加压氧化对抑制中间相沥青纤维氧化粘连并丝的影响Effect of Oxidization-Stabilization under Pressure on Inhibiting the Adhesion of Mesophase Pitch Fibers
孙祝林,吕永根,尉言哲,杨常玲
SUN Zhu-lin,Lü Yong-gen,YU Yan-zhe,YANG Chang-ling
摘要(Abstract):
为了解决中间相沥青纤维氧化稳定化过程中由于纤维表面发生小分子挥发以及低分子质量组分软化导致的粘连并丝问题,采用加压空气和加压氧气对中间相沥青纤维进行氧化稳定化热处理,研究氧气分压和氧化气体的总压力对沥青纤维氧化粘连的影响。利用悬垂度的测试表征氧化沥青纤维的粘连程度,悬垂度越大说明纤维粘连程度越小。结果表明:空气中压力由0.10 MPa增至2.60 MPa时,氧化沥青纤维束的悬垂度由6%增加到82%;纯氧气氛下压力从0.40 MPa提高到0.60 MPa时,纤维束的悬垂度从42%提高到68%。分析表明,氧分压的提高起到抑制粘连的主要作用,而在相同氧分压下,总压提高也有利于降低粘连。另外加压氧化的方式有效地提升了氧化沥青纤维的均匀性。
Filaments in a mesophase pitch fiber tow could adhere to each other during the oxidization-stabilization process due to the volatilization of small molecules and softening of low molecular components. In order to solve this problem, pitch fibers are oxidized in air and oxygen under different pressures, and the adhesion of oxidized fibers are studied. The adhesion degree of oxidized pitch fibers is characterized by drape degree test. The greater the drape degree, the smaller the adhesion degree. The results show that in air,when the pressure increase from 0.10 MPa to 2.60 MPa, the drape degree of oxidized pitch fibers increase from 6% to 82%, while in oxygen, when the pressure of pure oxygen increased from 0.40 MPa to 0.60 MPa,the drape degree of oxidized pitch fibers increase from 42% to 68%. It is concluded that the increase of oxygen partial pressure plays a major role in the inhibition of adhesion, and the increase of total pressure with the same oxygen partial pressure is also beneficial to reduce adhesion. In addition, the homogeneity of oxidized pitch fiber can be improved by pressurized oxidation.
关键词(KeyWords):
中间相沥青纤维;氧化稳定化;粘连并丝;悬垂度
mesophase pitch fiber;oxidization-stabilization;adhesion;drape degree
基金项目(Foundation): 国家自然科学基金项目(编号51672042)
作者(Author):
孙祝林,吕永根,尉言哲,杨常玲
SUN Zhu-lin,Lü Yong-gen,YU Yan-zhe,YANG Chang-ling
DOI: 10.16090/j.cnki.hcxw.2021.06.006
参考文献(References):
- [1]LIU Y D,KUMAR S.Recent progress in fabrication,structure,and properties of carbon fibers[J].Polymer Reviews,2012,52(3-4):234-258.
- [2]YANG K S.KIM B H,YOON S H.Pitch based carbon fibers for automotive body and electrodes[J].Carbon Letters,2014,15(3):162-170.
- [3]FRANK E,STEUDLE L M,INGILDEEV D,et al.Carbon fibers:Precursor systems,processing,structure,and properties[J].Angewandte Chemie-International Edition,2014,53(21):5262-5298.
- [4]CHAND S.Review carbon fibers for composites[J].Journal of Materials Science,2000,35(6):1303-1313.
- [5]HUANG X.Fabrication and properties of carbon fibers[J].Materials,2009,2(4):2369-2403.
- [6]DHAMI T L,MANOCHA L M,BAHL O P.Oxidation behaviour of pitch based carbon fibers[J].Carbon,1991,29(1):51-60.
- [7]EDIE D D.The effect of processing on the structure and properties of carbon fibers[J].Carbon,1998,36(4):345-362.
