ADEKA反应型乳化剂SR ER系列在乳液聚合中的应用PPT格式课件下载.pptx
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ADEKA反应型乳化剂SR ER系列在乳液聚合中的应用PPT格式课件下载.pptx
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EA=1:
1mmol;
Initiator0.1mmol;
Solvent5ml;
60,OCX24hr,在水性体系(胶束体系)中,使用水溶性聚合引发剂,会加快共聚速度。
SR-10和各种单体的共聚性,ADEKACORPORATION,8,ReactivityofSR-10withvariousmonomer,St,2EHAMMAEA,BA,AN,AAc,40,50,VAc80,6070ConvertionofSR-10(%),StAAcANBA2EHAMMAEAVAc,SR-10/monomer=1/1mol25%aq,24hr60oCInitiator:
V-50(Azotype)3wt%*NoagitationConversionat5hrLowAA,High,EA,VAc,30,50,70,90,0,10,20,Time(hr),C,no,ev,itr,Sfono,R,1-,(0,)%,VAcEA2EHAMMABAANAAcSt30,(5hr),单体的水溶解度,ADEKACORPORATION,9,Monomersolubilityinwater(25),Property,Hydrophilic,Hydrophobic,MonomerAcrylicacid(AAc)Acrylonitrile(AN)VinylAcetate(VAc)Methylmethacrylate(MMA)Ethylacrylate(EA)Butylacrylate(BA)Styrene(St)2-Ethylhexylacrylate(2-EHA),(g/100ml)*7.32.5*1.61.50.14*0.030.01,*20,反应性乳化剂聚合基的位置Classificationofreactivesurfactants,ADEKACORPORATION,10,Reactive,Hydrophilic,Hydrophobic,1.HeadBIMAX,DOW,R&
H,2.TailClariant,PPG,3.MiddleADEKA(SE,SR),胶束和单体可溶解位置Micelleandpositioningofmonomer,ADEKACORPORATION,11,Micelleoutside,Palisadelayer,BA,2-EHA,EA,MMA,AAc,Reactivesurfactantcopolymerization:
Tohaverelationbetweenmicelleandpositioningofmonomer,Micellcore,Hydrophilic,Hydrophobic,Q,e值,ADEKACORPORATION,12,共轭类Conjugative,非共轭类Nonconjugative烯丙基的共聚性,Q0.2:
e0:
非共轭类单体电子供给性,反应性低很容易链转移(退化的链转移),1)共鸣稳定效果、2)极性效果、3)单体水溶解度,决定单体和SR的共聚性变化,单体和SR-10的反应率比较(SR-10=2.5%onmonomer),ADEKACORPORATION,13,InitialMonomer/SAA=10/10%InitialMonomer/SAA=5/3%,B,/A,M,M,A,/,A,A,B,/A,tS,/,A,A,0,25,50,75,100,0,1,2,3,4,5,Time(hr),C,o,vn,re,is,o,(n,)%,SR-10Monomer,SR-10,SR-10,Monomer,0,25,50,75,100,0,2,4,6,Time(hr),C,o,vn,re,is,o,(n,)%,SR-10Monomer,0,25,50,75,100,0,2,4,6,Time(hr),C,o,vn,re,is,o,(n,)%,SR-10Monomer,0,25,50,75,100,0,2,4,6,Time(hr),C,o,vn,re,is,o,(n,)%,SR-10Monomer,通过优化配方,即使是St体系,也可提高SR的共聚率,HPLC图,ADEKACORPORATION,14,1)初期聚合结束之后,2)滴加1hr,3)滴加2hr,4)滴加3hr,5)成熟1hr,6)成熟2hr,SR-10polymer,总结,ADEKACORPORATION,15,烯丙基的均聚性很低,但是,当达到cmc以上的浓度时,聚合速度就会加快,当与丙烯酸单体共存的情况下,聚合速度就会更快。
一般情况下,和共轭类、电子接受性丙烯酸单体有着良好的共聚性,但是由于单体水溶解度的关系,和非共轭类的Vac也有着良好的共聚性。
与电子供给性的St的共聚率也可以达到70%。
SR-10的共聚速度在BA/St/AA体系中要比BA/MMA/AA体系中要慢。
初期单体/乳化剂比率影响SR-10的共聚率。
REASOAP的共聚性,ADEKACORPORATION,16,使用REASOA进行乳液聚合的配方,聚合过程及评价方法丙烯酸体系乳液聚合配方的探讨苯乙烯体系乳液聚合配方的探讨,聚合过程及评价方法丙烯酸体系乳液聚合配方的探讨苯乙烯体系乳液聚合配方的探讨,ADEKACORPORATION,17,聚合过程,ADEKACORPORATION,18,Initiator(APS、50%),Monomer(5-10%)Water(52%)Surfactant(1-20%),Monomer(90-95%)Water(48%)Surfactant(80-99%)Initiator(APS、50%),滴加乳液3hr(75oC),成熟2hr(75oC),1,2,3,4,Flask,Drop(feed),初期聚合15分钟(75oC),配方(Solid46%),引发剂,水:
