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酚醛树脂基球形活性炭的制备
分类号:
TQ424.1密级:
硕士学位论文
鞍山科技大学论文题目:
酚醛树脂基球形活性炭的制备及对苯酚吸附性能的初步研究
二○○六年一月五日
论文题目:
酚醛树脂基球形活性炭的制备及对
苯酚吸附性能的初步研究
Studyonthepreparationofphenolicresin-basedspherical
activatedcarbonandadsorptionofphenol
研究生姓名:
谢飞
指导教师姓名:
白金锋教授单位:
鞍山科技大学化工学院论文提交日期:
答辩日期:
学位授予日期:
授予单位:
论文评阅人:
单位:
单位:
鞍山科技大学硕士论文摘要
摘要
活性炭是一种优良的吸附剂,在工业、农业、医疗、卫生及军事等领域有广泛的应用。
酚醛树脂基球形活性炭具有机械强度高、炭化收率高、吸附能力强等优点,目前受到很多研究者的关注。
本文以苯酚和甲醛为原料合成酚醛树脂(PF)并以此为制备活性炭的前驱体,实验采用悬浮法制备酚醛树脂球,然后对其预氧化、炭化、活化处理,制得具有一定吸附能力的球形活性炭。
实验考察了原料配比和成球条件对酚醛树脂成球性能的影响,探讨了树脂球的预氧化、炭化、活化条件对活性炭碘值和苯值的影响规律;同时,采用比表面积测定仪和扫描电镜对所制备的酚醛树脂基球形活性炭进行了表征。
结果表明,当甲醛与苯酚的摩尔比为0.85、成球温度95℃、搅拌速度2000rpm、搅拌时间10min,以及成球液各组分的质量比为水:
固化剂S:
氟化钙:
氯化钾:
十二烷基硫酸钠:
十八烷基三甲基溴化铵=92.70:
3.07:
1.45:
2.76:
9.52×10-3:
1.52×10-2时,树脂加入量6wt%的条件下,可得到球形度为0.960,粒径分布450~900µm的百分含量达到95%以上且球间不发生粘连的酚醛树脂球。
在预氧化升温速率1℃.min-1、预氧化温度180℃、预氧化时间120min和炭化升温速率2℃.min-1、炭化温度800℃、炭化恒温时间80min以及活化温度800℃、活化时间1h、水蒸汽流量为0.4ml.min-1的条件下,可制得比表面积为726m2.g-1,活性炭收率、碘值、苯值及强度分别为47.51%、907mg.g-1、273mg.g-1、9.85N/粒的酚醛树脂基球形活性炭。
为了进一步提高球形活性炭的吸附性能,实验研究了在合成过程中添加乙二醇(EG)及聚乙二醇(PEG)和金属盐磷酸二氢钾、三氯化铁并采用水蒸汽活化处理来提高其吸附性能。
在上述适宜的炭化和活化条件下,在乙二醇添加量为36wt%时,活性炭可得到最大碘值为1837mg.g-1、比表面积为1682m2.g-1的球形活性炭;在PEG20K添加量为36wt%时,可得到最大苯值为442mg.g-1、比表面积为1092m2.g-1的球形活性炭。
当添加的KH2PO4与苯酚摩尔比为0.0055时,可得到碘值为1201m2.g-1、比表面积为1109m2.g-1的球形活性炭;当二者的摩尔比为0.011时,所制备的球形活性炭苯值为409mg.g-1、比表面积为979m2.g-1。
当添加的FeCl3与苯酚摩尔比为0.00825时,活性炭比表面积为993m2.g-1,碘值和苯值均达最大,分别为942mg.g-1、485mg.g-1。
III
鞍山科技大学硕士论文摘要
为了能够进一步了解酚醛树脂基球形活性炭对有机物的吸附性能,本文以苯酚为吸附物,考察了未加造孔剂的酚醛树脂基球形活性炭对水中苯酚的静态及动态吸附性能,并采用NaOH超声波再生法对饱和活性炭进行再生实验。
结果表明,本实验所制备的球形活性炭对水中的苯酚有良好的吸附性能。
关键词:
酚醛树脂,球形活性炭,炭化,活化,吸附性能
IV
鞍山科技大学硕士论文ABSTRACT
ABSTRACT
Anexcellentadsorbentmaterials,activatedcarbonhasextensiveapplicationinthefieldsofindustry,agriculture,medicineandmilitary.Phenolicresin-basedsphericalactivatedcarbonhasmanyadvantages,suchashighmechanicalintensity,highcarbonizationyield,betteradsorptionproperties,soithasbeenreceivedmoreattentionbymanyresearchersintheworld.
