中从背面看的结构示意图。Fig. 5 (a) is a schematic view showing the structure of the cleaning plate unit according to the present invention as seen from the front in the embodiment; and Fig. 5 (b) is a structural view showing the cleaning plate unit according to the present invention as seen from the back in the embodiment.
如图5所示,每个清洗板单元131都具有转动板131a、多个喷气嘴131b以及第一清洗液分布管131c。As shown in FIG. 5, each of the
转动板131a可转动地安装在壳本体111内,转动板131a包括板主体131a-1和转动轴131a-2。板主体131a-1通过转动轴131a-2安装在壳本体111中,转动轴131a-2固定在板主体131a-1的中间,转动轴131a-2可转动地安装在壳本体111的两个侧壁上。The
另外,在转动板131a的内部设有与所有的喷气嘴131b相连通的供气通道(图中未显示),该供气通道的入口A从转动轴131a-2的内部延伸出至与供气单元134相连通。Further, inside the
并且,转动板131a的内部还设有与第一清洗液分布管131c相连通的第一供水通道
(图中未显示),该第一供水通道的入口B从转动轴131a-2的内部延伸出至与供水单元135相连通。Moreover, the inside of the
多个喷气嘴131b分成八排均匀安装在转动板131a的正面(即、朝向进气口112a的一面)上,以转动轴131a-2为中线,上下各四排,用于向位于其右侧的过滤构件12喷气,从而将颗粒物从过滤构件12的过滤网中喷出。本实施例中,喷气嘴131b喷出的是高压气体,这样将颗粒物喷出的效果会更加好,气体压强为0.1-0.5Mpa,喷气嘴到过滤构件的距离在10-50cm范围内,喷气嘴131b按照1-10次/秒的速度间歇性地向过滤构件12喷气,间歇性喷气不仅能够提高将颗粒物喷出的效果,而且还能够节省用气量。The plurality of
喷气嘴131b从左向右对过滤构件12进行喷气后,过滤构件12内积存的颗粒物就会从过滤构件12的过滤网中喷出,并且大部分的颗粒物会被喷向另一个转动板131a的背面,例如,位于第二过滤构件122左侧的转动板131a的喷气嘴131b向第二过滤构件122喷气后,大部分的颗粒物会被喷向位于第二过滤构件122右侧的转动板131a的背面。After the
第一清洗液分布管131c安装在转动板131a的背面上,并位于背面的上部,能够沿着转动板131a的背面喷淋清洗液,处于清洗状态时,清洗液自上而下喷淋,吸收高压气吹出来的颗粒物,将喷到背面上的颗粒物淋洗下来,并将背面近旁的空气中的一部分颗粒也连带着淋洗下来,然后附着有颗粒物的清洗液沿着转动板131a的背面流下。第一清洗液分布管131c的长度与转动板131a的长度相当,第一清洗液分布管131c沿着径向方向均匀分布有出液孔。The first cleaning
这里,采用的清洗液优选为对颗粒物有粘性的,这样可以增加颗粒被清洗液吸附和粘着的效率。例如,采用具有粘性的泡沫除尘剂,泡沫除尘剂的成分可以为:添加有1~5%(体积分数)的十二烷基硫酸钠、脂肪醇聚氧乙烯醚硫酸钠、松香皂类发泡剂的水溶液。Here, the cleaning liquid used is preferably viscous to the particulate matter, which increases the efficiency of adsorption and adhesion of the particles by the cleaning liquid. For example, using a viscous foam dedusting agent, the foam dedusting agent may be composed of: 1 to 5% by volume of sodium lauryl sulfate, a fatty alcohol polyoxyethylene ether sulfate, and rosin soap foaming. An aqueous solution of the agent.
