水性中间相沥青溶液的可纺性研究
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摘要
以生焦为原料,通过混酸氧化制备得到水性中间相沥青(AMP)。对AMP的产率和温度之间的关系进行了研究,并由AMP制备得到纺丝溶液,用硫酸做凝固浴进行纺丝。利用热重、红外和流变等测试方法对不同温度下得到的AMP碳收率及其可纺性进行研究,结果表明:AMP在60℃氧化温度下最高产率达140%左右;当m(PAN)/m(AMP)为10%时,溶解于DMSO的纺丝液能够连续纺丝数千米。
The aqua-mesophase pitch(AMP) was prepared by a green needle coke and by mixed acid oxida-tion. The relationship between yield and temperature of AMP was studied. Then a gel solution was got bydissolving AMP, which was spun and coagulated by sulfuric acid. The carbon yield and spinning propertywere studied by TG, FT-IR and rotational rheometer. The results indicate that the maximum yield of AMPis about 140% at the oxidation temperature of 60 ℃. When m(PAN)/m(AMP) is 10%, the spinning solutioninto dimethylsulfoxide(DMSO) can spin fiber thousands of meters.
The aqua-mesophase pitch(AMP) was prepared by a green needle coke and by mixed acid oxida-tion. The relationship between yield and temperature of AMP was studied. Then a gel solution was got bydissolving AMP, which was spun and coagulated by sulfuric acid. The carbon yield and spinning propertywere studied by TG, FT-IR and rotational rheometer. The results indicate that the maximum yield of AMPis about 140% at the oxidation temperature of 60 ℃. When m(PAN)/m(AMP) is 10%, the spinning solutioninto dimethylsulfoxide(DMSO) can spin fiber thousands of meters.
引文
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[16]TATEISHI D,ESUMI K,HONDA H,et al.Preparation of carbonaceous gel beads[J].Carbon,1992,30(6):942-944.
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[19]RIZVI A,ANDALIB Z K M,PARK C B.Fiber-spun polypropylene/polyethylene terephthalate microfibrillar composites with enhanced tensile and rheological properties and foaming ability[J].Polymer,2017,110(Supplement C):139-148.
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[21]周游.高分子量高等规聚丙烯腈沉淀聚合和纺丝液流变性能及其预氧化的研究[D].北京:北京化工大学,2013.
[2]WATANABE F,KORAI Y,MOCHIDA I,et al.Structure of meltblown mesophase pitch-based carbon fiber[J].Carbon,2000,38(5):741-747.
[3]郑嘉明,王成扬,阮湘泉,等.催化缩聚法制备萘沥青和中间相沥青[J].天津大学学报,1995(2):215-220.
[4]PéREZ M,GRANDA M,SANTAMARI?A R,et al.A thermoanalytical study of the co-pyrolysis of coal-tar pitch and petroleum pitch[J].Fuel,2004,83(9):1257-1265.
[5]KORAI Y,MOCHIDA I.Molecular assembly of mesophase and isotropic pitches at their fused states[J].Carbon,1992,30(7):1019-1024.
[6]LüY,WU D,ZHA Q,et al.Skin-core structure in mesophase pitchbased carbon fibers:causes and prevention[J].Carbon,1998,36(12):1719-1724.
[7]MURAKAMI K,OKUMURA M,YAMAMOTO M,et al.Structural analysis of mesophase pitch with high-resolution,high-temperature13CNMR[J].Carbon,1996,34(2):187-192.
[8]XU Z,GAO C.Graphene chiral liquid crystals and macroscopic assembled fibres[J].Nature Communication,2011(2):571.
[9]XU Z,GAO C.Aqueous liquid crystals of graphene oxide[J].ACS Nano,2011,5(4):2908-2915.
[10]XU Z,GAO C.Graphene in macroscopic order:Liquid crystals and wet-spun fibers[J].Accounts of Chemical Research,2014,47(4):1267-1276.
[11]FUJII M,YAMADA Y,IMAMURA T.Preparation of aqua-mesophase by nitration or sulfonation of carbonaceous mesophase and properties of carbon material made from it[A]//18th Biennial Conference of Carbon[C].1987:405-406.
[12]SUGII H,ESUMI K,HONDA H,et al.Characterization of carbonaceous gel beads prepared in presence of polymer using water-in-oil emulsion[J].Carbon,1995,33(6):821-825.
[13]LI X,LIU L,SHEN S.Structure of ultrafine carbon powders prepared using a carbonaceous gel[J].Carbon,2001,39(9):1431-1433.
[14]WU W,ZHU Z,LIU Z.Amorphous carbon nano-particles prepared by explosion of nitrated pitch[J].Carbon,2002,40(11):2034-2037.
[15]ESUMI K,TATEISHI D,KUDOH S,et al.Carbonaceous gel obtained by oxidation of coaltar pitch with hydrogen perioxide[J].Carbon,1993,31(8):1357-1358.
[16]TATEISHI D,ESUMI K,HONDA H,et al.Preparation of carbonaceous gel beads[J].Carbon,1992,30(6):942-944.
[17]KREBS V,ELALAOUI M,MARECHE J F,et al.Carbonization of coal-tar pitch under controlled atmosphere—Part I:Effect of temperature and pressure on the structural evolution of the formed green coke[J].Carbon,1995,33(5):645-651.
[18]李元祥.日本针状焦性能研究[J].炭素技术,1993(4):7-12.
[19]RIZVI A,ANDALIB Z K M,PARK C B.Fiber-spun polypropylene/polyethylene terephthalate microfibrillar composites with enhanced tensile and rheological properties and foaming ability[J].Polymer,2017,110(Supplement C):139-148.
[20]JIA X,CHEN Y,SHI C,et al.Rheological properties of an amorphous cellulose suspension[J].Food Hydrocolloids,2014,39(Supplement C):27-33.
[21]周游.高分子量高等规聚丙烯腈沉淀聚合和纺丝液流变性能及其预氧化的研究[D].北京:北京化工大学,2013.