水性環(huán)氧上漿劑的制備及其在碳纖維增強PA6復合材料中的應用研究
發(fā)布時間：2019-04-15 22:47
【摘要】：由于碳纖維的脆性,在碳纖維的生產和加工過程中往往會經歷反復摩擦過程而發(fā)生斷裂,降低了纖維本體強度,且易產生大量毛絲,不利于后續(xù)應用。通過上漿工藝,碳纖維表面包覆一層聚合物上漿劑,在保護碳纖維本體性能同時可減少毛絲量,改善纖維集束性,使得碳纖維加工性能和生產環(huán)境得到顯著改善。另外,碳纖維表面包覆的上漿樹脂還可增加基體樹脂對碳纖維的浸潤性,減少界面缺陷,從而能提高纖維與樹脂基體間的界面結合強度。由此可見上漿劑在碳纖維生產加工過程中扮演十分重要的角色。本論文首先以環(huán)氧樹脂E-44、E-51及雙酚F型環(huán)氧樹脂BPF為上漿樹脂主體,外加多種復配乳化劑,制備了一類外加乳化型環(huán)氧上漿劑(EX-SA)；其次,以二乙醇胺(DEA)和對氨基苯甲酸(PABA)分別對環(huán)氧樹脂E-44進行改性,合成了DEA改性E-44和PABA改性E-44兩種新型的環(huán)氧樹脂,并采用自乳化的方法,成功制備了陽離子型上漿劑(CA-SA)和陰離子型上漿劑(AN-SA)；再次,以聚乙二醇(PEG)對環(huán)氧樹脂E-51進行改性,合成了PEG改性E-51的環(huán)氧樹脂,自乳化制備了非離子型上漿劑(NO-SA).探討研究了上述四類環(huán)氧樹脂乳液的最佳制備工藝。采用商購的日本上漿劑(JP-SA)和自制的四類環(huán)氧乳液上漿劑對碳纖維進行上漿處理,對碳纖維的上漿率、毛絲量、上漿碳纖維的表面形貌和性質,以及上漿碳纖維單絲力學性能等進行了評價。此外,對上漿碳纖維-聚酰胺復合材料的機械性能進行了研究。主要研究結果如下：1、EX-SA的最佳制備條件為環(huán)氧樹脂E-44、離子型乳化劑十二烷基硫酸鈉(SDS)加入量2%、非離子型乳化劑聚氧乙烯脫水山梨醇單油酸酯(T-80)加入量2%、非離子型乳化劑烷基酚聚氧乙烯醚(OP-10)加入量4%、乳化溫度80℃、乳化時間30 min、加水速率3mL/min。CA-SA的最佳制備條件為E-44與DEA摩爾比為1：1.1、反應溫度70℃、反應時間60 min、加冰乙酸成鹽溫度60℃、加水溫度80℃、加水速率5mL/min。AN-SA的最佳制備條件為PABA與E-44摩爾比1：1、反應溫度80℃、反應時間2h、成鹽時加入三乙醇胺(TEA)與PABA摩爾比1：0.8、成鹽溫度65℃,加水溫度60℃。NO-SA的最佳制備條件為E-51與PEG 1000的摩爾比1：1、催化劑三苯基膦(TPP)添加量0.5%、反應溫度180℃、反應時間3h、加水溫度80℃。2、EX-SA和JP-SA處理碳纖維的上漿率略高于自乳化上漿劑(CA-SA、AN-SA、 NO-SA)處理碳纖維的上漿率。碳纖維經上漿處理后,纖維毛絲量有較大幅度的減少。未上漿碳纖維表面有較為明顯凹凸不平的溝槽,上漿后纖維表面溝槽變淺。上漿處理后碳纖維表面O有較大幅度提高,此外,CA-SA和AN-SA處理碳纖維的表面還含有少量N元素。上漿后碳纖維在300-450℃范圍內出現上漿劑的失重現象。碳纖維單絲拉伸強度在上漿前后變化不大,但上漿后纖維拉伸強度的離散性減小。3、碳纖維復合材料的密度隨碳纖維含量的增加而增大,流動性隨著碳纖維含量的增加而減小。碳纖維復合材料的拉伸強度和彎曲強度隨碳纖維含量的增加而增大,與未上漿碳纖維相比,上漿碳纖維制備復合材料的拉伸強度與彎曲強度增加,未上漿碳纖維制備復合材料的懸臂梁缺口(Izod)沖擊強度隨碳纖維含量的增加而減小,而經上漿處理后制備復合材料的Izod沖擊強度隨碳纖維含量的增加先增加后減小。未上漿碳纖維制備復合材料的斷面,纖維與樹脂基體結合面光滑,而經過上漿處理碳纖維制備復合材料的斷面,碳纖維與樹脂基體結合面粗糙,基體樹脂與碳纖維結合緊密。隨著碳纖維含量的增加,復合材料的儲能模量逐漸增大,損耗角正切值減小且向高溫方向偏移。
[Abstract]:Due to the brittleness of the carbon fiber, the fracture is often experienced during the production and processing of the carbon fiber, so that the strength of the fiber body is reduced, and a large number of filaments are easily generated, and the subsequent application is not favorable. The surface of the carbon fiber is coated with a layer of polymer sizing agent through a sizing process, so that the performance of the carbon fiber body can be protected, the yarn amount can be reduced, the fiber bundling property is improved, and the processing performance and the production environment of the carbon fiber are greatly improved. In addition, the sizing resin coated on the surface of the carbon fiber can increase the wettability of the matrix resin to the carbon fiber and reduce the interface defect, so that the interface bonding strength between the fiber and the resin matrix can be improved. It can be seen that the sizing agent plays a very important role in the process of carbon fiber production. In this paper, epoxy resin E-44, E-51 and bisphenol F epoxy resin BPF are used as the main body of sizing resin, and a variety of compound emulsifiers are applied to prepare a kind of additive emulsion type epoxy sizing agent (EX-SA). Two new types of epoxy resins modified E-44 and PA-modified E-44 were synthesized with diethanolamine (DEA) and p-aminobenzoic acid (PABA), and the self-emulsifying method was used to successfully prepare cationic sizing agent (CA-SA) and anionic sizing agent (AN-SA). The epoxy resin E-51 was modified with polyethylene glycol (PEG), and the epoxy resin of PEG-modified E-51 was synthesized and the non-ionic sizing agent (NO-SA) was prepared by self-emulsification. The optimum preparation technology of the above four kinds of epoxy resin emulsion was discussed. A commercial Japanese sizing agent (JP-SA) and a self-made four-class epoxy emulsion sizing agent are used for sizing the carbon fiber, and the sizing rate of the carbon fiber, the filament amount, the surface appearance and the property of the sizing carbon fiber, and the mechanical property of the sizing carbon fiber monofilament are evaluated. In addition, the mechanical properties of the sizing carbon fiber-polycarbodiimide composite were studied. The main results are as follows:1. The best