- [8]FRANK E,HERMANUTZ F,BUCHMEISER M R.Carbon fibers:Precursors,manufacturing,and properties[J].Macromolecular Materials and Engineering,2012,297(6):493-501.
- [9]MINUS M L,KUMAR S.The processing,properties,and structure of carbon fibers[J].Journal of the Minerals Metals&Materials Society,2005,57(2):52-58.
- [10]BLANCO C,LU S,APPLEYARD S P,et al.The stabilization of carbon fibers studied by micro-thermal analysis[J].Carbon,2003,41(1):165-171.
- [11]LAVIN J G.Chemical-reactions in the stabilization of mesophase pitch-based carbon-fiber[J].Carbon,1992,30(3):351-357.
- [12]MIURA K,NAKAGAWA H,HASHIMOTOK.Examination of MP carbon fiber at the low temperature range[J].Carbon,1995,33(3):275-282.
- [13]吕永根.高性能炭纤维[M].北京:化学工业出版社,2016:3-4.
- [14]彭密雪,孙祝林,吕永根.集束液对中间相沥青纤维的集束性和抗并丝性的影响[J].合成纤维工业,2020,43(4):1-6.
- [15]YOON S H,KORAI Y,MOCHIDA I.Assessment and optimization of the stabilization process of mesophase pitch fibers by thermal analyses[J].Carbon,1994,32(2):281-287.
- [16]MOCHIDA I,TOSHIMA H,KORAI Y,et al.Oxygen distribution in the mesophase pitch fiber after oxidative stabilization[J].Journal of Materials Science,1989,24(2):389-394.
- [17]MOCHIDA I,YOON S H,TAKANO N,et al.Microstructure of mesophase pitch-based carbon fiber and its control[J].Carbon,1996,34(8):941-956.
- [18]MOCHIDA I,KORAI Y,KU C H,et al.Chemistry of synthesis,structure,preparation and application of aromatic-derived mesophase pitch[J].Carbon,2000,38(2):305-328.
- [19]YANG H,YOON S H,KORAI Y,et al.Microvoids present in anisotropic mesophase pitch,their as-spun and annealed fibers[J].Chemistry Letters,2003,32(2):168-169.
- [20]MATSUMOTO T,MOCHIDA I.A structural study on oxidative stabilization of mesophase pitch fibers derived from coal-tar[J].Carbon,1992,30(7):1041-1046.
- [21]LU Y G,WU D,ZHA Q F,et al.Skin-core structure in mesophase pitch-based carbon fibers:causes and prevention[J].Carbon,1998,36(12):17191724.
- [22]FATHOLLAHI B,JONES B,WHITE J L,et al.Injection and stabilization of mesophase pitch in the fabrication of carbon-carbon composites.Part III:Mesophase stabilization at low temperatures and elevated oxidation pressures[J].Carbon,2005,43(1):143-151.
- [23]LIEDTKE V,HUTTINGER K J.Mesophase pitches as matrix precursor of carbon fiber reinforced carbon:II.Stabilization of mesophase pitch matrix by oxygen treatment[J].Carbon,1996,34(9):1067-1079.
- [24]SHIMANOE H,SEUNGHYUN K,YOON S H,et al.Shortening Stabilization Time Using Pressurized Air Flow in Manufacturing Mesophase Pitch-Based Carbon Fiber[J].Polymers,2019,11(12):1911-1928.
- [25]TZENG S S,WANG P L.Oxidation of a petroleum pitch under pressure[J].Carbon,2001,39(7):1103-1106.
- [26]MOCHIDA I,SENG S M,KORAI Y.The introduction of a skin-core structure in mesophase pitch fibers by oxidative stabilization[J].Carbon,1990,28(1):193-198.
- [27]PEIRCE F T.The Handle of Cloth as a Measurable Quantity[J].Journal of the Textile Institute,1930,21(9):377-417.
- [28]贺福.碳纤维及石墨纤维[M].北京:化学工业出版社,2010:341-343.