CN115386722A - A method for separating rare earth and iron from pyrite roasted NdFeB waste - Google Patents
A method for separating rare earth and iron from pyrite roasted NdFeB waste Download PDFInfo
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Abstract
本申请提出了一种黄铁矿焙烧钕铁硼废料分离稀土和铁的方法，涉及稀土资源回收利用技术领域。一种黄铁矿焙烧钕铁硼废料分离稀土和铁的方法，包括以下步骤：将钕铁硼废料与黄铁矿混合，通入氧气，进行选择性硫酸化焙烧；将焙烧后的产物冷却后研磨，然后经过水浸和过滤，得到稀土浸出液和铁精矿。本申请的优点在于选择性硫酸化焙烧工艺流程简单，便于操作，在焙烧过程产生可溶性稀土硫酸盐，不会产生难溶的稀土铁酸盐物相。获得的焙砂利用水浸，稀土和铁的分离效果好。整个过程中不使用酸，极大减少废水处理量，最终不产生含酸废渣，对环境无污染，且铁资源可用作铁精矿，有价资源获得充分利用。
The application proposes a method for separating rare earth and iron from pyrite roasted NdFeB waste, which relates to the technical field of rare earth resource recovery and utilization. A method for separating rare earth and iron from pyrite roasted NdFeB waste, comprising the following steps: mixing NdFeB waste with pyrite, introducing oxygen, and performing selective sulfate roasting; cooling the roasted product Grinding, then soaking in water and filtering to obtain rare earth leachate and iron concentrate. The advantages of the present application are that the selective sulfation roasting process is simple and easy to operate, and soluble rare earth sulfates are produced during the roasting process without producing insoluble rare earth ferrite phases. The obtained calcine is immersed in water, and the separation effect of rare earth and iron is good. No acid is used in the whole process, which greatly reduces the amount of wastewater treatment. In the end, no acid-containing waste residue is produced, which has no pollution to the environment, and iron resources can be used as iron concentrates, making full use of valuable resources.
Description
技术领域technical field
本申请涉及稀土资源回收利用技术领域，具体而言，涉及一种黄铁矿焙烧钕铁硼废料分离稀土和铁的方法。The application relates to the technical field of rare earth resource recovery and utilization, in particular to a method for separating rare earth and iron from pyrite roasted NdFeB waste.
背景技术Background technique
钕铁硼永磁体广泛应用于风力涡轮机、电子设备、混合电动汽车等领域。钕铁硼永磁材料在生产加工过程中会产生约25％的废料，其中稀土含量约占30％(主要是钕、镨、镝)。对钕铁硼废料回收利用生产工艺与原矿开采生产工艺相比，可节约约88％的能源，减少约98％的有害气体排放。NdFeB permanent magnets are widely used in wind turbines, electronic equipment, hybrid electric vehicles and other fields. During the production and processing of NdFeB permanent magnet materials, about 25% of waste materials will be generated, of which the rare earth content accounts for about 30% (mainly neodymium, praseodymium, and dysprosium). Compared with the production process of raw ore mining, the production process of NdFeB waste recycling can save about 88% of energy and reduce about 98% of harmful gas emissions.
对钕铁硼废料回收通常采用盐酸优溶、硫酸全溶等技术工艺，该类工艺操作简单、稀土回收率高、与原矿生产工艺相类似，但该技术工艺消耗大量酸、产生大量废水、产生酸性固废，污染环境。此外在盐酸优溶工艺中首先对钕铁硼废料进行氧化焙烧，在氧化焙烧过程中会产生一部分难溶出的铁酸稀土物相，在后序盐酸优溶工艺中需要高浓度盐酸、高温长时间浸出，增加耗酸量，降低稀土浸出效率。The recovery of NdFeB waste usually adopts technical processes such as excellent dissolution of hydrochloric acid and complete dissolution of sulfuric acid. This type of process is simple to operate and has a high recovery rate of rare earths. Acid solid waste pollutes the environment. In addition, in the hydrochloric acid optimal dissolution process, the NdFeB waste is first oxidized and roasted. During the oxidation roasting process, a part of the ferrite rare earth phase that is difficult to dissolve will be produced. Leaching increases acid consumption and reduces rare earth leaching efficiency.
因此研究出一种高效且环保的钕铁硼废料回收方法具有较大的意义。Therefore, it is of great significance to develop an efficient and environmentally friendly recycling method for NdFeB waste.
发明内容Contents of the invention
本申请的目的在于提供一种黄铁矿焙烧钕铁硼废料分离稀土和铁的方法，此方法可以将钕铁硼废料中的稀土和铁进行分离，且整个过程简单、环保，对环境无污染。The purpose of this application is to provide a method for separating rare earth and iron from pyrite roasted NdFeB waste, which can separate rare earth and iron in NdFeB waste, and the whole process is simple, environmentally friendly, and has no pollution to the environment .
本申请解决其技术问题是采用以下技术方案来实现的。The application solves the technical problem by adopting the following technical solutions.
本申请实施例提供一种黄铁矿焙烧钕铁硼废料分离稀土和铁的方法，包括以下步骤：The embodiment of the present application provides a method for separating rare earth and iron from pyrite roasted NdFeB waste, comprising the following steps:
将钕铁硼废料与黄铁矿混合，通入氧气，进行选择性硫酸化焙烧；Mix NdFeB waste with pyrite, feed oxygen, and carry out selective sulfation roasting;
将焙烧后的产物冷却后研磨，然后经过水浸和过滤，得到稀土浸出液和铁精矿。The roasted product is cooled and then ground, then soaked in water and filtered to obtain rare earth leaching solution and iron concentrate.