preparation conditions for EX-SA are epoxy resin E-44, ionic emulsifier sodium dodecyl sulfate (SDS) adding amount of 2%, non-ionic emulsifier polyoxyethylene sorbitan monooleate (T-80) is added in an amount of 2%, the non-ionic emulsifier alkylphenol polyoxyethylene ether (OP-10) is added with an amount of 4 percent, the emulsifying temperature is 80 DEG C, the emulsification time is 30 minutes, the water adding rate is 3 mL/ min, the optimal preparation condition of the CA-SA is that the molar ratio of the E-44 to the DEA is 1: 1.1, the reaction temperature is 70 DEG C, the reaction time is 60 minutes, the glacial acetic acid is added to the salt temperature of 60 DEG C, The optimum preparation conditions for AN-SA were: the molar ratio of PABA to E-44 was 1:1, the reaction temperature was 80 鈩，
本文編號：2458556
[Abstract]:Due to the brittleness of the carbon fiber, the fracture is often experienced during the production and processing of the carbon fiber, so that the strength of the fiber body is reduced, and a large number of filaments are easily generated, and the subsequent application is not favorable. The surface of the carbon fiber is coated with a layer of polymer sizing agent through a sizing process, so that the performance of the carbon fiber body can be protected, the yarn amount can be reduced, the fiber bundling property is improved, and the processing performance and the production environment of the carbon fiber are greatly improved. In addition, the sizing resin coated on the surface of the carbon fiber can increase the wettability of the matrix resin to the carbon fiber and reduce the interface defect, so that the interface bonding strength between the fiber and the resin matrix can be improved. It can be seen that the sizing agent plays a very important role in the process of carbon fiber production. In this paper, epoxy resin E-44, E-51 and bisphenol F epoxy resin BPF are used as the main body of sizing resin, and a variety of compound emulsifiers are applied to prepare a kind of additive emulsion type epoxy sizing agent (EX-SA). Two new types of epoxy resins modified E-44 and PA-modified E-44 were synthesized with diethanolamine (DEA) and p-aminobenzoic acid (PABA), and the self-emulsifying method was used to successfully prepare cationic sizing agent (CA-SA) and anionic sizing agent (AN-SA). The epoxy resin E-51 was modified with polyethylene glycol (PEG), and the epoxy resin of PEG-modified E-51 was synthesized and the non-ionic sizing agent (NO-SA) was prepared by self-emulsification. The optimum preparation technology of the above four kinds of epoxy resin emulsion was discussed. A commercial Japanese sizing agent (JP-SA) and a self-made four-class epoxy emulsion sizing agent are used for sizing the carbon fiber, and the sizing rate of the carbon fiber, the filament amount, the surface appearance and the property of the sizing carbon fiber, and the mechanical property of the sizing carbon fiber monofilament are evaluated. In addition, the mechanical properties of the sizing carbon fiber-polycarbodiimide composite were studied. The main results are as follows:1. The best preparation conditions for EX-SA are epoxy resin E-44, ionic emulsifier sodium dodecyl sulfate (SDS) adding amount of 2%, non-ionic emulsifier polyoxyethylene sorbitan monooleate (T-80) is added in an amount of 2%, the non-ionic emulsifier alkylphenol polyoxyethylene ether (OP-10) is added with an amount of 4 percent, the emulsifying temperature is 80 DEG C, the emulsification time is 30 minutes, the water adding rate is 3 mL/ min, the optimal preparation condition of the CA-SA is that the molar ratio of the E-44 to the DEA is 1: 1.1, the reaction temperature is 70 DEG C, the reaction time is 60 minutes, the glacial acetic acid is added to the salt temperature of 60 DEG C, The optimum preparation conditions for AN-SA were: the molar ratio of PABA to E-44 was 1:1, the reaction temperature was 80 鈩，
本文編號：2458556
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