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申请号:201911267171.X 公开号:CN111004916A 主分类号:C22B3/08
摘要:【中文】本发明公开了一种红土镍矿高压酸浸方法。步骤为:洗矿选矿后的红土镍矿矿浆经浓密后,通过高压泵将浓密矿浆泵入管道化预热器中,在管道化预热器中矿浆与来自闪蒸器中的闪蒸二次蒸汽进行间接换热,末级管道化预热器采用生蒸汽、熔盐或导热油加热。预热后矿浆进入卧式高压反应釜中,在反应釜中加入浓硫酸进行高压浸出,最后浸出矿浆通过闪蒸器降温降压,得酸浸后的红土镍矿矿浆,送入下一工序处理。该方法特别适用于褐铁矿型和过渡型红土镍矿生产氢氧化镍产品。采用本发明提供的方法可显著降低项目投资,提高装置运转率,降低维护费用,节约能耗,从而提高项目盈利能力和生存能力。 【EN】The invention discloses a high-pressure acid leaching method for laterite-nickel ore. The method comprises the following steps: after the laterite-nickel ore pulp subjected to ore washing and dressing is thickened, the thickened pulp is pumped into a channelization preheater through a high-pressure pump, indirect heat exchange is carried out between the pulp and flash-evaporation secondary steam from a flash evaporator in the channelization preheater, and raw steam, molten salt or heat conducting oil is adopted for heating in a final stage channelization preheater. And (3) feeding the preheated ore pulp into a horizontal high-pressure reaction kettle, adding concentrated sulfuric acid into the reaction kettle for high-pressure leaching, cooling and depressurizing the leached ore pulp through a flash evaporator to obtain acid-leached laterite-nickel ore pulp, and feeding the acid-leached laterite-nickel ore pulp into the next working procedure for treatment. The method is particularly suitable for producing nickel hydroxide products from limonite type and transition type laterite-nickel ores. The method provided by the invention can obviously reduce project investment, improve the operation rate of the device, reduce maintenance cost and save energy consumption, thereby improving the profitability and the viability of the project.
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申请号:201911256248.3 公开号:CN111020187A 主分类号:C22B3/08
摘要:【中文】本发明属于湿法冶金领域,公开了一种氢氧化镍的制备方法,包括以下步骤:(1)对红土镍矿进行高压酸浸处理,即得硫酸镍溶液;(2)将氧化镁浆和硫酸镍溶液混合,调节pH至7.8‑8.0,反应,得到沉镍料浆;(3)将沉镍料浆浓缩,得到矿浆和上清液;(4)将部分矿浆作为晶种返回和步骤(2)的氧化镁浆、硫酸镍溶液混合,再将剩余矿浆压滤,得到滤饼和滤液,干燥滤饼,即得氢氧化镍。本发明采用碱性较弱的氧化镁作为沉淀剂避免了局部过碱现象,使溶液中一些杂质离子仍然留在沉镍后的贫液中,不至于大量进入沉镍渣中,提高了沉镍产品的品质,同时降低了整个生产系统除杂的负荷,有利于节约成本提高生产运转率。 【EN】The invention belongs to the field of hydrometallurgy, and discloses a preparation method of nickel hydroxide, which comprises the following steps: (1) carrying out high-pressure acid leaching treatment on the laterite-nickel ore to obtain a nickel sulfate solution; (2) mixing the magnesium oxide slurry and the nickel sulfate solution, adjusting the pH value to 7.8-8.0, and reacting to obtain nickel-precipitating slurry; (3) concentrating the nickel-precipitating slurry to obtain ore slurry and supernatant; (4) and (3) returning part of ore pulp as seed crystal to be mixed with the magnesium oxide pulp and the nickel sulfate solution in the step (2), then carrying out filter pressing on the rest ore pulp to obtain a filter cake and filtrate, and drying the filter cake to obtain the nickel hydroxide. The invention adopts magnesium oxide with weak alkalinity as a precipitator, avoids the phenomenon of local over-alkalinity, ensures that impurity ions in the solution still remain in barren liquor after nickel precipitation, and does not enter nickel precipitation slag in large quantity, improves the quality of nickel precipitation products, reduces the impurity removal load of the whole production system, and is beneficial to saving cost and improving the production operation rate.