相对于现有技术，本申请的实施例至少具有如下优点或有益效果：Compared with the prior art, the embodiments of the present application have at least the following advantages or beneficial effects:
本申请采用黄铁矿对钕铁硼废料进行选择性硫酸化焙烧，首先将钕铁硼废料中的稀土和铁离子氧化成氧化物，将黄铁矿中的硫离子氧化成二氧化硫或三氧化硫；然后稀土氧化物与二氧化硫或三氧化硫硫酸化反应生成可溶性稀土硫酸盐，经过水浸溶于水中，过滤后达到稀土和铁分离的目的。本申请的优点在于选择性硫酸化焙烧工艺流程简单，便于操作，在焙烧过程产生可溶性稀土硫酸盐，不会产生难溶的稀土铁酸盐物相。获得的焙砂利用水浸，稀土和铁的分离效果好。整个过程中不使用酸，极大减少废水处理量，最终不产生含酸废渣，对环境无污染，且铁资源可用作铁精矿，有价资源获得充分利用。This application uses pyrite to carry out selective sulfate roasting on NdFeB waste, firstly oxidizes the rare earth and iron ions in the NdFeB waste to oxides, and oxidizes the sulfur ions in the pyrite to sulfur dioxide or sulfur trioxide ; Then rare earth oxides react with sulfur dioxide or sulfur trioxide to generate soluble rare earth sulfates, which are dissolved in water by water immersion and filtered to achieve the purpose of separating rare earths and iron. The advantages of the present application are that the selective sulfation roasting process is simple and easy to operate, and soluble rare earth sulfates are produced during the roasting process without producing insoluble rare earth ferrite phases. The obtained calcine is immersed in water, and the separation effect of rare earth and iron is good. No acid is used in the whole process, which greatly reduces the amount of wastewater treatment. In the end, no acid-containing waste residue is produced, which has no pollution to the environment, and iron resources can be used as iron concentrates, making full use of valuable resources.
附图说明Description of drawings
为了更清楚地说明本申请实施例的技术方案，下面将对实施例中所需要使用的附图作简单地介绍，应当理解，以下附图仅示出了本申请的某些实施例，因此不应被看作是对范围的限定，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他相关的附图。In order to more clearly illustrate the technical solutions of the embodiments of the present application, the following will briefly introduce the accompanying drawings used in the embodiments. It should be understood that the following drawings only show some embodiments of the present application, so It should be regarded as a limitation on the scope, and those skilled in the art can also obtain other related drawings based on these drawings without creative work.
图1为本申请稀土氧化物与二氧化硫或三氧化硫反应的吉布斯自由能图；Fig. 1 is the Gibbs free energy diagram of the reaction of the rare earth oxide of the present application with sulfur dioxide or sulfur trioxide;
图2为本申请的工艺流程图。Fig. 2 is the process flow chart of the present application.
具体实施方式Detailed ways
为使本申请实施例的目的、技术方案和优点更加清楚，下面将对本申请实施例中的技术方案进行清楚、完整地描述。实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。In order to make the purpose, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below. Those who do not indicate the specific conditions in the examples are carried out according to the conventional conditions or the conditions suggested by the manufacturer. The reagents or instruments used were not indicated by the manufacturer, and they were all conventional products that could be purchased from the market.
需要说明的是，在不冲突的情况下，本申请中的实施例及实施例中的特征可以相互组合。下面将参考具体实施例来详细说明本申请。It should be noted that, in the case of no conflict, the embodiments in the present application and the features in the embodiments can be combined with each other. The present application will be described in detail below with reference to specific examples.
一种黄铁矿焙烧钕铁硼废料分离稀土和铁的方法，包括以下步骤：A method for separating rare earth and iron from pyrite roasted NdFeB waste, comprising the following steps:
将钕铁硼废料与黄铁矿混合，通入氧气，进行选择性硫酸化焙烧；Mix NdFeB waste with pyrite, feed oxygen, and carry out selective sulfation roasting;
将焙烧后的产物冷却后研磨，然后经过水浸和过滤，得到稀土浸出液和铁精矿。The roasted product is cooled and then ground, then soaked in water and filtered to obtain rare earth leaching solution and iron concentrate.
本发明的原理：钕铁硼废料与黄铁矿在氧气气氛中反应，钕铁硼废料中的稀土成分发生硫酸化焙烧生成稀土硫酸盐，钕铁硼废料中的铁转化为铁的氧化物，硫酸化焙烧过程可能发生的反应如下方程式(1)～(10)所示：The principle of the present invention: NdFeB waste reacts with pyrite in an oxygen atmosphere, the rare earth components in the NdFeB waste are sulfated and roasted to generate rare earth sulfate, and the iron in the NdFeB waste is converted into iron oxides. The reactions that may occur in the sulfation roasting process are shown in the following equations (1) to (10):
Nd+O2(g)＝Nd2O3 (1)Nd+O 2 (g)=Nd 2 O 3 (1)
Fe+O2(g)＝Fe2O3 (2)Fe+O 2 (g)=Fe 2 O 3 (2)
4FeS2+11O2(g)＝2Fe2O3+6SO2(g) (3)4FeS 2 +11O 2 (g)＝2Fe 2 O 3 +6SO 2 (g) (3)
2FeS2+7O2(g)＝Fe2(SO4)3+SO2(g) (4)2FeS 2 +7O 2 (g)＝Fe 2 (SO 4 ) 3 +SO 2 (g) (4)
FeS2+3O2(g)＝FeSO4+SO2(g) (5)FeS 2 +3O 2 (g) = FeSO 4 +SO 2 (g) (5)
Fe2(SO4)3＝Fe2O3+3SO3(g) (6)Fe 2 (SO 4 ) 3 ＝Fe 2 O 3 +3SO 3 (g) (6)
2FeSO4＝Fe2O3+SO3(g)+SO2(g) (7)2FeSO 4 ＝Fe 2 O 3 +SO 3 (g)+SO 2 (g) (7)
4FeSO4+O2(g)＝2Fe2O3+4SO3(g) (8)4FeSO 4 +O 2 (g)＝2Fe 2 O 3 +4SO 3 (g) (8)
Nd2O3+3SO2(g)+1.5O2(g)＝Nd2(SO4)3 (9)Nd 2 O 3 +3SO 2 (g)+1.5O 2 (g)＝Nd 2 (SO 4 ) 3 (9)
Nd2O3+3SO3(g)＝Nd2(SO4)3 (10)Nd 2 O 3 +3SO 3 (g)＝Nd 2 (SO 4 ) 3 (10)
在焙烧过程中，钕铁硼废料中的稀土和铁按反应(1)和(2)进行氧化焙烧，黄铁矿按反应(3)～(5)进行氧化燃烧反应，释放二氧化硫，同时生成的硫酸铁和硫酸亚铁按反应(6)～(8)释放二氧化硫或三氧化硫，生成的二氧化硫或三氧化硫按反应(9)和(10)将钕铁硼废料中的稀土相硫酸化为可溶性稀土硫酸盐。During the roasting process, the rare earth and iron in the NdFeB waste are oxidized and roasted according to the reactions (1) and (2), and the pyrite is oxidized and burned according to the reactions (3) to (5), releasing sulfur dioxide and producing Ferric sulfate and ferrous sulfate release sulfur dioxide or sulfur trioxide according to reactions (6)～(8), and the sulfur dioxide or sulfur trioxide generated will sulfate the rare earth phase in NdFeB waste materials according to reactions (9) and (10). Soluble Rare Earth Sulfates.
