發(fā)布時間：2018-05-17 13:31

  本文選題：碳酸稀土 + 萃取分離　； 參考：《內(nèi)蒙古大學(xué)》2017年碩士論文

【摘要】：本文針對內(nèi)蒙古航天金峽化工有限責(zé)任公司年產(chǎn)5000噸混合碳酸稀土萃取分離生產(chǎn)線工藝現(xiàn)狀及存在的主要問題,提出了對混合碳酸稀土萃取分離工藝技術(shù)中鑭鈰分組出口級數(shù)、鈰鐠分組出口設(shè)置等進(jìn)行了工藝路線改進(jìn),優(yōu)化了混合碳酸稀土萃取分離的工藝路線,提高了稀土分離產(chǎn)品的質(zhì)量。同時,針對稀土分離后成品和半成品質(zhì)量控制要求,改進(jìn)了釤銪釓料液濃度的分析方法,開發(fā)了混合稀土料液中硫酸根的重量分析法,改進(jìn)了鐠釹氧化物中鋁離子的ICP-AES檢測方法,建立完善了稀土分離成品和半成品的分析方法。論文主要研究內(nèi)容如下:1.內(nèi)蒙古航天金峽化工有限責(zé)任公司(金峽化工)年產(chǎn)5000噸混合碳酸稀土萃取分離生產(chǎn)線鑭鈰分組現(xiàn)采用88級串級萃取分離工藝,該流程通常在第8級出口產(chǎn)生氯化鑭料液,但是由于Na+、Ca2+、Mg2+等非稀土雜質(zhì)含量高,導(dǎo)致氯化鑭料液質(zhì)量超標(biāo),不符合要求,導(dǎo)致濃縮工序料液結(jié)塊,放料困難。基于此問題,通過實驗測定每一級數(shù)稀土料液中稀土雜質(zhì)和非稀土雜質(zhì)的含量,提出將氯化鑭料液在生產(chǎn)工藝流程中的停留時間延長,將氯化鑭料液的出口級數(shù)由8級升為12級。通過該工藝流程的改進(jìn),使得氯化鑭料液中非稀土雜質(zhì)Na+的含量由0.37%降為0.23%,Ca2+由2%降為1.0%。同時,實現(xiàn)了濃縮過程中釜內(nèi)物料高濃度下順利放料,無堵塞現(xiàn)象,保證了 24小時濃縮一釜的生產(chǎn)進(jìn)度,氯化鑭濃縮產(chǎn)品的品位可達(dá)45%以上,較之前提高了 1-2%。2.金峽化工年產(chǎn)5000噸混合碳酸稀土萃取分離生產(chǎn)線110級串級萃取分離工藝流程中,由于萃取槽出口設(shè)置不合理,導(dǎo)致鈰鐠分離線出口產(chǎn)生的鑭鈰料液中Na+、Ca2+、Mg2+等非稀土雜質(zhì)含量高,且以南方稀土礦為原料時鑭鈰配分達(dá)不到要求(鑭占35%和鈰占65%)。同時,還造成后續(xù)濃縮工序料液容易結(jié)塊,放料困難。基于此問題,通過實驗測定鈰鐠分離線各級數(shù)稀土料液中稀土雜質(zhì)和非稀土雜質(zhì)的含量,提出增加鈰鐠分離線料液出口,由原8和100料液兩個出口改為8、22、100三個料液出口。通過該工藝改進(jìn)和優(yōu)化,使第22級料液出口產(chǎn)出的鑭鈰純度得到很大提高,Na+、Ca2+、Mg2+等非稀土雜質(zhì)含量大大降低,Na+由0.31%降為0.1%,Ca2+由1.8%降為0.8%。3.金峽化工年產(chǎn)5000噸混合碳酸稀土萃取分離生產(chǎn)線需要對釹釤分組第40級出口產(chǎn)生的釤銪釓料液濃度進(jìn)行分析,通常直接采用國標(biāo)容量法或重量法進(jìn)行測定,但容量法在料液中鐵含量高時誤差大,超出允許范圍;而重量法耗時長,影響生產(chǎn)效率�；诖藛栴},提出在釤銪釓料液濃度測定前增加前處理工序,通過添加草酸將釤銪釓沉淀,經(jīng)充分洗滌除去鐵雜質(zhì),利用硝酸和高氯酸將稀土沉淀轉(zhuǎn)為釤銪釓料液,然后再采用容量法對其濃度進(jìn)行測定。該分析方法縮短了料液分析時間,提高料液濃度測定的準(zhǔn)確性,保證了生產(chǎn)效率。4.金峽化工年產(chǎn)5000噸混合碳酸稀土萃取分離生產(chǎn)線需要對生產(chǎn)過程中的鐠釹料液、碳酸鐠釹、鐠釹氧化物中的Al3+進(jìn)行測定,采用電感耦合等離子體原子發(fā)射光譜(ICP-AES)方法進(jìn)行測定時,為了消除基體對鋁的影響,配置標(biāo)準(zhǔn)溶液時需加入鐠釹作為基體進(jìn)行在峰校準(zhǔn),這種方法配置標(biāo)液耗時長且消耗大量氧化鐠和氧化釹基準(zhǔn)試劑,因此急需優(yōu)化分析測定方法,降低成本。為此我們對氧化鐠釹中鋁含量的測定方法進(jìn)行了改進(jìn),主要將原來的在峰校正方法改成離峰校正,操作過程體現(xiàn)在鋁測定的標(biāo)準(zhǔn)溶液的配置方法上。由此,改進(jìn)了配置標(biāo)準(zhǔn)溶液的方法,省略烘干氧化鐠和氧化釹步驟,通過儀器自動扣除鐠釹背底峰值,簡化了鋁離子的檢測步驟,為配置標(biāo)準(zhǔn)溶液節(jié)省了成本和時間。5.金峽化工年產(chǎn)5000噸混合碳酸稀土萃取分離生產(chǎn)線生產(chǎn)過程中需要對溶料過程產(chǎn)生的混合稀土料液中的硫酸根離子進(jìn)行測定。通常采用分光光度法進(jìn)行測定,該法需使用穩(wěn)定劑穩(wěn)定沉淀的硫酸根離子,由于穩(wěn)定劑的變化導(dǎo)致測定結(jié)果不穩(wěn)定,有時誤差會較大。為解決這個問題,建立了利用重量法測定混合稀土料液中的硫酸根離子的方法,通過將稀土料液調(diào)至弱酸性,加入過量氯化鋇溶液將稀土料液中的硫酸根離子生成硫酸鋇沉淀,再經(jīng)過濾、洗滌、烘干、稱重后計算硫酸根離子的含量,達(dá)到準(zhǔn)確測定混合稀土料液中硫酸根離子的目的。該法測定硫酸根離子的準(zhǔn)確度和穩(wěn)定性較分光光度法得到較大提高。
[Abstract]:In this paper, the present situation and main problems of the 5000 ton mixed rare earth extraction and separation production line in Inner Mongolia spaceflight golden gorge Chemical Co., Ltd. are presented, and the process route is improved and the mixing process is improved. The process route of extraction and separation of rare earth carbonate improves the quality of rare earth separation products. At the same time, in view of the quality control requirements of the finished product and the semi-finished product after the separation of rare earth, the analytical method of the concentration of samarium europium gadolinium solution is improved, the weight