吹气板单元132安装在壳本体111内,位于出气口部112与第三过滤构件123之间。吹气板单元132具有转动板132a和多个喷气嘴132b。转动板132a和喷气嘴132b的结构与上述转动板131a和喷气嘴131b的结构和相应的功能都一样,喷气嘴132b的数量也与清洗板单元131中的喷气嘴131b数量一样,故不再赘述。同样的,吹气板单元132也能够通过喷气嘴132b对向位于其右侧的第三过滤构件123喷气,从而将颗粒物从过滤构件12的过滤网中喷出。The
第二清洗液分布管133安装在壳本体111的最右侧的右侧壁的顶部,顺着壳本体111的右侧壁喷淋清洗液,该第二清洗液分布管133的结构和相应的功能都与第一清洗液分布管131c一样,即、第二清洗液分布管133的长度与安装该第二清洗液分布管133的右侧壁的长度相当,第二清洗液分布管133沿着径向方向均匀分布有出液孔,喷淋的清洗液也跟第一清洗液分布管131c一样。The second cleaning
另外,第二清洗液分布管133的进液口(图中未显示)延伸出壳本体111,并与供水单元135相连通。In addition, a liquid inlet (not shown) of the second cleaning
供气单元134与三个转动板131a和132a的三个供气通道的入口A都相连,通过供
气通道为喷气嘴131b供气。The
供水单元135与第一供水通道的入口B和第二清洗液分布管133的进液口相连,为第一清洗液分布管131c和第二清洗液分布管133供水。The
三个超声振动件136分别安装在三个过滤构件12的三个固定框上,在清洗状态时,通过超声振动件136带动过滤构件12振动,在超声波的作用下,过滤网上的粉尘会加速脱离,从而可以提高清洗效果。The three ultrasonic vibrating
如图3所示,清洗液排出单元137安装在壳本体111的底部,将附着有颗粒物的清洗液从壳本体111内排出。本实施例中,清洗液排出单元137包括三个清洗液排出阀137a,清洗液排出阀137a的数量正好与第一清洗液分布管131c和第二清洗液分布管133的总数量相等。如图1所示,从右往左看,三个清洗液排出阀137a分别安装在壳本体111的右侧壁与第一过滤构件121之间的壳本体111的底壁安装部111a上、第一过滤构件121与第一块清洗板单元131之间的底壁安装部111a上、第二过滤构件122与第二块清洗板单元131之间的底壁安装部111a上。As shown in FIG. 3, the cleaning
并且,每个底壁安装部111a都呈横截面从上至下递减的漏斗形,这种形状能够很好地引导清洗液流入清洗液排出阀137a,并从清洗液排出阀137a排出。Further, each of the bottom wall mounting portions 111a has a funnel shape whose cross section decreases from top to bottom, and this shape can well guide the cleaning liquid to flow into the cleaning
如图4所示,清洗控制单元138与两个清洗板单元131、吹气板单元132、第二清洗液分布管133、供气单元134、供水单元135、三个超声振动件136以及清洗液排出单元137都相连,用于控制它们的运行。As shown in FIG. 4, the
另外,清洗控制单元138还与四层电磁铁过滤网(图中未显示)和风机113a相连,能够控制四层电磁铁过滤网进行通电和断电,并控制风机113a的开启和关闭。In addition, the
具体地,在过滤状态时,清洗控制单元138能够控制所有的转动板131a和132a都转动至与对应的过滤构件12相垂直,并控制四层电磁铁过滤网通电使其具有磁性,然后控制风机113a启动抽气。通过将转动板131a和132a都转动至与对应的过滤构件12相垂直可以保证空气的正常流通,使得过滤过程顺利进行。Specifically, in the filtered state, the
在清洗状态时,清洗控制单元138能够控制风机113a停止运转,四层电磁铁过滤网断电消磁,并控制所有的转动板131a和132a都转动至正面平行朝向对应的过滤构件12,然后控制三个超声振动件136进行振动、供气单元134向喷气嘴131b供气、供水单元135向第一清洗液分布管131c和第二清洗液分布管供水,进一步控制所有的喷气嘴131b和132b进行喷气,并控制第一清洗液分布管131c和第二清洗液分布管133喷淋清洗液,还控制三个清洗液排出阀137a开启进行排液。In the cleaning state, the
在清洗状态结束后,清洗控制单元138控制所有的喷气嘴131b和132b停止喷气,并控制第一清洗液分布管131c和第二清洗液分布管133停止喷淋清洗液,还控制供气单元134停止供气、供水单元135停止供水,进一步在排液结束后控制三个清洗液排出阀137a关闭。After the cleaning state is over, the
这里所说的清洗状态是指:过滤装置10的通风量下降到90%,需要对过滤构件进
行清洗的状态;或者是指:达到设定的清洗周期,例如,设定的清洗周期可以为每隔一天清洗一次。本实施例中,以清洗周期为例进行说明。The cleaning state referred to herein means that the ventilation amount of the
图6是本发明涉及的清洗控制单元在实施例中的控制流程图。Fig. 6 is a control flow chart of the cleaning control unit according to the present invention in the embodiment.