本申请反应(9)和(10)在常压、不同温度下的标准吉布斯自由能如图1所示，从图1中可以看出，在温度273～1273K范围内，其反应标准吉布斯自由能均小于零，因此理论上上述反应是可行的。The standard Gibbs free energies of the application's reactions (9) and (10) at normal pressure and different temperatures are shown in Figure 1. As can be seen from Figure 1, within the scope of temperature 273～1273K, the reaction standard Gibbs free energy Booth free energy is less than zero, so the above reaction is theoretically feasible.
经焙烧后生成可溶性稀土硫酸盐和铁氧化物，将焙烧后的产物冷却后进行水浸，此时稀土硫酸盐溶于水中，成为硫酸稀土溶液，过滤后得到硫酸稀土溶液和铁精矿，实现钕铁硼废料中稀土和铁的分离。After roasting, soluble rare earth sulfates and iron oxides are generated, and the roasted products are cooled and then soaked in water. At this time, the rare earth sulfates are dissolved in water and become a rare earth sulfate solution. After filtration, rare earth sulfate solutions and iron concentrates are obtained. Separation of rare earths and iron from NdFeB scrap.
综上，本申请采用黄铁矿对钕铁硼废料进行选择性硫酸化焙烧，首先将钕铁硼废料中的稀土和铁离子氧化成氧化物，将黄铁矿中的硫离子氧化成二氧化硫或三氧化硫；然后稀土氧化物与二氧化硫或三氧化硫硫酸化反应生成可溶性稀土硫酸盐，经过水浸溶于水中，过滤后达到稀土和铁分离的目的。本申请的优点在于选择性硫酸化焙烧工艺流程简单，便于操作，在焙烧过程产生可溶性稀土硫酸盐，不会产生难溶的稀土铁酸盐物相。获得的焙砂利用水浸，稀土和铁的分离效果好。整个过程中不使用酸，极大减少废水处理量，最终不产生含酸废渣，对环境无污染，且铁资源可用作铁精矿，有价资源获得充分利用。In summary, this application uses pyrite to carry out selective sulfate roasting of NdFeB waste, firstly oxidizes the rare earth and iron ions in the NdFeB waste to oxides, and oxidizes the sulfur ions in the pyrite to sulfur dioxide or Sulfur trioxide; then the sulfation reaction of rare earth oxides with sulfur dioxide or sulfur trioxide to generate soluble rare earth sulfates, which are dissolved in water by water immersion and filtered to achieve the purpose of separating rare earths and iron. The advantages of the present application are that the selective sulfation roasting process is simple and easy to operate, and soluble rare earth sulfates are produced during the roasting process without producing insoluble rare earth ferrite phases. The obtained calcine is immersed in water, and the separation effect of rare earth and iron is good. No acid is used in the whole process, which greatly reduces the amount of wastewater treatment. In the end, no acid-containing waste residue is produced, which has no pollution to the environment, and iron resources can be used as iron concentrates, making full use of valuable resources.
在本申请的一些实施例中，上述钕铁硼废料包括油泥废料、废旧钕铁硼磁体、钕铁硼氧化物中的一种或多种的混合物。通过本申请的分离方法可以将油泥废料、废旧钕铁硼磁体或钕铁硼氧化物中的稀土与铁进行分离。In some embodiments of the present application, the aforementioned NdFeB waste materials include oil sludge waste, waste NdFeB magnets, and a mixture of one or more of NdFeB oxides. The rare earth and iron in sludge waste, waste NdFeB magnets or NdFeB oxides can be separated by the separation method of the present application.
在本申请的一些实施例中，上述黄铁矿中的硫含量＞52％。采用高硫含量的黄铁矿可以保证在焙烧反应过程中对钕铁硼废料中的稀土相进行充分的硫酸化，从而提高稀土和铁的分离效果。In some embodiments of the present application, the sulfur content in the aforementioned pyrite is >52%. The use of pyrite with high sulfur content can ensure sufficient sulfation of the rare earth phase in the NdFeB waste during the roasting reaction, thereby improving the separation effect of rare earth and iron.
在本申请的一些实施例中，上述钕铁硼废料与上述黄铁矿的质量比为1：(0.5～2)。可根据本黄铁矿中的硫含量调整黄铁矿的加入比例。In some embodiments of the present application, the mass ratio of the aforementioned NdFeB waste to the aforementioned pyrite is 1: (0.5-2). The addition ratio of pyrite can be adjusted according to the sulfur content in the pyrite.
在本申请的一些实施例中，上述通入氧气的流量为1～3L/min。通入合适流量的氧气，既可以对黄铁矿和钕铁硼废料进行充分的氧化，又不至于浪费。In some embodiments of the present application, the above-mentioned flow rate of introducing oxygen is 1-3 L/min. Introducing an appropriate flow of oxygen can fully oxidize the pyrite and NdFeB waste without wasting it.