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申请号:201911170241.X 公开号:CN111001373A 主分类号:B01J20/04
摘要:【中文】本发明公开了一种掺杂ⅢA元素的锂离子筛及其制备方法和用途,该方法包括以下步骤:将锰源与锂源混合,研磨均匀;加入ⅢA元素的盐或单质,研磨均匀,然后干燥;干燥后的原料干磨成粉末,在氧气或空气氛围中、300~800℃分段焙烧0.5~16h,冷却后得到离子筛前驱体;离子筛前驱体酸洗4~12h,过滤、干燥后得到离子筛;所述ⅢA元素的盐或单质是Na2B4O7·10H2O、硼粉、硫酸铝、氢氧化铝、氯化镓、硝酸镓、氢氧化铟或三氟乙酸铊中的一种以上。用本发明制备的离子筛产品4h吸附量接近20mg/g,酸洗锰损失相比λ‑MnO2作为离子筛减少1倍,优于LiMn2O4作为前驱体制备离子筛的吸附性能。 【EN】The invention discloses a IIIA element-doped lithium ion sieve and a preparation method and application thereof, wherein the method comprises the following steps: mixing a manganese source and a lithium source, and uniformly grinding; adding IIIA element salt or simple substance, grinding uniformly, and drying; the dried raw materials are dry-ground into powder, the powder is roasted for 0.5 to 16 hours in an oxygen or air atmosphere at a temperature of 300 to 800 ℃ in a segmented mode, and an ion sieve precursor is obtained after cooling; pickling the precursor of the ion sieve for 4-12 h, filtering and drying to obtain the ion sieve; the IIIA element salt or simple substance is Na2B4O7·10H2O, boron powder, aluminum sulfate, aluminum hydroxide, gallium chloride, gallium nitrate, indium hydroxide or thallium trifluoroacetate. The 4-hour adsorption capacity of the ionic sieve product prepared by the method is close to 20mg/g, and the loss of acid-washing manganese is compared with that of lambda-MnO2AsThe ion sieve is reduced by 1 time and is superior to LiMn2O4The precursor is used for preparing the adsorption performance of the ionic sieve.
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申请号:201911152879.0 公开号:CN111017896A 主分类号:C01B25/30
摘要:【中文】本发明属于锂离子电池领域,公开了一种正极材料添加剂的制备方法,包括以下步骤:(1)将磷酸铁锂材料与铁源混合,破碎,筛分,得到混合粉料;(2)将混合粉料置于还原性气体中,加热进行还原处理,得到磷铁合金和锂的化合物;(3)将磷铁合金和锂的化合物进行球磨,再进行筛分,得到正极材料添加剂。本发明将制备的磷铁合金和锂化合物作为正极材料添加剂添加到锂离子电池正极材料中,可明显改善锂电池的倍率性能及循环性能,达到优化电池性能的目的。 【EN】The invention belongs to the field of lithium ion batteries, and discloses a preparation method of a positive electrode material additive, which comprises the following steps: (1) mixing a lithium iron phosphate material with an iron source, crushing and screening to obtain mixed powder; (2) placing the mixed powder in reducing gas, heating and reducing to obtain a ferrophosphorus alloy and lithium compound; (3) and ball-milling the ferrophosphorus alloy and the lithium compound, and then screening to obtain the anode material additive. The prepared ferrophosphorus alloy and lithium compound are used as the positive electrode material additive to be added into the positive electrode material of the lithium ion battery, so that the rate capability and the cycle performance of the lithium battery can be obviously improved, and the aim of optimizing the battery performance is fulfilled.