First,phenolicresinspheresismadefromthephenolicresin(PF)precursorwhichissynthesizedwithphenolandformaldehydebysuspensionmethod.Second,thesphericalactivatedcarbonispreparedbytheprocessesofcarbonizationandactivationwithstabilizationphenolicresinspheres.Theeffectsofincludingthemoleratioofmaterialcomponents,sphericizingconditions,stabilization,carbonizationandactivationontheiodinevalueandbenzenevalue,arediscussedinthethesis.Theresultsshowthatsphericityisover0.960andtheamountofspheresizefrom20to40meshisover95%;andthesuitablesphericizingconditionsarethesphericizingtemperature95℃,theweightpercentageofspheresizefrom450~900µmisover45wt%;andthesuitablesphericizingconditionsarethesphericizingtemperature95℃,stirringrate2000rpm,stirringtime10min,phenolicresin6wt%,theweightconstitutionofsolution,water:
curingagentcontent:
CaF2:
KCl:
sodiumdodecylsulphate:
octadecyletrimethylammoniumbromide=92.70:
3.07:
1.45:
2.76:
9.52×10-3:
1.52×10-2.Thesphericalactivatedcarbonismadeatthestabilizationheatingrate1℃.min-1,stabilizationtemperature180℃,stabilizationtime120minandcarbonizationheatingrate2℃.min-1,carbonizationtemperature800℃,carbonizationtime80minandactivationtemperature800℃,activationtime1h,watervaporflux0.4ml.min-1.Underoptimumconditions,thespecificsurfacearea,iodinevalueandbenzenevalue,yieldandintensityofthesphericalactivatedcarbonare726m2.g-1,907mg.g-1,273mg.g-1,47.51%,9.85N/granule,respectively.Toimproveadsorptionproperties,ethyleneglycol(EG),polyethyleneglycol(PEG),KH2PO4,andFeCl3areaddedduringthesynthesizingphenolicresinasadditivesintheV
鞍山科技大学硕士论文ABSTRACTexperiment.Underaboveconditions,theiodinevalueis1837mg.g-1,uptothegreatest,andspecificsurfaceareaofactivatedcarbonis1682m2.g-1;whentheweightpercentageofadditiveEGreducesto36wt%,whileitsgreatestvaluesforbenzeneandthespecificsurfaceareaare442mg.g-1and1092m2.g-1,respectively;whenthepercentageofadditivePEG20Kis36wt%.Theiodinevalueandspecificsurfaceareaoftheactivatedcarbonare1201mg.g-1and1109m2.g-1,respectively;whenthemoleratioofKH2PO4tophenolis0.0055,whileitsbenzenevalueandspecificsurfaceareaare409mg.g-1and979m2.g-1respectivelywhenthemoleratioofthemis0.011.WhenthemoleratioofFeCl3tophenolis0.00825,itsspecificsurfaceareais993m2.g-1,andiodinevalueandbenzenevalueare942mg.g-1and485mg.g-1,respectively.
Theadsorptionofphenolisstudiedinordertoinvesttheadsorptionoforganicsonphenolicresin-basedsphericalactivatedcarbon.Furthermore,themethodofNaOHandultrasonicwaveisusedtoregenerateactivatedcarbon.Theresultsshowthatphenolhasgoodadsorptiononactivatedcarbon.
Keywords:
phenolicresin,sphericalactivatedcarbon,
carbonization,activation,adsorptionproperties
VI
鞍山科技大学硕士论文目录
目录
摘要........................................................................................................................III
ABSTRACT.....................................................................................................................V
引言...................................................................................................................1
1文献综述......................................................................................................................2
1.1活性炭的发展概述............................................................................................2
1.1.1活性炭的发展历史..................................................................................2
1.1.2国内外活性炭研究概况..........................................................................2
1.2活性炭的性质及结构........................................................................................3
1.2.1活性炭的微晶结构..................................................................................3
1.2.2活性炭的孔隙结构..................................................................................3
1.2.3孔隙的作用..............................................................................................4
1.3活性炭的制备....................................................................................................4
1.3.1制备活性炭的原料..................................................................................4
1.3.2活性炭的制备方法..................................................................................7
1.4球形活性炭及其应用........................................................................................9
1.4.1沥青基球形活性炭..................................................................................9
1.4.2树脂基球形活性炭................................................................................10
1.4.3煤基球形活性炭.....................................................................................11
1.4.4球形活性炭的应用.................................................................................11
1.5开展本课题的研究思路..................................................................................13
2实验部分....................................................................................................................14
2.1实验药品及设备..............................................................................................14
2.2酚醛树脂球的制备工艺过程..........................................................................14
2.3酚醛树脂球的预氧化处理..............................................................................15
2.4酚醛树脂基球形活性炭的炭化和活化工艺过程..........................................15
2.5酚醛树脂基球形活性炭性能的表征..............................................................15
2.5.1平均球形度的测定................................................................................15
2.5.2成球液表面张力的测定........................................................................16
2.5.3粒径分布的测定....................................................................................16
2.5.4颗粒压碎强度的测定............................................................................16
2.5.5活性炭碘吸附值测定............................................................................16
2.5.6活性炭苯吸附值测定............................................................................16
V
鞍山科技大学硕士论文目录
2.5.7酚醛树脂球和球形活性炭的形态结构................................................16
2.5.8比表面积测定及孔结构表征................................................................16
2.5.9红外谱图分析........................................................................................17
2.5.10热重分析..............................................................................................17
2.6水中苯酚吸附性能检测..................................................................................17
2.6.1静态吸附性能检测................................................................................17
2.6.2动态吸附性能检测................................................................................17
3结果与讨论................................................................................................................18
3.1酚醛树脂的合成条件......................................................................................18
3.1.1原料配比对酚醛树脂微球球形度的影响............................................18
3.2悬浮法制备酚醛树脂球..................................................................................20
3.2.1成球温度................................................................................................20
3.2.2搅拌速度................................................................................................21
3.2.3搅拌时间................................................................................................22
3.2.3固化剂S的添加量................................................................................23
3.2.4表面活性剂....................................................................................