在本申请的一些实施例中，上述焙烧的温度为500～800℃，所述焙烧时间为1～3h。在上述焙烧温度和时间下，可以充分对黄铁矿和钕铁硼废料进行氧化和硫酸化反应。In some embodiments of the present application, the above-mentioned calcination temperature is 500-800° C., and the calcination time is 1-3 hours. Under the above roasting temperature and time, the pyrite and NdFeB waste can be fully oxidized and sulfated.
在焙烧过程中，过量的黄铁矿会分解生成过量的二氧化硫或三氧化硫，还需要对尾气吸收处理用于制备硫酸，以防止三氧化硫气体逸散在空气中造成环境污染。During the roasting process, excess pyrite will be decomposed to generate excess sulfur dioxide or sulfur trioxide, and tail gas absorption treatment is required to prepare sulfuric acid to prevent sulfur trioxide gas from escaping into the air and causing environmental pollution.
在本申请的一些实施例中，上述焙烧后的产物冷却至28～35℃。将焙烧后的产物冷却至室温后进行水浸。In some embodiments of the present application, the calcined product is cooled to 28-35°C. After the calcined product is cooled to room temperature, it is soaked in water.
在本申请的一些实施例中，上述焙烧后的产物研磨后过200～400目筛。在进行氧化前还可以对黄铁矿和钕铁硼废料进行研磨，将黄铁矿和钕铁硼废料研磨成细粉后进行高温焙烧，可以增大黄铁矿和钕铁硼废料的比表面积，从而增加其与氧气的反应速率，更有利于钕铁硼废料中稀土相与二氧化硫或三氧化硫生成可溶性稀土硫酸盐，进而加快焙烧过程中各个反应速率，节约反应时间和反应成本。对焙烧后产物进行研磨，增加其与水的接触面积，促进可溶性稀土硫酸盐在水中的溶解速率。In some embodiments of the present application, the roasted product is ground and passed through a 200-400 mesh sieve. Before oxidation, pyrite and NdFeB waste can also be ground. Grinding pyrite and NdFeB waste into fine powder and roasting at high temperature can increase the specific surface area of pyrite and NdFeB waste. Thereby increasing its reaction rate with oxygen is more conducive to the rare earth phase in NdFeB waste to form soluble rare earth sulfate with sulfur dioxide or sulfur trioxide, thereby speeding up each reaction rate in the roasting process and saving reaction time and reaction cost. The calcined product is ground to increase its contact area with water and accelerate the dissolution rate of soluble rare earth sulfate in water.
在本申请的一些实施例中，上述水浸步骤中的液固比为(3～10)：1，上述水浸时间为0.5～3h。在水浸的过程中还可对焙烧产物进行搅拌，同时还可以采用超声波进行振荡，这样可以加快可溶性稀土硫酸盐在水中的溶解效率，以提高稀土与铁的分离效果。In some embodiments of the present application, the liquid-solid ratio in the water immersion step is (3-10):1, and the water immersion time is 0.5-3 hours. In the process of water immersion, the roasted product can also be stirred, and at the same time, it can be oscillated by ultrasonic waves, which can speed up the dissolution efficiency of soluble rare earth sulfate in water, so as to improve the separation effect of rare earth and iron.
以下结合实施例对本申请的特征和性能作进一步的详细描述。The characteristics and performance of the present application will be described in further detail below in conjunction with the examples.
实施例1Example 1
一种黄铁矿焙烧钕铁硼废料分离稀土和铁的方法，其工艺流程如图2所示，包括以下步骤：A method for separating rare earth and iron from pyrite roasted NdFeB waste, its technological process as shown in Figure 2, comprises the following steps:
将钕铁硼废料和黄铁矿混合均匀研磨至-200目(74μm)占90％以上，钕铁硼废料中稀土含量为25％、铁含量为69％，黄铁矿中硫含量为55.6％、铁含量为43.0％。按照钕铁硼废料与黄铁矿的质量比为1：1.3将钕铁硼和黄铁矿混合均匀并送入管式炉中，通入氧气，氧气浓度为100％，氧气流量为2L/min，加热至600℃，在此温度下焙烧120min，焙烧完成后冷却研磨成细粉，过300目筛。焙烧过程中的反应为：Mix and grind the NdFeB waste and pyrite evenly until -200 mesh (74μm) accounts for more than 90%. The rare earth content in the NdFeB waste is 25%, the iron content is 69%, and the sulfur content in the pyrite is 55.6%. , Iron content is 43.0%. According to the mass ratio of NdFeB waste to pyrite is 1:1.3, mix NdFeB and pyrite evenly and send them into the tube furnace, and feed oxygen with the oxygen concentration of 100% and the oxygen flow rate of 2L/min , heated to 600°C, and roasted at this temperature for 120 minutes, cooled and ground into fine powder after roasting, and passed through a 300-mesh sieve. The reaction during the roasting process is:
Nd+O2(g)＝Nd2O3 (1)Nd+O 2 (g)=Nd 2 O 3 (1)
Fe+O2(g)＝Fe2O3 (2)Fe+O 2 (g)=Fe 2 O 3 (2)
4FeS2+11O2(g)＝2Fe2O3+6SO2(g) (3)4FeS 2 +11O 2 (g)＝2Fe 2 O 3 +6SO 2 (g) (3)
2FeS2+7O2(g)＝Fe2(SO4)3+SO2(g) (4)2FeS 2 +7O 2 (g)＝Fe 2 (SO 4 ) 3 +SO 2 (g) (4)
FeS2+3O2(g)＝FeSO4+SO2(g) (5)FeS 2 +3O 2 (g) = FeSO 4 +SO 2 (g) (5)
Fe2(SO4)3＝Fe2O3+3SO3(g) (6)Fe 2 (SO 4 ) 3 ＝Fe 2 O 3 +3SO 3 (g) (6)
2FeSO4＝Fe2O3+SO3(g)+SO2(g) (7)2FeSO 4 ＝Fe 2 O 3 +SO 3 (g)+SO 2 (g) (7)
4FeSO4+O2(g)＝2Fe2O3+4SO3(g) (8)4FeSO 4 +O 2 (g)＝2Fe 2 O 3 +4SO 3 (g) (8)
Nd2O3+3SO2(g)+1.5O2(g)＝Nd2(SO4)3 (9)Nd 2 O 3 +3SO 2 (g)+1.5O 2 (g)＝Nd 2 (SO 4 ) 3 (9)
Nd2O3+3SO3(g)＝Nd2(SO4)3 (10)Nd 2 O 3 +3SO 3 (g)＝Nd 2 (SO 4 ) 3 (10)
将研磨后的焙烧产物用去离子水浸出，室温(30℃)，液固比为10：1，浸出时间60min，浸出完成后过滤分离，其中液体为硫酸稀土溶液，固体为铁精矿。焙烧产物稀土浸出率为94.5％，铁浸出率为0.5％，铁精矿中铁品位为66.6％。The ground roasted product was leached with deionized water at room temperature (30°C), the liquid-solid ratio was 10:1, and the leaching time was 60 minutes. After the leaching was completed, it was filtered and separated. The liquid was rare earth sulfate solution, and the solid was iron concentrate. The rare earth leaching rate of the roasted product is 94.5%, the iron leaching rate is 0.5%, and the iron grade in the iron concentrate is 66.6%.