如图6所示,清洗控制单元138的工作流程包括如下步骤:As shown in FIG. 6, the workflow of the
步骤S1-1:Step S1-1:
控制所有的转动板131a和132a都转动至与对应的过滤构件12相垂直的水平状态,然后进入步骤S1-2;Controlling all of the
步骤S1-2:Step S1-2:
控制四层电磁铁过滤网通电,然后进入步骤S1-3;Controlling the four-layer electromagnet filter to be energized, and then proceeds to step S1-3;
步骤S1-3:Step S1-3:
控制风机113a启动抽气,然后进入步骤S1-4;
步骤S1-4:Step S1-4:
判断是否到达清洗周期,在判断为是进入步骤S1-5,否则返回步骤S1-2;Determining whether the cleaning cycle is reached, it is determined that the process proceeds to step S1-5, otherwise returns to step S1-2;
步骤S1-5:Step S1-5:
控制风机113a停止运转,然后进入步骤S1-6;
步骤S1-6:Step S1-6:
控制四层电磁铁过滤网断电消磁,然后进入步骤S1-7;Controlling the four-layer electromagnet filter power off degaussing, and then proceeds to step S1-7;
步骤S1-7:Step S1-7:
控制所有的转动板131a和132a都转动至正面平行朝向对应的过滤构件12的竖直状态,然后进入步骤S1-8;Controlling all of the
步骤S1-8:Step S1-8:
控制三个超声振动件136进行振动,然后进入步骤S1-9;Controlling the three ultrasonic vibrating
步骤S1-9:Step S1-9:
控制供气单元134向喷气嘴131b供气,供水单元135向第一清洗液分布管131c和第二清洗液分布管供水,然后进入步骤S1-10;Control the
步骤S1-10:Step S1-10:
控制所有的喷气嘴131b和132b进行喷气,然后进入步骤S1-11;Control all the
步骤S1-11:Step S1-11:
控制第一清洗液分布管131c和第二清洗液分布管133喷淋清洗液,然后进入步骤S1-12;Control the first cleaning
步骤S1-12:Step S1-12:
控制三个清洗液排出阀137a开启进行排液,然后进入步骤S1-13;Controlling three cleaning
步骤S1-13:Step S1-13:
判断是否完成设定的清洗时间,在判断为是进入步骤S1-14,否则返回步骤S1-10;Determining whether the set cleaning time is completed, and determining to proceed to step S1-14, otherwise returning to step S1-10;
步骤S1-14: Step S1-14:
控制所有的喷气嘴131b和132b停止喷气、第一清洗液分布管131c和第二清洗液分布管133停止喷淋清洗液、供气单元134停止供气、供水单元135停止供水,三个清洗液排出阀137a关闭,然后进入结束状态。Control all the
另外,在本实施例中,过滤装置100还可以包括图中未显示的固液过滤装置和清洗液循环利用器。固液过滤装置与三个清洗液排出阀137a相连,用于对排出的吸附有颗粒物的清洗液进行固液分离,将颗粒物分离出清洗液,并将分离后的清洗液排向清洗液循环利用器。清洗液循环利用器的入口与分离器固液连收集其排出的清洗液,出口与第一清洗液分布管131c和第二清洗液分布管133相连,将收集的清洗液再提供给第一清洗液分布管131c和第二清洗液分布管133。这样就可以循环利用清洗液,从而进一步降低成本。Further, in the present embodiment, the
又如图1所示,母液储存装置200存储有浓缩结晶装置中析出晶体后余下的氢氧化锂母液,由于氢氧化锂母液中氢氧根含量非常高,因此能够高效地吸收空气中的二氧化碳。Further, as shown in Fig. 1, the mother