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申请号:201911170253.2 公开号:CN110983045A 主分类号:C22B7/00
摘要:【中文】本发明公开了一种镍钴锰溶液除铁铝的方法,该方法包括以下步骤:向含有铁铝杂质的镍钴锰溶液中加入氧化剂溶液和沉淀剂溶液,搅拌加热至50‑80℃,控制pH值为2.5‑3.0,反应0.5‑1.0h;然后继续加入沉淀剂溶液,搅拌加热至50‑80℃,并控制pH值为4.6‑5.1,陈化,过滤,得到铁铝渣和去除铁铝杂质的镍钴锰溶液。本发明采用两段除铁铝,一段采用控制料液pH值同时并流加料先将铁离子大部分沉淀,二段单向加料加入沉淀剂溶液调节pH值至4.6‑5.1,将铝离子和剩余的铁离子沉淀,整体除铁铝效果高,产生的渣颗粒大,过滤性能好,且渣中夹带的镍钴锰等有价金属少,渣中铁铝含量高。 【EN】The invention discloses a method for removing iron and aluminum from a nickel-cobalt-manganese solution, which comprises the following steps: adding an oxidant solution and a precipitator solution into a nickel-cobalt-manganese solution containing iron-aluminum impurities, stirring and heating to 50-80 ℃, controlling the pH value to be 2.5-3.0, and reacting for 0.5-1.0 h; and then continuously adding the precipitant solution, stirring and heating to 50-80 ℃, controlling the pH value to be 4.6-5.1, aging, and filtering to obtain the iron-aluminum slag and the nickel-cobalt-manganese solution with iron-aluminum impurities removed. The method adopts two sections to remove iron and aluminum, one section adopts the concurrent flow feeding to control the pH value of the feed liquid, firstly most of iron ions are precipitated, the other section adopts the one-way feeding to add the precipitator solution to adjust the pH value to 4.6-5.1, and aluminum ions and the rest iron ions are precipitated.
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申请号:201911179174.8 公开号:CN110994062A 主分类号:H01M10/54
摘要:【中文】本发明涉及一种废旧锂离子电池前段除氟的回收方法以及一种废旧锂离子电池回收前段的除氟处理方法,所述除氟处理方法包括以下步骤:将含氟电池粉料与溶氟助剂溶液混合,加热,搅拌,过滤,得到除氟后电池粉和含氟洗液;将沉锂剂加入含氟洗液,加热,搅拌,过滤,得到含锂渣和除锂后液;将除氟剂加入除锂后液,搅拌,过滤,得到含氟渣和除氟后液;将除氟后液配制成溶氟助剂溶液,重复上述步骤。采用本发明的方法可将废旧锂离子电池在进入回收工序前,将氟含量降低至0.11%以下,除氟率高达90%,有利于解决电池回收工艺中因氟造成的一系列问题;本发明洗液循环利用率高,大幅度减少了水的用量,节省了成本,具有极大的应用前景。 【EN】The invention relates to a method for recycling front-section defluorination of waste lithium ion batteries and a defluorination treatment method for the front-section recycling of the waste lithium ion batteries, wherein the defluorination treatment method comprises the following steps: mixing fluorine-containing battery powder with a fluorine-dissolving auxiliary agent solution, heating, stirring and filtering to obtain defluorinated battery powder and fluorine-containing washing liquor; adding a lithium precipitation agent into fluorine-containing washing liquid, heating, stirring and filtering to obtain lithium-containing slag and a liquid after lithium removal; adding a fluorine removing agent into the liquid after lithium removal, stirring and filtering to obtain fluorine-containing slag and the liquid after fluorine removal; and (4) preparing the defluorinated solution into a fluorine dissolving auxiliary agent solution, and repeating the steps. By adopting the method, the fluorine content of the waste lithium ion battery can be reduced to be below 0.11 percent before entering the recovery process, and the fluorine removal rate is up to 90 percent, thereby being beneficial to solving a series of problems caused by fluorine in the battery recovery process; the washing liquid has high cyclic utilization rate, greatly reduces the using amount of water, saves the cost and has great application prospect.