实施例2Example 2
一种黄铁矿焙烧钕铁硼废料分离稀土和铁的方法，包括以下步骤：A method for separating rare earth and iron from pyrite roasted NdFeB waste, comprising the following steps:
将钕铁硼废料和黄铁矿混合均匀研磨至-200目(74μm)占90％以上，钕铁硼废料中稀土含量为20％、铁含量为50％，黄铁矿中硫含量为55.6％、铁含量为43.0％。按照钕铁硼废料与黄铁矿的质量比为1：1.1将钕铁硼和黄铁矿混合均匀并送入管式炉中，通入氧气，氧气浓度为100％，氧气流量为3L/min，加热至600℃，在此温度下焙烧120min，焙烧完成后冷却研磨成细粉，过400目筛。焙烧过程中的反应为：Mix and grind the NdFeB waste and pyrite evenly until -200 mesh (74μm) accounts for more than 90%, the rare earth content in the NdFeB waste is 20%, the iron content is 50%, and the sulfur content in the pyrite is 55.6% , Iron content is 43.0%. According to the mass ratio of NdFeB waste to pyrite as 1:1.1, mix NdFeB and pyrite evenly and send them into the tube furnace, and feed oxygen, the oxygen concentration is 100%, and the oxygen flow rate is 3L/min , heated to 600°C, and roasted at this temperature for 120 minutes, cooled and ground into fine powder after roasting, and passed through a 400-mesh sieve. The reaction during the roasting process is:
Nd+O2(g)＝Nd2O3 (1)Nd+O 2 (g)=Nd 2 O 3 (1)
Fe+O2(g)＝Fe2O3 (2)Fe+O 2 (g)=Fe 2 O 3 (2)
4FeS2+11O2(g)＝2Fe2O3+6SO2(g) (3)4FeS 2 +11O 2 (g)＝2Fe 2 O 3 +6SO 2 (g) (3)
2FeS2+7O2(g)＝Fe2(SO4)3+SO2(g) (4)2FeS 2 +7O 2 (g)＝Fe 2 (SO 4 ) 3 +SO 2 (g) (4)
FeS2+3O2(g)＝FeSO4+SO2(g) (5)FeS 2 +3O 2 (g) = FeSO 4 +SO 2 (g) (5)
Fe2(SO4)3＝Fe2O3+3SO3(g) (6)Fe 2 (SO 4 ) 3 ＝Fe 2 O 3 +3SO 3 (g) (6)
2FeSO4＝Fe2O3+SO3(g)+SO2(g) (7)2FeSO 4 ＝Fe 2 O 3 +SO 3 (g)+SO 2 (g) (7)
4FeSO4+O2(g)＝2Fe2O3+4SO3(g) (8)4FeSO 4 +O 2 (g)＝2Fe 2 O 3 +4SO 3 (g) (8)
Nd2O3+3SO2(g)+1.5O2(g)＝Nd2(SO4)3 (9)Nd 2 O 3 +3SO 2 (g)+1.5O 2 (g)＝Nd 2 (SO 4 ) 3 (9)
Nd2O3+3SO3(g)＝Nd2(SO4)3 (10)Nd 2 O 3 +3SO 3 (g)＝Nd 2 (SO 4 ) 3 (10)
将研磨后的焙烧产物用去离子水浸出，室温(30℃)，液固比为10：1，浸出时间60min，浸出完成后过滤分离，其中液体为硫酸稀土溶液，固体为铁精矿。焙烧产物稀土浸出率为93.6％，铁浸出率为0.3％，铁精矿中铁品位为67.1％。The ground roasted product was leached with deionized water at room temperature (30°C), the liquid-solid ratio was 10:1, and the leaching time was 60 minutes. After the leaching was completed, it was filtered and separated. The liquid was rare earth sulfate solution, and the solid was iron concentrate. The rare earth leaching rate of the roasted product is 93.6%, the iron leaching rate is 0.3%, and the iron grade in the iron concentrate is 67.1%.