本实施例中,吸收塔300具有气体入口部31、吸收剂入口部32、塔体33、气体排出口部34、液体排出口部35、换向阀36、以及pH值检测控制器37。In the present embodiment, the
吸收塔300的主体部分为常见的降膜吸收塔,这里说的主体部分包括:气体入口部31、吸收剂入口部32、塔体33、气体排出口部34以及液体排出口部35。The main body portion of the
气体入口部31与过滤装置100中的出气口部113相连通,将过滤后空气引入。从气体入口部31进入的过滤后空气的流量为1~20m3/min。The
吸收剂入口部32与母液储存装置200相连通,引入氢氧化锂母液作为吸收剂。从吸收剂入口部32进入的吸收剂的流量为0.5~1m3/min。The
塔体33与气体入口部31相连通,并与吸收液入口部32相连通,用吸收剂来对过滤后空气中的二氧化碳进行吸收以获得无二氧化碳气体。塔体33内氢氧化锂母液吸收二氧化碳后生成的碳酸锂,碳酸锂因溶解度小会结晶出晶体,因此塔体33的下部还安装有固液分离器33-1,能够将晶体与吸收了二氧化碳的吸收剂溶液相分离,并通过管道将碳酸锂晶体送至苛化装置作为原料进行苛化反应,重新生成氢氧化锂。The
气体排出口部34与塔体33相连通,将无二氧化碳气体排出。The gas
液体排出口部35与塔体33相连通,将吸收了二氧化碳的吸收剂溶液作为吸收溶液排出。The liquid
换向阀36安装在液体排出口部35上,具有一个入口和两个出口,入口与液体排出口部35相连通,一个出口作为第一出口与母液储存装置200相连通,另一个出口作为第二出口与苛化装置相连通。The reversing
pH值检测控制器37与液体排出口部35和换向阀36都相连,检测位于液体排出口部35中的吸收溶液的pH值,并在检测结果为pH值≤13时,表明吸收溶液中存在大量的碳酸锂(氢氧化锂母液吸收二氧化碳后会生成碳酸锂),控制换向阀36转向至第二出
口,使吸收溶液排向苛化装置,进行苛化反应,重新生成氢氧化锂;否则,表明吸收溶液还具有良好的吸收二氧化碳的性能,控制换向阀36转向至第一出口,使吸收溶液排向母液储存装置200继续循环使用。The
图7是本发明涉及的pH值检测控制器在实施例中的控制流程图。Fig. 7 is a control flow chart of the pH detecting controller according to the present invention in the embodiment.
如图7所示,pH值检测控制器37的工作流程包括如下步骤:As shown in FIG. 7, the workflow of the
步骤S2-1:Step S2-1:
检测位于液体排出口部35中的吸收溶液的pH值,然后进入步骤S2-2;Detecting the pH value of the absorption solution located in the liquid
步骤S2-2:Step S2-2:
判断pH值≤13是否成立,如果是进入步骤S2-3,否则进入步骤S2-4;Determine whether the pH value ≤ 13 is established, if it is to proceed to step S2-3, otherwise proceed to step S2-4;
步骤S2-3:Step S2-3:
控制换向阀36转向至第二出口,使吸收溶液排向苛化装置,然后返回步骤S2-2;Controlling the
步骤S2-4:Step S2-4:
控制换向阀36转向至第一出口,使吸收溶液排向母液储存装置200,然后返回步骤S2-2。The
pH值检测控制器37不断重复上述过程,直到被关机。The
气体干燥装置400与气体排出口部34相连通,对无二氧化碳气体进行干燥,得到保护气体。气体干燥装置400包括气液旋风分离器41、干燥器42以及干燥控制单元43。The
图8是本发明涉及的气液旋风分离器在实施例中的结构示意图。Figure 8 is a schematic view showing the structure of a gas-liquid cyclone separator according to the present invention in an embodiment.