根据固体分而定单体:
90g乳化剂:
0.675-2.25g:
0.2g,Flask,Drop(feed),乳化剂=对单体0.75-2.5wt%引发剂=对单体0.2wt%,项目固体分()单体转化率,ADEKACORPORATION,19,测定方法1052小时,干燥样品,从其前后质量比中,算出固体分由固体分算出,凝聚物量(),用#200网眼的滤布过滤树脂乳液,残渣量对乳液的比值,以wt%表示,粒子径(nm)SR共聚率(%),耐水性(hr),动态光散乱法,测定温度25由HPLC法所测出的测量线算出SR的反应率往乳液中添加3%的TEXANOL成膜助剂,后用涂布器在玻璃板上制作2密耳厚的涂膜,干燥3天后,浸入50的温水中,测定直至8号文字所不能辨认为止时所花的时间,评价方法,聚合过程及评价方法丙烯酸体系乳液聚合配方的探讨BA/MMA/AA=49/49/2wt%苯乙烯体系乳液聚合配方的探讨,ADEKACORPORATION,20,-1.添加量效果,ADEKACORPORATION,21,SR-10onmonomer(%)InitialSR-10(%)Initialmonomer(%),2.535,1.555,0.75105,57.20,deeF,F,al,ks,mE,lu,is,no,Results,ADEKACORPORATION,22,160,234,180,50,100,250,300,150200Particlesize(nm),0.75,1.5,2.5,1,0.08,0.05,0,0.1,0.4,0.5,0.20.3Coagulation(%),0.75,1.5,2.5,95,95,95,0.75,1.5,2.5,Totalemulsifier=2.5%,2,216,340,0,100,500,600,200300400Waterresistance(hr),0.75,1.5,2.5,SR-10onmonomer(%),0255075100ConversionofSR-10(%)添加量越多,耐水性也越好。
SR-10onmonomer(%),2-2.SR-10=2.5%时的配方最优化(初期单体/乳化剂比),ADEKACORPORATION,23,Coagulation(%),Waterresistance(hr/50),SR-10Conversion(%),0.121695,0.0519695,0.0534095,0.0550495,deeF,F,al,ks,E,m,lu,is,no,Recommendation,Results,ADEKACORPORATION,24,145,145,180,280,50,100,250,300,150200Particlesize(nm),10/10,5/10,5/3,5/1,0.1,0.05,0.05,0.05,0,0.1,0.4,0.5,0.20.3Coagulation(%),10/10,5/10,5/3,5/1,Totalemulsifier=2.5%,504,100,500,600,200300400Waterresistance(hr),Monomer%/SAA%,Monomer%/SAA%,02550751000ConversionofSR-10(%)初期单体5%/初期乳化剂1%时,耐水性最好。
单体和SR转化率的推移,ADEKACORPORATION,25,Monomer,SR-10,0,25,50,75,100,0,6,C,vmo,re,is,o,n,%(,),MonomerSR-10,Monomer,SR-10,0,25,50,75,100,0,C,vmo,re,is,o,n,(,)%,MonomerSR-10,SAA单体减量,Monomerdroplet,Monomer,droplet,24Time(hr)初期聚合单体/SR-10=5/10wt%,单体转化率过快,SR残留,246Time(hr)初期聚合单体/SR-10=5/1wt%单体和SR的聚合速度接近时,是比较容易共聚的环境,聚合动向及其对涂膜的影响(推断),ADEKACORPORATION,26,Monomer/SR相互共聚,高,低,聚合物链,SR相互共聚,SR局部存在,融合过程,F,ADEKACORPORATION,27,ism,2-3.SR-10=1.5%时的配方最优化(初期单体/乳化剂比)Recommendation,Results,ADEKACORPORATION,28,Particlesize(nm),Coagulation(%),Totalemulsifier=1.5%,336,500,600,200300400Waterresistance(hr),Monomer%/SAA%,Monomer%/SAA%,02550751000100ConversionofSR-10(%)初期单体5%/初期乳化剂1%时,耐水性最好。
2-4.推荐配方(结果),ADEKACORPORATION,29,1,2,3,4,SR-10,TNS-100,SampleNo.SurfactantkindSAAonmonomer(%),InitialSR-10(%)Initialmonomer(%)Solid(%),Averageparticlesize(nm),Coagulation(%),Waterresistance(hr/50),SR-10Conversion(%),SR-10=2.5%SR-10=1.5%,调整聚合配方,可降低凝聚物量、耐水性可达到340hr调整聚合配方,可降低凝聚物量、耐水性可达到216hr,Recommendation
(1),Recommendation
(2),E,um,sl,oi,n,TNS-100:
