聚烯烃接枝N，N-二烯丙基三聚氰胺和纤维的制备及性能研究
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摘要
聚丙烯、聚乙烯等聚烯烃作为目前应用最广泛的热塑性聚合物材料,由于其非极性与半结晶性,一定程度地限制了其应用范围。通过对聚烯烃反应挤出接枝改性,可在非极性的聚烯烃分子链上引入极性或功能性侧基,赋予其特殊功能,大大拓宽其应用领域。同时,熔喷纺丝法和共混纺丝法是制备聚合物微／纳米纤维的重要途径,进一步为功能化聚烯烃材料的应用提供了方法。
本文在结合国内外聚烯烃功能改性研究成果的基础上,选择熔喷用聚丙烯(PP)、低密度聚乙烯(LDPE)和等规聚丙烯(iPP)三种有代表性的聚烯烃材料,以N,N-二烯丙基三聚氰胺(NDAM)为功能单体,采用双螺杆挤出机进行聚烯烃反应挤出接枝改性,制备获得了熔喷用聚丙烯接枝N,N-二烯丙基三聚氰胺(PP-g-NDAM),低密度聚乙烯接枝N,N-二烯丙基三聚氰胺(LDPE-g-NDAM)和等规聚丙烯接枝N,N-二烯丙基三聚氰胺(iPP-g-NDAM)三种接枝聚烯烃共聚物。在此基础上,采用熔喷纺丝法制备了PP-g-NDAM熔喷纤维,采用共混纺丝法将乙酸丁酸纤维素(CAB)与LDPE-g-NDAM, CAB/iPP-g-NDAM体系熔融挤出,利用丙酮出去CAB后,获得LDPE-g-NDAM与iPP-g-NDAM纳米纤维。
在PP-g-NDAM的研究中,利用红外光谱表征了接枝反应的发生,PP-g-NDAM的接枝率(GD)随过氧化二异丙苯(DCP)用量增加先上升后下降,随NDAM用量增加先快速上升而后缓慢上升；而PP-g-NDAM的熔体流动指数(MFI)随DCP用量增加表现为先下降后上升,随NDAM用量增加出现小幅下降；同时,利用抗氧剂Irganox1010/Irgafos168复配体系很好地抑制了反应挤出过程中PP的降解反应,提高了PP-g-NDAM的热稳定性。与PP相比,PP-g-NDAM未发生晶型转变,熔融温度(Tm)略有下降,结晶温度(Tc)明显上升,且大幅度提高了热稳定性。以最佳原料质量比制得的PP-g-NDAM熔喷纤维的平均直径为3.1μm。熔喷织物的断裂伸长率下降,透气性上升。纤维氯含量最高可达380μg/g PP-g-NDAM熔喷纤维,且氯漂可再生性较好。
在LDPE-g-NDAM的研究中,利用红外光谱表征了接枝反应的发生LDPE-g-NDAM的GD随过氧化苯甲酰(BPO)用量增加先上升后下降,随NDAM用量单调上升;而LDPE-g-NDAM的MFI随BPO用量增加而下降,随NDAM用量增加而上升；同时,利用液体石蜡、油酸很好地抑制了反应挤出过程中的交联反应。与LDPE相比,LDPE-g-NDAM的Tm略有下降,Tc小幅上升,且热稳定性变化不大。利用共混纺丝工艺制得的LDPE-g-NDAM纳米纤维的平均直径为486nm,活性氯含量最高可达35μg/g LDPE-g-NDAM纳米纤维,且氯漂可再生性较好。
在iPP-g-NDAM的研究中,利用红外光谱表征了接枝反应的发生,iPP-g-NDAM的GD随着DCP用量增加而上升,随NDAM用量增加而上升；而iPP-g-NDAM的MFI随DCP用量增加而明显上升,随NDAM用量增加而缓慢下降；与iPP相比,iPP-g-NDAM未发生晶型转变,Tm略有下降,Tc明显上升,且热稳定性提高。利用共混纺丝工艺制得的iPP-g-NDAM纳米纤维的平均直径为317nm,活性氯含量最高可达700μg/g iPP-g-NDAM纳米纤维,且氯漂可再生性较好。
As the most widely used thermoplastic polymer materials at present, the applications of polyolefin, particularly polypropylene and polyethylene, are restricted to some extent due to nonpolar and semicrystallization. Polar or functional lateral groups can be grafted onto nonpolar molecular chains of polyolefin via reactive extrusion, enduing it with special functions and making it applicable for more extensive fields. Meanwhile, melt-blown spinning and blended spinning are two important methods to prepare micro/nano fibers, which can be employed to applications of functional polyolefin.
In this paper, on the basis of present researches on the applications of functional polyolefin both in China and abroad, with melt-blown polypropylene (PP), low density polyethylene (LDPE) and isotactic polypropylene (iPP) selected as the representative polyolefin, and N,N-Diallylmelamine as the functional monomer, the grafting modification of polyolefin via reactive extrusion was taken on a twin-screw extruder. Consequently, melt-blown polypropylene grafted N,N-Diallylmelamine (PP-g-NDAM), low density polyethylene grafted N,N-Diallylmelamine (LDPE-g-NDAM), and isotactic polypropylene grafted N,N-Diallylmelamine (iPP-g-NDAM) were obtained. On the basis of previous study, PP-g-NDAM melt-blown fibers were prepared via melt-blown spinning, cellulose acetate butyrate (CAB)/LDPE-g-NDAM and CAB/iPP-g-NDAM binary hybrids melt extruded, obtaining corresponding nano-fibers via blended spinning.