analysis method of sulphuric acid in the mixed rare earth solution is developed, and the ICP-AES detection of aluminum ions in the praseodymium and neodymium oxide is improved. The main research contents of the paper are as follows: 1. the lanthanum cerium group in the 5000 ton mixed rare earth extraction and separation production line of Inner Mongolia spaceflight golden gorge Chemical Co., Ltd. (Jin Xia chemical) is now used in class 88 cascade extraction and separation process, which is usually produced at the level of eighth level. Lanthanum chloride solution is produced, but the high content of non rare earth impurities, such as Na+, Ca2+ and Mg2+, leads to the high quality of lanthanum chloride solution, which does not meet the requirements, which leads to the agglomeration of the material liquid in the concentrating process, which is difficult. Based on this problem, the content of rare earth and non rare earth impurities in the rare earth solution of each series is determined by experiment. When the residence time in the production process is prolonged, the outlet series of lanthanum chloride liquid is raised from 8 to 12. Through the improvement of the process, the content of non rare earth impurity Na+ in lanthanum chloride is reduced from 0.37% to 0.23%, and Ca2+ is reduced from 2% to 1.0%.. The production schedule of concentrating one kettle for 24 hours is guaranteed, and the grade of lanthanum chloride concentrating products can be up to 45%. In the process of separating the 110 grade cascade extraction separation process of 1-2%.2. golden gorge with 5000 tons of mixed rare earth extraction and separation production line, the output of lanthanum produced by the export of cerium praseodymium separation line is caused by the unreasonable exportation of the extraction trough. The content of non rare earth impurities such as Na+, Ca2+ and Mg2+ in the cerium solution is high, and the coordination separation of lanthanum and cerium can not be reached when the south rare earth ore is used as raw material (lanthanum is 35% and cerium is 65%). At the same time, the material liquid in the subsequent concentration process is easy to caking and the discharge is difficult. Based on this problem, the rare earth impurities and the non dilute materials in the rare earth solution at all levels of the cerium praseodymium separation line are determined by experiments. The content of soil impurities is proposed to increase the export of cerium praseodymium separation line liquid, from the two exits of the original 8 and 100 materials to the 8,22100 three outlet. Through the improvement and optimization of the process, the purity of lanthanum and cerium produced in the export of twenty-second grade liquid is greatly improved, the content of non rare earth impurities such as Na+, Ca2+, Mg2+ and other non rare earth impurities are greatly reduced, Na+ from 0.31% to 0.1%, Ca2+ by 1.8 It is necessary to analyze the concentration of samarium and europium gadolinium solution produced in the fortieth stage of the neodymium samarium group by 5000 tons of 0.8%.3., which is usually directly adopted