通用型沥青基炭纤维纺丝工艺的优化研究
|
摘要
以软化点为294℃、喹啉不溶物为28.35%的各向同性沥青为原料,以通用型沥青基炭纤维的丝径与抗拉强度为评价指标,选择原丝制备过程中的纺丝温度、纺丝压力和拉伸速率工艺参数,运用三元二次回归正交设计对纺丝工艺进行优化组合,探究了最佳的纺丝工艺条件。研究结果表明,纺丝温度及纺丝压力对炭纤维丝径与抗拉强度的显著性影响大于拉伸速率的显著性影响。在纺丝温度为383℃、纺丝压力为0.26 MPa、拉伸速率为319 m/min的条件下进行熔融纺丝,将纺制的原丝经过预氧化和炭化处理后,获得的炭纤维丝径为15.6μm,其抗拉强度达到631 MPa。
The isotropic spinning pitch with the softening point of 294 ℃ and the quinoline insoluble of 28.35% was used as the raw material to prepare pitch based carbon fibers. The diameter and the tensile strength of the carbon fiber were used as the evaluation index, and the spinning temperature, spinning pressure and spinning velocity were used as technological parameters. The optimization condition of the spinning was studied by the quadratic regression orthogonal design. The results showed that the significant effect of spinning temperature and spinning pressure on the diameter and tensile strength of the carbon fiber is greater than that of tensile velocity. The carbon fiber with a diameter of 15.6 μm and tensile strength of 631 MPa was obtained using the spinning temperature of 383 ℃, spinning pressure of 0.26 MPa and the tensile velocity of 319 m/min and after pre-oxidation and carbonization.
The isotropic spinning pitch with the softening point of 294 ℃ and the quinoline insoluble of 28.35% was used as the raw material to prepare pitch based carbon fibers. The diameter and the tensile strength of the carbon fiber were used as the evaluation index, and the spinning temperature, spinning pressure and spinning velocity were used as technological parameters. The optimization condition of the spinning was studied by the quadratic regression orthogonal design. The results showed that the significant effect of spinning temperature and spinning pressure on the diameter and tensile strength of the carbon fiber is greater than that of tensile velocity. The carbon fiber with a diameter of 15.6 μm and tensile strength of 631 MPa was obtained using the spinning temperature of 383 ℃, spinning pressure of 0.26 MPa and the tensile velocity of 319 m/min and after pre-oxidation and carbonization.
引文
[1]邓洪贵,唐寄云,张秀云,等.通用型沥青基炭纤维的发展和应用[J].炭素技术,2015,34(1):40-44.
[2]Yang J,Nakabayashi K,Jin M,et al.Preparation of pitch based carbon fibers using hyper-coal as a raw material[J].Carbon,2016,106:28-36.
[3]Kim B J,Kotegawa T,Eom Y,et al.Enhancing the tensile strength of isotropic pitchbased carbon fibers by improving the stabilization and carbonization properties of precursor Pitch[J].Carbon,2015,99:649-657.
[4]Wang S,Chen Z H,Ma W J,et al.Influence of heat treatment on physical-chemical properties of PAN-based carbon fiber[J].Ceramics International,2006,32(3):291-295.
[5]Ismail K,Soy T.Investigation of structural transformations taking place during oxidative stabilization of viscose rayon precursor fibers prior to carbonization and activation[J].Journal of Molecular Structure,2013,1041(43):2009-2021.
[6]Alcaniz-Monge J,Cazorla-Amoros D,Linares-Solano A,et al.Preparation of general purpose carbon fibers from coal tar pitches with low softening point[J].Carbon,1997,35(8):1079-1087.
[7]Maeda T,Zeng S M,Tokumitsue K,et al.Preparation of isotropic pitch precursors for general purpose carbon fibers(GPCF)by air blowing-Ⅰ.Preparation of spinnable isotropic pitch precursor from coal tar by air blowing[J].Carbon,1993,31(3):407-412.