如图1和8所示,气液旋风分离器41具有气液入口部411、分离部412、气出口部413以及液出口部414。As shown in FIGS. 1 and 8, the gas-
气液入口部411与气体排出口部34相连通,让无二氧化碳气体进入气液旋风分离器41。气液入口部411中安装有雾化水喷头411-1,用于清洗空气中可能带入的微量碳酸锂溶液,并使空气中的微小液滴聚集,增加分离效果。The gas-
分离部412与气液入口部411相连通,对进入的无二氧化碳气体进行气液分离。The
气出口部413与分离部412相连通,将分离后的低含水量气体排出。气出口部413包括第一出口单元413a和第二出口单元413b,The
第一出口单元413a与苛化装置、浓缩结晶装置和晶体干燥装置这些对保护气体中含水量要求不高的装置相连通,用于将一部分的低含水量气体直接供给这些装置。The
第二出口单元413b与干燥器42相连通,将另一部分的低含水量气体送往干燥器42。The second outlet unit 413b is in communication with the
液出口部414安装在分离部412的底部,用于将分离后的液体排出。The
干燥器42与出口部413相连通,对低含水量气体进行干燥。它具有两个干燥塔421和一个第一转向阀422和第二转向阀423。The
每个干燥塔421都具有导入部421a、干燥部421b、导出部421c以及加热部421d。Each drying
导入部421a与气出口部413相连通,将低含水量气体导入。The
干燥部421b与导入部421a相连通,填装有干燥剂,吸收低含水量气体中的水分,
得到高度干燥的气体。采用的干燥剂为高吸水干燥剂,并且,该干燥剂吸水后,经加热,吸收的水分能够被蒸发出,恢复吸水性能,从而能够被重复使用。The drying
导出部421c与干燥部421b相连通,将干燥后得到的保护气体导出。The lead-out unit 421c communicates with the drying
加热部421d安装在干燥部421b上,对干燥剂进行加热,除去吸附的水分。The heating unit 421d is attached to the
第一转向阀422安装在两个干燥塔421与气出口部413之间,具有:一个第一进入口和两个第一排出口。第一进入口与气出口部413相连通,两个第一排出口分别与两个干燥塔42的导入部421a相连通,The
第二转向阀423安装在两个干燥塔42与储气装置40之间。第二转向阀423具有两个第二进入口和一个第二排出口,两个第二进入口分别与两个干燥塔42的导出部421c相连通,第二进入口与储气装置600相连通,The
干燥控制单元43与第一转向阀422和两个加热部421d以及第二转向阀423相连。它能够在一个干燥塔421吸水达到饱和时,控制第一转向阀422转向至与另一个干燥塔421的导入部421a相连通,并控制第二转向阀423转向至与另一个干燥塔42的导出部421c相连通,还控制达到饱和的干燥塔42的加热部421d进行加热,从而将吸收的水分蒸发出,并恢复吸水性能。The drying
图9是本发明涉及的干燥控制单元在实施例中的控制流程图。Figure 9 is a control flow chart of the drying control unit according to the present invention in the embodiment.
如图9所示,干燥控制单元43的工作流程包括如下步骤,为了便于描述,以下将两个干燥塔421分别记为第一干燥塔421和第二干燥塔421,并以第一干燥塔421吸水性能达到饱和为例进行说明:As shown in FIG. 9, the workflow of the drying
步骤S3-1:Step S3-1:
控制第一转向阀422和第二转向阀423分别与第一干燥塔421的导入部421a和导出部421c相连通,然后进入步骤S3-2;Controlling the
步骤S3-2:Step S3-2:
判断第一干燥塔421的吸水性能是否达到饱和(可以通过例如,吸水时间来判断),在判断为是时进入步骤S3-3,否则返回步骤S3-1;Determining whether the water absorption performance of the
步骤S3-3:Step S3-3:
控制第一转向阀422和第二转向阀423分别转向至与第二干燥塔421的导入部421a和导出部421c相连通,然后进入步骤S3-4;Controlling the
步骤S3-4:Step S3-4:
控制第一干燥塔42的加热部421d进行加热,直到第一干燥塔42恢复吸水性能。The heating portion 421d that controls the first drying
第二干燥塔421达到饱和状态的控制过程也与第一干燥塔421一样,这里不再赘述。The control process in which the
供给装置500与气体干燥装置400和储气装置600相连通,将保护气体提供给制备子系统。供给装置500包括:将第一出口单元413a与苛化装置、浓缩结晶装置和晶体干燥装置相连通并进行送气的管道和气体输送构件,和将储气装置600与破碎装置和筛分包装装置相连通并进行送气的管道和气体输送构件。
The
储气装置600与第二转向阀423的第二排出口相连通,存储高度干燥后的保护气体。The
下面表1~3是以苛化装置和浓缩结晶装置中具体的苛化反应釜、LiOH溶液中转与存储装置,以及LiOH母液中,没有通保护气体、通氮气作为保护气体,以及通本发明的净化后空气作为保护气体分别做的实验数据表,表4是成本比较表,以这些数据为例来证明本方案的效果:Tables 1 to 3 below are specific causticizing reactors, LiOH solution transfer and storage devices, and LiOH mother liquors in a causticizing apparatus and a concentrated crystallization apparatus, without a shielding gas, nitrogen gas as a shielding gas, and the present invention. The experimental data table for the cleaned air as a protective gas, Table 4 is the cost comparison table, using these data as an example to prove the effect of the program:
表1、没有气氛保护下进行的实验Table 1. Experiments without atmosphere protection
表2、氮气保护下实验Table 2, experiment under nitrogen protection
表3、净化空气保护下实验Table 3, experiment under purified air protection
表4、氮气和净化空气成本对比Table 4, nitrogen and clean air cost comparison
从以上表中可以看出,采用本发明的保护气体后,各个装置或者工序中碳酸根的含量得到了有效地抑制,效果与采用惰性气体的相当,但是投入的成本则远低于采用惰性气体作为保护气体的方案。It can be seen from the above table that after the shielding gas of the present invention, the content of carbonate in each device or process is effectively suppressed, and the effect is equivalent to that of using an inert gas, but the input cost is much lower than that of using an inert gas. As a solution to protect the gas.
实施例的作用与效果The role and effect of the embodiment
根据本实施例所描述的氢氧化锂制备系统,因为保护气体供给子系统中,过滤装置能够滤除空气中的颗粒物,吸收塔能够利用浓缩结晶装置中析出晶体后余下的氢氧化锂母液作为吸收剂来对过滤后空气中的二氧化碳进行吸收,由于氢氧化锂母液中氢氧根浓度非常高,因此能够充分吸收空气中的二氧化碳,从而达到有效地去除二氧化碳的目的,进一步,再由气体干燥装置来对无二氧化碳气体进行干燥得到保护气体,并且供给装置能够将这些保护气体提供给制备子系统,从而能够采用空气这种廉价的气体作为制备子系统中大量使用的保护气体,有效地降低了氢氧化锂的制备成本。According to the lithium hydroxide preparation system described in the embodiment, since the filter device can filter out particulate matter in the air in the protective gas supply subsystem, the absorption tower can utilize the remaining lithium hydroxide mother liquor as the absorption after the crystal is precipitated in the concentrated crystallization device. The agent absorbs the carbon dioxide in the filtered air. Since the hydrogen hydroxide concentration in the lithium hydroxide mother liquor is very high, the carbon dioxide in the air can be sufficiently absorbed, thereby achieving the purpose of effectively removing carbon dioxide, and further, the gas drying device The carbon dioxide-free gas is dried to obtain a shielding gas, and the supply device can supply the shielding gas to the preparation subsystem, so that an inexpensive gas such as air can be used as a shielding gas used in a large quantity in the preparation subsystem, thereby effectively reducing hydrogen. The cost of preparing lithium oxide.
进一步,由于干燥控制单元43能够在一个干燥塔421吸水达到饱和时,控制第一转向阀422转向至与另一个干燥塔421的导入部421a相连通,并控制第二转向阀423转向至与另一个干燥塔42的导出部421c相连通,还控制达到饱和的干燥塔42的加热
部421d进行加热,从而将吸收的水分蒸发出,并恢复吸水性能。这样就可以保证气体干燥过程可以连续进行,从而使得整个保护气体供给子系统能够连续供气。Further, since the drying
另外,由于pH值检测控制器37能够检测位于液体排出口部35中的吸收溶液的pH值,并在检测结果为pH值≤13时,控制换向阀36转向至第二出口,使吸收溶液排向苛化装置,进行苛化反应,重新生成氢氧化锂;否则,控制换向阀36转向至第一出口,使吸收溶液排向母液储存装置200继续循环使用。这样就可以合理地循环使用吸收溶液,既能够保证二氧化碳被有效吸收,又能够将达到饱和的吸收溶液重新送回苛化装置进行反应。In addition, since the
气体过滤过程可以连续进行,从而使得整个保护气体供给子系统能够连续供气。The gas filtration process can be carried out continuously so that the entire shielding gas supply subsystem can continuously supply gas.