C13H27O(EO)10SO3NH4(非反应性乳化剂),聚合配方及评价方法丙烯酸体系乳液聚合配方的探讨苯乙烯体系乳液聚合配方的探讨BA/St/AA=49/49/2wt%,ADEKACORPORATION,30,*CS-12=3%/B-943=0.1%,ADEKACORPORATION,31,al,ism,Results,ADEKACORPORATION,32,166,136,127,50,100,150,200,Particlesize(nm),0.75%,1.5%,2.5%,1,0.054,0.045,0,0.2,0.8,1,0.40.6Coagulation(%),0.75%,1.5%,2.5%,53,60,89,0.75%0255075100,1.5%,2.5%,3,48,144,0,150,50100Waterresistance(hr),0.75%,1.5%,2.5%,ConversionofSR-10(%)SR-10的用量越多,耐水性也越好。
SR-10onmonomer(%),SR-10onmonomer(%),3-2.SR-10=2.5%时的配方最优化(初期单体/乳化剂比),ADEKACORPORATION,33,deeF,F,kasl,mE,lu,is,no,Recommendation,Results,ADEKACORPORATION,34,116,113,118,127,50,100,150,200,Particlesize(nm),10/20,10/10,5/5,5/3,0.39,0.15,0.058,0.045,0,0.1,0.4,0.5,0.20.3Coagulation(%),10/20,10/10,5/5,5/3,0,75,100,2550ConversionofSR-10(%),Totalemulsifier=2.5%,144,0,150,50100Waterresistance(hr),Monomer%/SAA%,Monomer%/SAA%,初期单体5%/初期表面活性剂3%时,耐水性最好。
单体和SR转化率的推移,ADEKACORPORATION,35,Monomer,SR-10,0,25,50,75,100,0,2,4,6,Time(hr),C,vmo,re,is,o,n,(,)%,MonomerSR-10,Monomer,SR-10,0,25,50,75,100,0,2,4,6,Time(hr),C,mo,ev,sr,oi,n,(,)%,MonomerSR-10,单体转化率过快,SR残留,单体和SR的聚合速度接近时,是比较容易共聚的环境,SAA单体减量,Monomerdroplet,Monomerdroplet,ADEKACORPORATION,36,deeF,F,kasl,mE,lu,is,no,3-3.SR-10=1.5%时的配方最优化(初期单体/乳化剂比)Recommendation,Results,ADEKACORPORATION,37,50,100,150,200,Particlesize(nm),0.3,0,0.1,0.4,0.5,0.20.3Coagulation(%),48,47,60,65,0,75,100,2550ConversionofSR-10(%),10/10,5/10,5/5,5/1,Totalemulsifier=1.5%,36,36,36,36,0,50100,150,Waterresistance(hr),10/10,5/10,5/5,5/1,Monomer%/SAA%,Monomer%/SAA%,添加量少时,即使调整初期单体/初期表面活性剂比率,耐水性也很难提高追加投料聚合,以提高共聚率,追加投料聚合过程(对单体SR-10=1.5%),ADEKACORPORATION,38,Initiator(APS、50%),Monomer(5%)Water(52%)Emulsifier(5%),Monomer(95%)Water(48%)Emulsifier(95%)Initiator(APS、50%),滴加乳液,3hr(75oC),成熟,2hr(75oC),1,2,3,4,初期聚合15分(75oC),配方(Solid46%),水单体,:
108g:
90g,乳化剂SR-10:
1.35g,APS,追加引发剂,:
0.2g:
0.2g,Flask,Drop(feed),Pastinitiator,1,2,3,4,5,成熟,1-3hr(60-75oC),6,调整温度,(60-75oC),追加投料聚合(对单体SR-10=1.5%),ADEKACORPORATION,39,Blank-,1APS,2TBH,3APS,4KPS,5V-50,SampleNo.InitiatortypeReductantAgingtemperatureSolid(%),Averageparticlesize(nm),Coagulation(%),Waterresistance(hr/50),SR-10Conversion(%),Redox体系(TBHorAPS/NaHSO3),能抑制凝聚物的产生,而且可进一步提高共聚率,CS-12(3%)、B-943(0.1%)R.T4days,E,m,lu,is,no,3-4推荐配方(结果),ADEKACORPORATION,40,SR-10=2.5%SR-10=1.5%,Recommendation
(1),Recommendation
(2),TNS-100:
C13H27O(EO)10SO3NH4(非反应性乳化剂)调整聚合配方,可降低凝聚物量,耐水性可达到144hr调整聚合配方,并进行追加投料聚合,以提高耐水性,mE,lu,is,no,总结在Ac体系,即使在Ac/St体系中,通过调整优化初期单体/SR-10,可提高SR-10共聚率及至耐水性SR-10的添加量越多,共聚率也越高、耐水性也越好(2.51.50.75%)。
显示出聚合初期乳化剂量的重要性。
像Ac/St体系那样使用疏水性的单体,SR-10的添加量较少时,可通过追加投料聚合提高耐水性。
若要控制凝聚物量,建议使用Redox体系低温条件下的追加投料聚合。
ADEKACORPORATION,41,
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- ADEKA反应型乳化剂SR ER系列在乳液聚合中的应用 ADEKA 反应 乳化剂 SR ER 系列 乳液聚合 中的 应用