[8]Maeda T,Zeng S M,Tokumitsu K,et al.Preparation of isotropic pitch precursors for general purpose carbon fibers(GPCF)by air blowing-Ⅱ.Air blowing of coal tar,hydrogenated coal tar,and petroleum pitches[J].Carbon,1993,31(3):413-419.
[9]Mdada T,Zeng S M,Tokumitsue K.Preparation of isotropic pitch precursors for general purpose carbon fibers(GPCF)by air blowing-Ⅲ.Air blowing of isotropic naphthalene and hydrogenated coal tar pitches with addition of 1,8-dinitro naphthalene[J].Carbon,1993,31(3):421-426.
[10]Mora E,Blanco C,Prada V,et al.A study of pitch-based precursors for general purpose carbon fibres[J].Carbon,2002,40(14):2719-2725.
[11]Mora E,Blanco C,Santamaria R,et al.A novel method to obtain a petroleum-derived mesophase pitch suitable as carbon fibre precursor[J].Carbon,2003,41(3):445-452.
[12]Edie D D,Dunham M G.Melt spinning pitch-based carbon fibers[J].Carbon,1989,27(5):647-655.
[13]贺福.碳纤维及其应用技术[M].北京:化学工业出版社,2004:8-9.
[2]Yang J,Nakabayashi K,Jin M,et al.Preparation of pitch based carbon fibers using hyper-coal as a raw material[J].Carbon,2016,106:28-36.
[3]Kim B J,Kotegawa T,Eom Y,et al.Enhancing the tensile strength of isotropic pitchbased carbon fibers by improving the stabilization and carbonization properties of precursor Pitch[J].Carbon,2015,99:649-657.
[4]Wang S,Chen Z H,Ma W J,et al.Influence of heat treatment on physical-chemical properties of PAN-based carbon fiber[J].Ceramics International,2006,32(3):291-295.
[5]Ismail K,Soy T.Investigation of structural transformations taking place during oxidative stabilization of viscose rayon precursor fibers prior to carbonization and activation[J].Journal of Molecular Structure,2013,1041(43):2009-2021.
[6]Alcaniz-Monge J,Cazorla-Amoros D,Linares-Solano A,et al.Preparation of general purpose carbon fibers from coal tar pitches with low softening point[J].Carbon,1997,35(8):1079-1087.
[7]Maeda T,Zeng S M,Tokumitsue K,et al.Preparation of isotropic pitch precursors for general purpose carbon fibers(GPCF)by air blowing-Ⅰ.Preparation of spinnable isotropic pitch precursor from coal tar by air blowing[J].Carbon,1993,31(3):407-412.
[8]Maeda T,Zeng S M,Tokumitsu K,et al.Preparation of isotropic pitch precursors for general purpose carbon fibers(GPCF)by air blowing-Ⅱ.Air blowing of coal tar,hydrogenated coal tar,and petroleum pitches[J].Carbon,1993,31(3):413-419.
[9]Mdada T,Zeng S M,Tokumitsue K.Preparation of isotropic pitch precursors for general purpose carbon fibers(GPCF)by air blowing-Ⅲ.Air blowing of isotropic naphthalene and hydrogenated coal tar pitches with addition of 1,8-dinitro naphthalene[J].Carbon,1993,31(3):421-426.
[10]Mora E,Blanco C,Prada V,et al.A study of pitch-based precursors for general purpose carbon fibres[J].Carbon,2002,40(14):2719-2725.
[11]Mora E,Blanco C,Santamaria R,et al.A novel method to obtain a petroleum-derived mesophase pitch suitable as carbon fibre precursor[J].Carbon,2003,41(3):445-452.
[12]Edie D D,Dunham M G.Melt spinning pitch-based carbon fibers[J].Carbon,1989,27(5):647-655.
[13]贺福.碳纤维及其应用技术[M].北京:化学工业出版社,2004:8-9.