废催化剂中铂族金属提取的离子交换技术研究

密级：学校代码：10075分类号：学号：20090934理学硕士学位论文废催化剂中铂族金属提取的离子交换技术研究学位申请人：董珊指导教师：李志林副教授学位类别：理学硕士学科专业：无机化学授予单位：河北大学答辩日期：二〇一二年五月ClassifiedIndex:CODE:10075U.D.C.:NO:20090934ADissertationforDegreeofM.ScienceExtractionofPlatinum-groupMetalsInWasteCatalystbyIonExchangeTechnologyCandidate:DongShanSupervisor:ViceProf.LiZhilinAcademicDegreeAppliedfor:MasterofScienceSpecialty:InorganicChemistryUniversity:HebeiUniversityDateofOralExamination:May，2012摘要I摘要铂族金属的性质非常相似，而且往往共同存在于矿体中，对于其中各个金属的分离纯化非常困难。本文在查阅大量国内外文献的基础上，主要采用离子交换技术提取、分离了废催化剂中的铂族金属。本文主要采用焙烧、树脂吸附、解吸、氯化铵沉淀、水合肼还原等一系列操作提取到高纯度的精铂和海绵钯。并采用湿法浸出废催化剂中的铂族金属，考察了铂族金属浸出过程中浸出率的影响因素，确定了昀佳浸出条件：废催化剂的固液比为1:5,HCl的浓度为6mol/L，H2O2为30%，NaF的浓度为0.02g/L，在100℃条件下恒温反应6h，铂族金属的浸出率可以达到：Pt90.5%、Pd96.0%。针对阴离子树脂上金属Fe和贵金属Pd的解吸工艺进行了研究。通过查阅文献确定了树脂的昀佳解吸剂为pH=1.1的盐酸和25%的氨水溶液。运用X射线荧光光谱仪（XRF）探讨了解吸过程的时间、温度、解吸液用量等因素与解吸率之间的关系，确定了昀佳解吸条件为：120min、常温、解吸剂与树脂的体积比为5:1时，铁的解吸率可达88.6%。解吸速率常数k=3.33×10-4s-1，解吸表观活化能为2.91kJ/(mol·K)。25%的氨水溶液对Pd的解吸率可达90.6%。此结果与用国标法测得的结果90.0%基本相吻合，说明XRF在定量分析方面具有一定的可行性以及分析数据的准确性。关键词废催化剂铂族金属提取D201BR树脂XRFAbstractIIAbstractThepropertiesofplatinum-groupmetalsaresimilar.Theyalwaysexistinthedeposittogether.Theseparationandpurificationofthemetalsaredifficult.Onthebasisofconsultingtheinternalandexternalreferences,thetechnologyofionexchangeresinisusedtoextractandseparatetheplatinum-groupmetalsinthespentcatalysts.Mainlyadopttheoperationofroasting,adsorption,elutionofresin,sedimentofammoniumchlorideandreductionofhydratehydrazine.Theplatinumandpalladiuminhighdegreeofpurityarereceived.Recoveryofplatinum-groupmetalsfromwastecatalystsbywetleachingmethodisinspected.Afterinvestigatingvariouseffectsontheleachingofplatinum-groupmetals,theoptimumleachingconditionsaredetermined.Theextractionrateofplatinumcanreach90.5%andpalladium96.0%fromthemixedsolutionof6mol/LHCl-30%H2O2-0.02g/LNaFandstirring6hoursunder100℃.Thevolumeratioofsolid-liquidinthespentcatalystsis1:5.Theelutioncraftoftheironandpalladiumintheanionexchangeresinarestudied.Throughconsultingthereferences,thehydrochloric(pH=1.1)andammonia(25%)areregardedasthebestelutingagent.Studiesontherelationshipoftheelutionratewiththeelutiontime,thetemperatureandtheconsumptionofelutingagentarecarriedoutusingtheX-rayfluorescence.Andtheoptimumelutionconditionsarefixed.Theelutionrateofironcanreach88.6%andpalladium90.6%undertheconditionsoftheelutiontimeof120min,normaltemperature,andvolumetricratioofelutingagenttoresinof5:1.Theelutionrateconstant(k)is3.33×10-4s-1andtheapparentactivationenergyis2.91kJ/(mol·K).TheelutionrateofPdcanreach90.6%.TheresultisinaccordancewiththeresultdeterminedbyGB/T.ThetechnologyofXRFhasagoodfeasibilityforchemicalelementandveracityforquantitativedatainquantitativeanalysis.Keywordswastecatalystsplatinum-groupmetalsextractD201BRresinXRF目录III目录第1章序言........................................................................................................................11.1引言.................................................................................................................................11.2铂族金属概述.................................................................................................................21.2.1铂、钯的性质及用途...............................................................................................21.2.2铂、钯的回收现状...................................................................................................21.2.3铂、钯的回收工艺...................................................................................................31.3离子交换树脂概述.........................................................................................................41.3.1离子交换树脂的发展简史.......................................................................................41.3.2离子交换树脂的结构...............................................................................................51.3.3离子交换树脂的分类...............................................................................................61.3.4离子交换树脂的应用领域.......................................................................................61.4离子交换法概述.............................................................................................................71.4.1离子交换法原理.......................................................................................................71.4.2离子交换技术应用现状...........................................................................................81.5树脂解吸概述.................................................................................................................91.5.1解吸方法介绍...........................................................................................................91.5.2树脂解吸的影响因素...............................................................................................91.6本文的研究目的和意义...............................................................................................101.7创新点...........................................................................................................................10第2章废催化剂中铂族金属的提取..............................................