利用晋城煤矸石制备聚合氯化铝铁及其性能评价

论文题目：利用晋城煤矸石制备聚合氯化铝铁及其性能评价专业：应用化学姓名：杨正虎（签名）指导导师：蔡会武（签名）摘要聚合氯化铝铁(PAFC)作为一种无机高分子絮凝剂已广泛应用于水质净化和污水处理。我国煤矸石资源非常丰富，煤矸石中含有一定量的Al、Fe元素，可以作为制备聚合氯化铝铁的廉价原料。本文以煤矸石和硫酸废渣为原料，采用两步法制备聚合氯化铝铁。通过正交实验及单因素实验研究了焙烧温度、焙烧时间、酸浸温度、酸浸时间和液固比等因素对煤矸石中氧化铝溶出率的影响；研究了聚合反应中铝酸钙粉加入量、反应温度、反应时间等对聚合氯化铝铁盐基度的影响；对产品的理化性能进行了分析与测试，并对产品进行了净化生活废水和印染废水的实验研究，得到如下结论：用煤矸石和硫酸废渣制备聚合氯化铝铁的工艺流程为：首先将一定粒度的煤矸石焙烧，焙烧后加入一定量的硫酸废渣（调节Fe含量），然后与适量的盐酸混合进行酸浸反应。将酸浸液过滤，滤液加热搅拌进行聚合反应，并加入适量的铝酸钙粉增加产品的氧化铝含量，同时调节产品盐基度。反应一定时间后，冷却熟化即为液体聚合氯化铝铁，继续蒸发干燥可得固体聚合氯化铝铁。正交实验及单因素实验优化的煤矸石焙烧最佳工艺参数为：焙烧温度800℃、焙烧时间2.5h；优化的酸浸反应最佳工艺参数为：酸浸温度105℃、酸浸时间3.5h、液固比为3.0mL/g。对氧化铝浸出率的影响程度由大到小依次为：焙烧温度酸浸温度酸浸时间液固比焙烧时间。在最优条件下煤矸石中氧化铝的溶出率为79.5%。优化的聚合反应最佳工艺参数为：加入铝酸钙粉的百分比为25%（以10g煤矸石为基准）、反应温度98℃、反应时间4h。制得固体产品中Al2O3含量28.47%，铁含量2.51%，盐基度80.16%。通过红外光谱分析表明，PAFC当中既有以羟基架桥联结的铝聚合物，又有以羟基架桥联结的铁聚合物，与文献报道的PAC结构稍有不同；由PAFC的凝胶色谱可知，采用两步法制备聚合氯化铝铁，合理的控制条件，可以获得分子量较大，聚合度较高的产品；通过热重分析可知，产品失重主要在40~150℃和150~600℃两个阶段，在600℃之后样品的质量基本不再变化。将产品用于生活废水处理，当水样的pH在7.0~9.0时，浊度、COD、色度去除率可分别达到83.4%、79.8%、86%；用于印染废水处理，其絮凝沉降速度快，形成的矾花大而密实，产品的加入量为300mg/L时，印染废水的色度、浊度、COD的去除率分别可以达到83.3%、80.6%、81.7%，去除效果均优于市售产品。关键词：聚合氯化铝铁；煤矸石；硫酸废渣；焙烧；酸浸；聚合；絮凝研究类型：应用研究SubiectSubiectSubiectSubiect:Preparation:Preparation:Preparation:PreparationofofofofPolymericPolymericPolymericPolymericaluminumaluminumaluminumaluminumferricferricferricferricchloridechloridechloridechloride（PAFCPAFCPAFCPAFC）fromfromfromfromJinJinJinJinchengchengchengchengcoalcoalcoalcoalganguegangueganguegangueandandandandpppperformanceerformanceerformanceerformanceevaluationevaluationevaluationevaluationSpecialtySpecialtySpecialtySpecialty:Applied:Applied:Applied:AppliedChemistryChemistryChemistryChemistryNameNameNameName:Yang:Yang:Yang:YangZhenghuZhenghuZhenghuZhenghu(Signature)(Signature)(Signature)(Signature)InstructorInstructorInstructorInstructor:Cai:Cai:Cai:CaiHuiwuHuiwuHuiwuHuiwu(Signature)(Signature)(Signature)(Signature)ABSTRACTABSTRACTABSTRACTABSTRACTPolymericaluminumferricchloride（PAFC）asinorganicpolymerflocculantwhichiswidelyusedforwaterpurificationandwastewatertreatment.CoalgangueresourcesisveryrichinChina.CoalganguecontainsacertainamountofAlandFeelements,andcouldbeusedascheaprawmaterialsforPAFCpreparation.Thispapertakingtwo-stepmethodforpreparingPAFC,withcoalgangueandwasteresidueofsulfateasthematerial.Studiedtheeffectsofparticlesize,calcinationtemperature,acidleachingtemperature,acidleachingtimeandliquid-solidratiotothealuminaleachingrateofcoalganguebyorthogonalexperimentandsingleexperiment.Thentheeffectsofadditionamountofcalciumaluminateinpolymerizationreaction,reactiontemperatureandreactiontimetothePAFCbasicitywasstudied.Theanalysisandtestofphysicalandchemicalpropertiesoftheproductwasstudied,andtheproducthadbeentakenforpurificationexperimentsofdomesticwastewateranddyeingwastewater.Theresultswasasfollowing:TheprocesschartofPAFCpreparedbycoalgangueandwasteresidueofsulfateisasfollows,first,roastthecertaincoalgangue,thenaddamountofwasteresidueofsulfate(whichisusedtoadjustthecontentofFe),andmixedwithhydrochloricacidforleachingreaction.Afterfilter,thefiltrateisheatedstirringforthepolymerization,thenputamountofcalciumaluminatetoincreasethealuminacontentoftheproduct,whileadjustingthebasicity.Afteracertainreactiontime,theliquidPAFCisobtainedaftercooldownandmaturation,thendrytoderivedthesolidproduct.Theoptimumprocessparametersofcoalgangueroastaredeterminedbyorthogonalexperimentandsingleexperiment:theroasttemperatureis800℃andtheroasttimeis2.5h.Theoptimumprocessparametersofacidleachingreactionareasfollow,acidleachingtemperatureis105℃,acidleachingtimeis3.5handtheratioofliquid-to-solidis3.0mL/g.Theprimarysequenceaffectingtheleachingrateofthealuminaoxideis:calciningtemperatureacidleachingtemperatureacidleachingtimetheratioofliquid-to-solidcalciningtime.Und-ertheoptimalcondition,theleachingrateofthealuminaoxideis79.5%.Theoptimumproce-ssparametersofpolymerizationareasfollowing,theadditionofthecalciumaluminateis25%(basedon10gcoalgangue),thereactiontemperatureis98℃andthereactiontimeis4h.Thesolidproduct,theAl2O3contentis28.47%,ironcontentis2.51%andthebasicityis80.16%.TheinfraredspectrumindicatedthatthestructureofPAFChadbothaluminumpolymerandferricpolymerwithhydroxylbridgingconnection,whichwasslightlydifferentfromPACreportedinthepaper;ThegelchromatographyofPAFCindicatesthat,thepolymericaluminumferricchloridewithhighpolymerizationdegreeandlargemolecularweightsynthesizedbytakingtwostepsmethod.Thethermogravimetricanalysis(TGA)showsthat,weightlossofproductmainlyinthestagesof40~150℃and150~600℃,thequalityofsamplebasicallyhasnochangeafter600℃.Theproductisusedforlifewastewatertreatment,whenthepHisin7.0~9.0,turbidityremovalrateisupto83.4%,CODremovalrateis79.8%,chromaremovalrateis86%;Theproductisusedforprintinganddyeingwastewatertreatment,theresultshowsthattheflocculationsettlementvelocityishigh,largeandcompactflocsformed,whenflocculationagentfor300mg/L,chromaremovalrateisupto83.3%,turbidityremovalrateis80.6%,CODremovalrateis81.7%,Theflocculationeffectthansimilarproductssaledinthemarket.KeyKeyKeyKeywords:words:words:words:Po