by the national standard volume method or gravimetric method, but the volumetric method has a high error and exceed the allowable range when the content of iron is high in the liquid, and the weight method is consumed. On the basis of this problem, it is proposed to increase the pretreatment process before the determination of the concentration of SM EU gadolinium solution. By adding oxalic acid to precipitate samarium europium gadolinium, the iron impurity is removed by full washing, and the rare earth precipitation is converted to samarium europium gadolinium solution by nitric acid and perchloric acid, and then the concentration is measured by capacity method. The accuracy of the determination of the concentration of the liquid is shortened, and the production efficiency of the 5000 ton mixed rare earth extraction and separation line of the annual production efficiency of.4. Jin Xia is guaranteed. The Al3+ of praseodymium and neodymium carbonate in the production process, the praseodymium neodymium carbonate and the praseodymium neodymium oxide are measured, and the inductively coupled plasma atomic emission spectrometry (ICP-AES) is used. In order to eliminate the influence of the matrix on the aluminum, the praseodymium and neodymium should be added as the matrix to calibrate the standard solution. This method configuring the standard solution is long and consumes a large amount of praseodymium oxide and neodymium oxide reference reagent. Therefore, it is urgent to optimize the analytical method and reduce the cost. Therefore, we have the aluminum content in the praseodymium oxide neodymium oxide. The method is improved, the original method of peak correction is changed to peak correction. The operation process is embodied in the method of allocation of standard solution for aluminium determination. Thus, the method of configuring the standard solution is improved, the steps of praseodymium oxide and neodymium oxide are omitted, the peak of the back bottom of the praseodymium and neodymium is automatically deducted by the instrument, and the detection of the aluminum ion is simplified. In the process of measuring the standard solution, the cost and time are saved, the 5000 tons of mixed rare earth extraction and separation production line of.5. Jin Xia chemical industry production process needs to be measured in the mixed rare-earth solution produced by the solution process. In order to solve this problem, a method for the determination of sulfate ion in mixed rare-earth solution is established by using the gravimetric method to determine the sulphuric acid root ion in the mixture of rare earth mixture. Barium sulfate is precipitated and then filtered, washed, dried and weighed, the content of the sulfate ion is calculated to achieve the purpose of accurate determination of the sulfate ion in the mixed rare-earth solution. The accuracy and stability of the determination of sulfate radical ions are greatly improved by this method.
【學(xué)位授予單位】：內(nèi)蒙古大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：TQ028.32;TQ133.3

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