另外,在过滤装置中,由于两个过滤构件中一共有四层过滤网为磁性过滤网,所以能够对磁性异物进行吸附,从而有效地除去磁性异物。Further, in the filter device, since a total of four filter screens of the two filter members are magnetic filters, magnetic foreign matter can be adsorbed, thereby effectively removing magnetic foreign matter.
并且,由于在过滤状态时,控制单元能够将转动板转动至与过滤构件相垂直,从而确保过滤的正常进行,而在过滤构件积存了大量的粉尘等颗粒物、需要被进行清洗时(在清洗状态时),控制单元能够将转动板转动至使安装有喷气嘴的侧面朝向过滤构件,这样,喷气嘴就能够向过滤构件进行喷气,从而将颗粒物从过滤构件喷出,并将颗粒物喷向壳本体的与过滤构件的另一侧相对向的内侧壁上,再由清洗液分布管沿着该内侧壁喷淋清洗液,并通过清洗液排出阀将附着有颗粒物的清洗液从壳本体内排出。因此,本空气过滤装置能够在不直接对过滤构件进行喷淋的前提下,有效地对滤网构件进行清洁,切实避免了过滤构件吸水后导致的破碎破损和网孔阻塞等问题,确保了过滤构件的过滤效果和使用寿命。Moreover, since the control unit can rotate the rotating plate to be perpendicular to the filtering member in the filtering state, thereby ensuring normal filtration, and when a large amount of dust or the like is accumulated in the filtering member and needs to be cleaned (in the cleaning state) The control unit is capable of rotating the rotating plate such that the side on which the air nozzle is mounted faces the filter member, so that the air nozzle can eject the filter member to eject the particulate matter from the filter member and spray the particulate matter toward the shell body. On the inner side wall opposite to the other side of the filter member, the cleaning liquid is sprayed along the inner side wall by the cleaning liquid distribution pipe, and the cleaning liquid to which the particulate matter adheres is discharged from the casing body through the cleaning liquid discharge valve. Therefore, the air filtering device can effectively clean the filter member without directly spraying the filter member, thereby effectively avoiding problems such as breakage and meshage caused by the filter member after water absorption, and ensuring filtration. The filtering effect and service life of the components.
进一步,由于喷气嘴喷出的是高压气体,这样能够更好地将颗粒物从过滤构件中喷出;并且,由于喷气嘴是按照1-10次/秒的速度间歇性地向过滤构件喷气,这样不仅能够进一步提高将颗粒物喷出的效果,而且还能够节省用气量,从而降低成本。Further, since the air nozzle ejects a high-pressure gas, the particulate matter can be better ejected from the filter member; and, since the air nozzle intermittently ejects the filter member at a speed of 1-10 times/second, Not only can the effect of ejecting particulate matter be further improved, but also the amount of gas used can be saved, thereby reducing the cost.
更进一步,由于在清洗状态时,超声振动件能够带动过滤构件振动,在超声波的作用下,过滤网上的粉尘会加速脱离,从而可以更近一步地提高清洗效果。Further, since the ultrasonic vibrating member can drive the filter member to vibrate in the cleaning state, the dust on the filter net is accelerated and desorbed under the action of the ultrasonic wave, so that the cleaning effect can be further improved.
以上实施例仅仅是对本发明技术方案所做的举例说明。本发明所涉及的氢氧化锂制备系统并不仅仅限定于在以上实施例中所描述的结构,而是以权利要求所限定的范围为准。本发明所属领域技术人员在该实施例的基础上所做的任何修改或补充或等效替换,都在本发明的权利要求所要求保护的范围内。The above embodiments are merely illustrative of the technical solutions of the present invention. The lithium hydroxide preparation system according to the present invention is not limited to the structure described in the above embodiments, but is subject to the scope defined by the claims. Any modifications or additions or equivalent substitutions made by those skilled in the art to which this invention pertains are within the scope of the appended claims.