实施例3Example 3
一种黄铁矿焙烧钕铁硼废料分离稀土和铁的方法，包括以下步骤：A method for separating rare earth and iron from pyrite roasted NdFeB waste, comprising the following steps:
将钕铁硼废料和黄铁矿混合均匀研磨至-200目(74μm)占90％以上，钕铁硼废料中稀土含量为24％、铁含量为66％，黄铁矿中硫含量为55.6％、铁含量为43.0％。按照钕铁硼废料与黄铁矿的质量比为1：1将钕铁硼和黄铁矿混合均匀并送入管式炉中，通入氧气，氧气浓度为100％，氧气流量为3L/min，加热至650℃，在此温度下焙烧150min，焙烧完成后冷却研磨成细粉，过400目筛。焙烧过程中的反应为：Mix and grind the NdFeB waste and pyrite evenly until -200 mesh (74μm) accounts for more than 90%. The rare earth content in the NdFeB waste is 24%, the iron content is 66%, and the sulfur content in the pyrite is 55.6%. , Iron content is 43.0%. According to the mass ratio of NdFeB waste to pyrite is 1:1, mix NdFeB and pyrite evenly and send them into the tube furnace, and feed oxygen, the oxygen concentration is 100%, and the oxygen flow rate is 3L/min , heated to 650°C, roasted at this temperature for 150 minutes, cooled and ground into fine powder after roasting, and passed through a 400-mesh sieve. The reaction during the roasting process is:
Nd+O2(g)＝Nd2O3 (1)Nd+O 2 (g)=Nd 2 O 3 (1)
Fe+O2(g)＝Fe2O3 (2)Fe+O 2 (g)=Fe 2 O 3 (2)
4FeS2+11O2(g)＝2Fe2O3+6SO2(g) (3)4FeS 2 +11O 2 (g)＝2Fe 2 O 3 +6SO 2 (g) (3)
2FeS2+7O2(g)＝Fe2(SO4)3+SO2(g) (4)2FeS 2 +7O 2 (g)＝Fe 2 (SO 4 ) 3 +SO 2 (g) (4)
FeS2+3O2(g)＝FeSO4+SO2(g) (5)FeS 2 +3O 2 (g) = FeSO 4 +SO 2 (g) (5)
Fe2(SO4)3＝Fe2O3+3SO3(g) (6)Fe 2 (SO 4 ) 3 ＝Fe 2 O 3 +3SO 3 (g) (6)
2FeSO4＝Fe2O3+SO3(g)+SO2(g) (7)2FeSO 4 ＝Fe 2 O 3 +SO 3 (g)+SO 2 (g) (7)
4FeSO4+O2(g)＝2Fe2O3+4SO3(g) (8)4FeSO 4 +O 2 (g)＝2Fe 2 O 3 +4SO 3 (g) (8)
Nd2O3+3SO2(g)+1.5O2(g)＝Nd2(SO4)3 (9)Nd 2 O 3 +3SO 2 (g)+1.5O 2 (g)＝Nd 2 (SO 4 ) 3 (9)
Nd2O3+3SO3(g)＝Nd2(SO4)3 (10)Nd 2 O 3 +3SO 3 (g)＝Nd 2 (SO 4 ) 3 (10)
将研磨后的焙烧产物用去离子水浸出，室温(30℃)，液固比为5：1，浸出时间30min，浸出完成后过滤分离，其中液体为硫酸稀土溶液，固体为铁精矿。焙烧产物稀土浸出率为94.7％，铁浸出率为0.2％，铁精矿中铁品位为67.2％。The ground roasted product is leached with deionized water at room temperature (30°C), the liquid-solid ratio is 5:1, and the leaching time is 30 minutes. After the leaching is completed, it is filtered and separated. The liquid is rare earth sulfate solution, and the solid is iron concentrate. The rare earth leaching rate of the roasted product was 94.7%, the iron leaching rate was 0.2%, and the iron grade in the iron concentrate was 67.2%.
实施例4Example 4
一种黄铁矿焙烧钕铁硼废料分离稀土和铁的方法，包括以下步骤：A method for separating rare earth and iron from pyrite roasted NdFeB waste, comprising the following steps:
将钕铁硼废料和黄铁矿混合均匀研磨至-200目(74μm)占90％以上，钕铁硼废料中稀土含量为24％、铁含量为66％，黄铁矿中硫含量为55.6％、铁含量为43.0％。按照钕铁硼废料与黄铁矿的质量比为1：0.5将钕铁硼和黄铁矿混合均匀并送入管式炉中，通入氧气，氧气浓度为100％，氧气流量为3L/min，加热至500℃，在此温度下焙烧180min，焙烧完成后冷却研磨成细粉，过400目筛。焙烧过程中的反应为：Mix and grind the NdFeB waste and pyrite evenly until -200 mesh (74μm) accounts for more than 90%. The rare earth content in the NdFeB waste is 24%, the iron content is 66%, and the sulfur content in the pyrite is 55.6%. , Iron content is 43.0%. According to the mass ratio of NdFeB waste to pyrite is 1:0.5, mix NdFeB and pyrite evenly and send them into the tube furnace, and feed oxygen with the oxygen concentration of 100% and the oxygen flow rate of 3L/min , heated to 500°C, and roasted at this temperature for 180 minutes, cooled and ground into fine powder after roasting, and passed through a 400-mesh sieve. The reaction during the roasting process is:
Nd+O2(g)＝Nd2O3 (1)Nd+O 2 (g)=Nd 2 O 3 (1)
Fe+O2(g)＝Fe2O3 (2)Fe+O 2 (g)=Fe 2 O 3 (2)
4FeS2+11O2(g)＝2Fe2O3+6SO2(g) (3)4FeS 2 +11O 2 (g)＝2Fe 2 O 3 +6SO 2 (g) (3)
2FeS2+7O2(g)＝Fe2(SO4)3+SO2(g) (4)2FeS 2 +7O 2 (g)＝Fe 2 (SO 4 ) 3 +SO 2 (g) (4)
FeS2+3O2(g)＝FeSO4+SO2(g) (5)FeS 2 +3O 2 (g) = FeSO 4 +SO 2 (g) (5)
Fe2(SO4)3＝Fe2O3+3SO3(g) (6)Fe 2 (SO 4 ) 3 ＝Fe 2 O 3 +3SO 3 (g) (6)
2FeSO4＝Fe2O3+SO3(g)+SO2(g) (7)2FeSO 4 ＝Fe 2 O 3 +SO 3 (g)+SO 2 (g) (7)
4FeSO4+O2(g)＝2Fe2O3+4SO3(g) (8)4FeSO 4 +O 2 (g)＝2Fe 2 O 3 +4SO 3 (g) (8)
Nd2O3+3SO2(g)+1.5O2(g)＝Nd2(SO4)3 (9)Nd 2 O 3 +3SO 2 (g)+1.5O 2 (g)＝Nd 2 (SO 4 ) 3 (9)
Nd2O3+3SO3(g)＝Nd2(SO4)3 (10)Nd 2 O 3 +3SO 3 (g)＝Nd 2 (SO 4 ) 3 (10)
将研磨后的焙烧产物用去离子水浸出，室温(30℃)，液固比为3：1，浸出时间120min，浸出完成后过滤分离，其中液体为硫酸稀土溶液，固体为铁精矿。焙烧产物稀土浸出率为94.6％，铁浸出率为0.2％，铁精矿中铁品位为66.8％。The ground roasted product is leached with deionized water at room temperature (30°C), the liquid-solid ratio is 3:1, and the leaching time is 120 minutes. After the leaching is completed, it is filtered and separated. The liquid is rare earth sulfate solution, and the solid is iron concentrate. The rare earth leaching rate of the roasted product is 94.6%, the iron leaching rate is 0.2%, and the iron grade in the iron concentrate is 66.8%.