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申请号:201911348511.1 公开号:CN111041248A 主分类号:C22B47/00
摘要:【中文】本发明属于湿法冶金领域,公开了一种回收含氯废液中有价金属的方法,包括以下步骤:(1)利用氢氧化钠溶液调节含氯废液的pH至0.8‑1.2;(2)将絮凝剂加入步骤1)处理过的含氯废液中,同时加入氢氧化钠溶液调节含氯废液的pH至4.1±0.1,静置,过滤,得到滤液A和滤渣B;(3)将滤液A通过大孔螯合树脂柱,进行柱层析分离,得到溶液C;(4)用硫酸溶液对大孔螯合树脂进行再生,得到脱吸液;(5)将碳酸钠溶液加入溶液C中反应,陈化,过滤,得到碳酸锰;(6)将碳酸钠溶液加入脱吸液中反应,陈化,过滤,得到碳酸锌。本发明的回收方法可将含氯废液中铁、锌、锰等元素逐步进行分离,实现废弃物的资源化,减量化处理。 【EN】The invention belongs to the field of wet metallurgy, and discloses a method for recovering valuable metals in chlorine-containing waste liquid, which comprises the following steps: (1) adjusting the pH value of the chlorine-containing waste liquid to 0.8-1.2 by using a sodium hydroxide solution; (2) adding a flocculating agent into the chlorine-containing waste liquid treated in the step 1), adding a sodium hydroxide solution to adjust the pH of the chlorine-containing waste liquid to 4.1 +/-0.1, standing, and filtering to obtain a filtrate A and a filter residue B; (3) passing the filtrate A through a macroporous chelate resin column, and performing column chromatography separation to obtain a solution C; (4) regenerating the macroporous chelating resin by using a sulfuric acid solution to obtain a desorption liquid; (5) adding a sodium carbonate solution into the solution C for reaction, aging and filtering to obtain manganese carbonate; (6) and adding a sodium carbonate solution into the desorption liquid for reaction, aging and filtering to obtain the zinc carbonate. The recovery method can gradually separate the elements such as iron, zinc, manganese and the like in the chlorine-containing waste liquid, thereby realizing the recycling and reduction treatment of the waste.
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申请号:202010042366.0 公开号:CN111204757A 主分类号:C01B32/215
摘要:【中文】本发明属于锂离子电池领域,公开了一种退役动力电池中石墨净化修复再生的方法,包括以下步骤:将退役动力电池依次经过放电、粗破、热解、细破、分选,得到电极材料粉;将电极材料粉和酸性浸出液混合,搅拌,过滤,得到滤渣;将滤渣与酸性净化液混合,搅拌,过滤,得到粗石墨;将粗石墨加入酸性净化液中,进行水热反应,过滤,得到净化石墨;将净化石墨和活化液混合搅拌,通入臭氧曝气,过滤,得到滤渣;将滤渣水洗,过滤,干燥,得到活化石墨;将活化石墨加入熔融状态的修复剂中进行修复,得到悬浊液;将悬浊液进行喷雾热解,冷却后过筛,得到电池级石墨。本发明采用水热法除杂净化石墨,净化后不会再与杂质发生二次粘结,得到高纯石墨。 【EN】The invention belongs to the field of lithium ion batteries, and discloses a method for purifying, repairing and regenerating graphite in a retired power battery, which comprises the following steps: sequentially carrying out discharging, rough breaking, pyrolysis, fine breaking and sorting on the retired power battery to obtain electrode material powder; mixing the electrode material powder and the acidic leaching solution, stirring and filtering to obtain filter residue; mixing the filter residue with the acidic purification solution, stirring and filtering to obtain crude graphite; adding the coarse graphite into the acidic purification solution, carrying out hydrothermal reaction, and filtering to obtain purified graphite; mixing and stirring purified graphite and activating solution, introducing ozone for aeration, and filtering to obtain filter residue; washing the filter residue with water, filtering and drying to obtain activated graphite; adding activated graphite into a repairing agent in a molten state for repairing to obtain turbid liquid; and carrying out spray pyrolysis on the turbid liquid, cooling and sieving to obtain the battery grade graphite. According to the invention, the hydrothermal method is adopted to remove impurities and purify graphite, and secondary bonding with impurities can not occur after purification, so that high-purity graphite is obtained.