另外,在上述实施例中,保护气体供给子系统中还包括储气装置,并且干燥器的第二转向阀的第二进入口是与储气装置相连通,这样通过储气装置可以将用不完的高度干燥的保护气体存储起来。在本发明中,根据实际情况,例如,过滤装置进气量不大,导致干燥器干燥后的出气量不大,在这种情况下,保护气体供给子系统中就可以设置储气装置,并让供给装置直接与干燥器的第二转向阀的第二进入口相连通。In addition, in the above embodiment, the shielding gas supply subsystem further includes a gas storage device, and the second inlet port of the second steering valve of the dryer is in communication with the gas storage device, so that the gas storage device can be used The finished highly dry protective gas is stored. In the present invention, depending on the actual situation, for example, the amount of intake air of the filter device is not large, resulting in a small amount of air output after the dryer is dried. In this case, a gas storage device can be disposed in the protective gas supply subsystem, and The supply device is brought into direct communication with the second inlet of the second steering valve of the dryer.
另外,在上述实施例中,采用的都是转向阀来与两个进入连接管或者与两个送出连 接管连。本发明还可以采用两个阀门开关与两个进入连接管连,并采用两个阀门开关与两个送出连接管连,然后控制单元通过对各个阀门开关进行控制来实现导通和关闭功能。In addition, in the above embodiment, all of the steering valves are used to connect with the two inlet pipes or the two. Take over. The invention can also use two valve switches connected with two inlet connecting pipes, and two valve switches are connected with two sending connecting pipes, and then the control unit realizes the turning on and off functions by controlling the respective valve switches.
另外,在上述实施例中,空气过滤装置是具有三个过滤构件,根据实际过滤情况的要求,作为本发明的空气过滤装置,也可以设置仅仅具有两个过滤构件,或者具有三个以上的过滤构件,并且过滤构件的过滤粒径也可以根据情况进行选择。过滤构件数量越多,粒径越细、过滤效果越好,但是过滤时间会变长并且成本也会增大。Further, in the above embodiment, the air filtering device has three filter members, and as the air filtering device of the present invention, it is also possible to provide only two filter members or have three or more filters depending on the actual filtering conditions. The member, and the filter particle size of the filter member can also be selected depending on the situation. The more the number of filter members, the finer the particle size and the better the filtration effect, but the filtration time will be longer and the cost will increase.
另外,在上述实施例中,为了过滤磁性异物,第一过滤构件和第二过滤构件的位于最外层的过滤网都为磁性过滤网,在本发明的空气过滤装置中,只要至少一个过滤构件中的至少一层过滤网为磁性过滤网,就可以对磁性异物进行过滤,同样的,磁性过滤网的数量越多除磁异的效果就越好,但是相应的成本会增加,所以可以根据实际情况的需要来确定磁性过滤网的数量。 Further, in the above embodiment, in order to filter the magnetic foreign matter, the filter mesh located at the outermost layer of the first filter member and the second filter member is a magnetic filter mesh, and in the air filter device of the present invention, at least one filter member is provided At least one layer of the filter is a magnetic filter, and the magnetic foreign matter can be filtered. Similarly, the more the number of the magnetic filter, the better the effect of the magnetic difference, but the corresponding cost will increase, so it can be based on actual conditions. The need for the situation to determine the number of magnetic filters.
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| CN201610964636.7A CN106495188B (en) | 2016-10-28 | 2016-10-28 | Lithium hydroxide preparation system |
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| CN112624158A (en) * | 2020-12-23 | 2021-04-09 | 中南大学 | Novel environment-friendly process for producing lithium hydroxide monohydrate |
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| CN106348318B (en) * | 2016-10-28 | 2017-08-08 | 荆门市格林美新材料有限公司 | Lithia prepares automated system |
| CN106495188B (en) * | 2016-10-28 | 2017-08-08 | 荆门市格林美新材料有限公司 | Lithium hydroxide preparation system |
| JP7072405B2 (en) * | 2018-03-01 | 2022-05-20 | 住友化学株式会社 | Manufacturing method of lithium hydroxide powder, manufacturing method of positive electrode active material for lithium secondary battery, and packaging |
| CN115138426A (en) * | 2022-07-01 | 2022-10-04 | 江西金辉锂业有限公司 | Ultrafine grinding device for battery-grade lithium hydroxide |
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