实施例5Example 5
一种黄铁矿焙烧钕铁硼废料分离稀土和铁的方法，包括以下步骤：A method for separating rare earth and iron from pyrite roasted NdFeB waste, comprising the following steps:
将钕铁硼废料和黄铁矿混合均匀研磨至-200目(74μm)占90％以上，钕铁硼废料中稀土含量为24％、铁含量为66％，黄铁矿中硫含量为55.6％、铁含量为43.0％。按照钕铁硼废料与黄铁矿的质量比为1：0.9将钕铁硼和黄铁矿混合均匀并送入管式炉中，通入氧气，氧气浓度为100％，氧气流量为3L/min，加热至800℃，在此温度下焙烧80min，焙烧完成后冷却研磨成细粉，过400目筛。焙烧过程中的反应为：Mix and grind the NdFeB waste and pyrite evenly until -200 mesh (74μm) accounts for more than 90%. The rare earth content in the NdFeB waste is 24%, the iron content is 66%, and the sulfur content in the pyrite is 55.6%. , Iron content is 43.0%. According to the mass ratio of NdFeB waste to pyrite is 1:0.9, mix NdFeB and pyrite evenly and send them into the tube furnace, and feed oxygen with the oxygen concentration of 100% and the oxygen flow rate of 3L/min , heated to 800 ° C, roasted at this temperature for 80 minutes, cooled and ground into fine powder after roasting, and passed through a 400-mesh sieve. The reaction during the roasting process is:
Nd+O2(g)＝Nd2O3 (1)Nd+O 2 (g)=Nd 2 O 3 (1)
Fe+O2(g)＝Fe2O3 (2)Fe+O 2 (g)=Fe 2 O 3 (2)
4FeS2+11O2(g)＝2Fe2O3+6SO2(g) (3)4FeS 2 +11O 2 (g)＝2Fe 2 O 3 +6SO 2 (g) (3)
2FeS2+7O2(g)＝Fe2(SO4)3+SO2(g) (4)2FeS 2 +7O 2 (g)＝Fe 2 (SO 4 ) 3 +SO 2 (g) (4)
FeS2+3O2(g)＝FeSO4+SO2(g) (5)FeS 2 +3O 2 (g) = FeSO 4 +SO 2 (g) (5)
Fe2(SO4)3＝Fe2O3+3SO3(g) (6)Fe 2 (SO 4 ) 3 ＝Fe 2 O 3 +3SO 3 (g) (6)
2FeSO4＝Fe2O3+SO3(g)+SO2(g) (7)2FeSO 4 ＝Fe 2 O 3 +SO 3 (g)+SO 2 (g) (7)
4FeSO4+O2(g)＝2Fe2O3+4SO3(g) (8)4FeSO 4 +O 2 (g)＝2Fe 2 O 3 +4SO 3 (g) (8)
Nd2O3+3SO2(g)+1.5O2(g)＝Nd2(SO4)3 (9)Nd 2 O 3 +3SO 2 (g)+1.5O 2 (g)＝Nd 2 (SO 4 ) 3 (9)
Nd2O3+3SO3(g)＝Nd2(SO4)3 (10)Nd 2 O 3 +3SO 3 (g)＝Nd 2 (SO 4 ) 3 (10)
将研磨后的焙烧产物用去离子水浸出，室温(32℃)，液固比为10：1，浸出时间180min，浸出完成后过滤分离，其中液体为硫酸稀土溶液，固体为铁精矿。焙烧产物稀土浸出率为94.8％，铁浸出率为0.2％，铁精矿中铁品位为67.4％。The ground roasted product was leached with deionized water at room temperature (32°C), the liquid-solid ratio was 10:1, and the leaching time was 180 minutes. After the leaching was completed, it was filtered and separated. The liquid was rare earth sulfate solution, and the solid was iron concentrate. The rare earth leaching rate of the roasted product is 94.8%, the iron leaching rate is 0.2%, and the iron grade in the iron concentrate is 67.4%.