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申请号:201911099470.7 公开号:CN111106331A 主分类号:H01M4/36
摘要:【中文】本发明属于锂离子电池领域,公开了一种层状‑尖晶石相复合正极材料,所述层状‑尖晶石相复合正极材料是由层状结构的LiNixCoyMnzO2与尖晶石相LiM2O4构成的复合材料aLiM2O4·(1‑a)LiNixCoyMnzO2;其中0.5≤x≤0.8,0.02≤y≤0.2,0.02≤z≤0.4,0<a≤0.5,M为Ni、Co和Mn中的一种或几种。本发明采用一次烧结形成缺锂型正极材料,并通过特殊的降温工艺促进部分层状结构转化成尖晶石相,在此基础上二次烧结补锂得到层状‑尖晶石相复合正极材料,改善正极材料的倍率性能的同时能进一步提升材料的热稳定性。 【EN】The invention belongs to the field of lithium ion batteries, and discloses a layered-spinel phase composite positive electrode material which is LiNi with a layered structurexCoyMnzO2With spinel phase LiM2O4Constituting composite material aLiM2O4·(1‑a)LiNixCoyMnzO2(ii) a Wherein x is more than or equal to 0.5 and less than or equal to 0.8, y is more than or equal to 0.02 and less than or equal to 0.2, z is more than or equal to 0.02 and less than or equal to 0.4, and x is more than or equal to 0.5 and less than or equal to 0.8<a is less than or equal to 0.5, and M is one or more of Ni, Co and Mn. The invention adopts one-time sintering to form the lithium-deficient anodeThe material promotes partial lamellar structure to be converted into spinel phase through a special cooling process, and on the basis, the layered-spinel phase composite anode material is obtained by secondary sintering and lithium supplement, so that the rate capability of the anode material is improved, and the thermal stability of the material is further improved.
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申请号:202010021573.8 公开号:CN111082031A 主分类号:H01M4/36
摘要:【中文】本发明属于锂离子电池正极材料领域,公开了一种磷酸锂包覆高镍三元正极材料的制备方法,包括以下步骤:(1)采用高温烧结法制得高镍三元正极材料;(2)将磷酸盐溶于水中,得到包覆液;(3)将高镍三元正极材料和水混合,再加入锂源搅拌,得到悬浊液;(4)将包覆液滴入悬浊液中反应,抽滤,得到湿料;(5)将湿料干燥,过筛,烧结并保温,即得。本发明使用水作为溶剂进行包覆,在工业上有可操作性和可靠性;本发明在水溶液中溶解后再沉淀,属于化学包覆的过程,包覆均匀,包覆剂没有自团聚或者偏聚。 【EN】The invention belongs to the field of lithium ion battery anode materials, and discloses a preparation method of a lithium phosphate coated high-nickel ternary anode material, which comprises the following steps: (1) preparing a high-nickel ternary cathode material by adopting a high-temperature sintering method; (2) dissolving phosphate in water to obtain a coating solution; (3) mixing the high-nickel ternary positive electrode material with water, adding a lithium source, and stirring to obtain a suspension; (4) dripping the coating liquid into the suspension for reaction, and performing suction filtration to obtain a wet material; (5) drying the wet material, sieving, sintering and keeping the temperature to obtain the material. The invention uses water as solvent to coat, and has operability and reliability in industry; the invention is dissolved in water solution and then reprecipitated, belongs to the process of chemical coating, and has uniform coating and no self-agglomeration or segregation of the coating agent.
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