实施例6Example 6
一种黄铁矿焙烧钕铁硼废料分离稀土和铁的方法，包括以下步骤：A method for separating rare earth and iron from pyrite roasted NdFeB waste, comprising the following steps:
将钕铁硼废料和黄铁矿混合均匀研磨至-200目(74μm)占90％以上，钕铁硼废料中稀土含量为24％、铁含量为66％，黄铁矿中硫含量为55.6％、铁含量为43.0％。按照钕铁硼废料与黄铁矿的质量比为1：2将钕铁硼和黄铁矿混合均匀并送入管式炉中，通入氧气，氧气浓度为100％，氧气流量为3L/min，加热至750℃，在此温度下焙烧120min，焙烧完成后冷却研磨成细粉，过400目筛。焙烧过程中的反应为：Mix and grind the NdFeB waste and pyrite evenly until -200 mesh (74μm) accounts for more than 90%. The rare earth content in the NdFeB waste is 24%, the iron content is 66%, and the sulfur content in the pyrite is 55.6%. , Iron content is 43.0%. According to the mass ratio of NdFeB waste to pyrite is 1:2, mix NdFeB and pyrite evenly and send them into the tube furnace, and feed oxygen with the oxygen concentration of 100% and the oxygen flow rate of 3L/min , heated to 750°C, and roasted at this temperature for 120 minutes, cooled and ground into fine powder after roasting, and passed through a 400-mesh sieve. The reaction during the roasting process is:
Nd+O2(g)＝Nd2O3 (1)Nd+O 2 (g)=Nd 2 O 3 (1)
Fe+O2(g)＝Fe2O3 (2)Fe+O 2 (g)=Fe 2 O 3 (2)
4FeS2+11O2(g)＝2Fe2O3+6SO2(g) (3)4FeS 2 +11O 2 (g)＝2Fe 2 O 3 +6SO 2 (g) (3)
2FeS2+7O2(g)＝Fe2(SO4)3+SO2(g) (4)2FeS 2 +7O 2 (g)＝Fe 2 (SO 4 ) 3 +SO 2 (g) (4)
FeS2+3O2(g)＝FeSO4+SO2(g) (5)FeS 2 +3O 2 (g) = FeSO 4 +SO 2 (g) (5)
Fe2(SO4)3＝Fe2O3+3SO3(g) (6)Fe 2 (SO 4 ) 3 ＝Fe 2 O 3 +3SO 3 (g) (6)
2FeSO4＝Fe2O3+SO3(g)+SO2(g) (7)2FeSO 4 ＝Fe 2 O 3 +SO 3 (g)+SO 2 (g) (7)
4FeSO4+O2(g)＝2Fe2O3+4SO3(g) (8)4FeSO 4 +O 2 (g)＝2Fe 2 O 3 +4SO 3 (g) (8)
Nd2O3+3SO2(g)+1.5O2(g)＝Nd2(SO4)3 (9)Nd 2 O 3 +3SO 2 (g)+1.5O 2 (g)＝Nd 2 (SO 4 ) 3 (9)
Nd2O3+3SO3(g)＝Nd2(SO4)3 (10)Nd 2 O 3 +3SO 3 (g)＝Nd 2 (SO 4 ) 3 (10)
将研磨后的焙烧产物用去离子水浸出，室温(32℃)，液固比为10：1，浸出时间180min，浸出完成后过滤分离，其中液体为硫酸稀土溶液，固体为铁精矿。焙烧产物稀土浸出率为94.5％，铁浸出率为0.3％，铁精矿中铁品位为67.2％。The ground roasted product was leached with deionized water at room temperature (32°C), the liquid-solid ratio was 10:1, and the leaching time was 180 minutes. After the leaching was completed, it was filtered and separated. The liquid was rare earth sulfate solution, and the solid was iron concentrate. The rare earth leaching rate of the roasted product is 94.5%, the iron leaching rate is 0.3%, and the iron grade in the iron concentrate is 67.2%.
综上所述，本申请实施例的一种黄铁矿焙烧钕铁硼废料分离稀土和铁的方法，具有以下优点：In summary, a method for separating rare earth and iron from pyrite roasted NdFeB waste according to the embodiment of the present application has the following advantages:
本申请采用黄铁矿对钕铁硼废料进行选择性硫酸化焙烧，首先将钕铁硼废料中的稀土和铁离子氧化成氧化物，将黄铁矿中的硫离子氧化成二氧化硫或三氧化硫；然后稀土氧化物与二氧化硫或三氧化硫硫酸化反应生成可溶性稀土硫酸盐，经过水浸溶于水中，过滤后达到稀土和铁分离的目的。本申请的优点在于选择性硫酸化焙烧工艺流程简单，便于操作，在焙烧过程产生可溶性稀土硫酸盐，不会产生难溶的稀土铁酸盐物相。获得的焙砂利用水浸，稀土和铁的分离效果好。整个过程中不使用酸，极大减少废水处理量，最终不产生含酸废渣，对环境无污染，且铁资源可用作铁精矿，有价资源获得充分利用。This application uses pyrite to carry out selective sulfate roasting on NdFeB waste, firstly oxidizes the rare earth and iron ions in the NdFeB waste to oxides, and oxidizes the sulfur ions in the pyrite to sulfur dioxide or sulfur trioxide ; Then rare earth oxides react with sulfur dioxide or sulfur trioxide to generate soluble rare earth sulfates, which are dissolved in water by water immersion and filtered to achieve the purpose of separating rare earths and iron. The advantages of the present application are that the selective sulfation roasting process is simple and easy to operate, and soluble rare earth sulfates are produced during the roasting process without producing insoluble rare earth ferrite phases. The obtained calcine is immersed in water, and the separation effect of rare earth and iron is good. No acid is used in the whole process, which greatly reduces the amount of wastewater treatment. In the end, no acid-containing waste residue is produced, which has no pollution to the environment, and iron resources can be used as iron concentrates, making full use of valuable resources.
以上所描述的实施例是本申请一部分实施例，而不是全部的实施例。本申请的实施例的详细描述并非旨在限制要求保护的本申请的范围，而是仅仅表示本申请的选定实施例。基于本申请中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本申请保护的范围。The embodiments described above are some of the embodiments of the present application, but not all of them. The detailed description of the embodiments of the application is not intended to limit the scope of the claimed application, but merely represents selected embodiments of the application. Based on the embodiments in this application, all other embodiments obtained by persons of ordinary skill in the art without creative efforts fall within the protection scope of this application.
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