In the study of PP-g-NDAM, the FTIR spectra illustrate that NDAM was successfully grafted onto PP backbone. The grafting degree (GD) of PP-g-NDAM increased firstly, then decreased with the increase of dicumyl peroxide (DCP) concentration, whereas the GD increased fast originally and then increased gently with the increase of NDAM concentration. However, the melt flow index (MFI) of PP-g-NDAM decreased originally, and then increased with increasing DCP concentration, and decreased slightly with the increase of NDAM concentration. Meanwhile, the degradation of PP was restrained and the thermal stability of PP-g-NDAM was improved after using the antioxygen Irganox1010/Irgafosl68 blends. No crystal tranformation occurred in PP-g-NDAM, as compared with PP, while its melting temperature (Tm) decreased slightly, crystallization temperature (Tc) increased obviously, and thermal stability was enhanced. The PP-g-NDAM melt-blown fibers prepared with the best weight ratio of raw material had an average diameter of 3.1μm. The elongation at break of obtained melt-blown fibers decreased, the air permeability was improved. The active chlorine content was 380μg/g PP-g-NDAM melt-blown fibers at the maximum, and PP-g-NDAM melt-blown fibers had excellent rechargeability of chlorine bleaching.
In the study of LDPE-g-NDAM, the FTIR spectra showed NDAM was successfully grafted on the backbone of LDPE. The GD of LDPE-g-NDAM increased firstly then decreased as the BPO concentration increased, and increased as the NDAM concentration increased. However, MFI of LDPE-g-NDAM decreased as the BPO concentration increased, and increased slightly as the NDAM concentration increased. Meanwhile, the crosslinking reaction of LDPE was restrained under using the liquid paraffin and oleic acid. Compared with LDPE, Tm of LDPE-g-NDAM decreased slightly, Tc increased, and thermal stability changed little. The LDPE-g-NDAM nano-fibers, which were prepared via blended spinning, had an average diameter of 486nm. The active chlorine content was 350μg/g LDPE-g-NDAM nano-fibers at the maximum, and LDPE-g-NDAM nano-fibers had excellent rechargeability of chlorine bleaching.
In the study of iPP-g-NDAM, the FTIR spectra showed NDAM was successfully grafted onto iPP backbone. The GD of iPP-g-NDAM increased as the DCP concentration increased, and increased as the NDAM concentration increased. However, MFI of iPP-g-NDAM increased as the DCP concentration increased, and increased slowly as the NDAM concentration increased. Compared with iPP, no crystal tranformation occurred in PP-g-NDAM, its Tm decreased slightly, Tc increased obviously, and thermal stability was enhanced. The iPP-g-NDAM nanofibers, which were prepared via combined spinning, had an average diameter of 317nm. The active chlorine content was 700μg/g iPP-g-NDAM nanofibers at the maximum, and iPP-g-NDAM nano-fibers had excellent rechargeability of chlorine bleaching.
本文在结合国内外聚烯烃功能改性研究成果的基础上,选择熔喷用聚丙烯(PP)、低密度聚乙烯(LDPE)和等规聚丙烯(iPP)三种有代表性的聚烯烃材料,以N,N-二烯丙基三聚氰胺(NDAM)为功能单体,采用双螺杆挤出机进行聚烯烃反应挤出接枝改性,制备获得了熔喷用聚丙烯接枝N,N-二烯丙基三聚氰胺(PP-g-NDAM),低密度聚乙烯接枝N,N-二烯丙基三聚氰胺(LDPE-g-NDAM)和等规聚丙烯接枝N,N-二烯丙基三聚氰胺(iPP-g-NDAM)三种接枝聚烯烃共聚物。在此基础上,采用熔喷纺丝法制备了PP-g-NDAM熔喷纤维,采用共混纺丝法将乙酸丁酸纤维素(CAB)与LDPE-g-NDAM, CAB/iPP-g-NDAM体系熔融挤出,利用丙酮出去CAB后,获得LDPE-g-NDAM与iPP-g-NDAM纳米纤维。
在PP-g-NDAM的研究中,利用红外光谱表征了接枝反应的发生,PP-g-NDAM的接枝率(GD)随过氧化二异丙苯(DCP)用量增加先上升后下降,随NDAM用量增加先快速上升而后缓慢上升；而PP-g-NDAM的熔体流动指数(MFI)随DCP用量增加表现为先下降后上升,随NDAM用量增加出现小幅下降；同时,利用抗氧剂Irganox1010/Irgafos168复配体系很好地抑制了反应挤出过程中PP的降解反应,提高了PP-g-NDAM的热稳定性。与PP相比,PP-g-NDAM未发生晶型转变,熔融温度(Tm)略有下降,结晶温度(Tc)明显上升,且大幅度提高了热稳定性。以最佳原料质量比制得的PP-g-NDAM熔喷纤维的平均直径为3.1μm。熔喷织物的断裂伸长率下降,透气性上升。纤维氯含量最高可达380μg/g PP-g-NDAM熔喷纤维,且氯漂可再生性较好。
在LDPE-g-NDAM的研究中,利用红外光谱表征了接枝反应的发生LDPE-g-NDAM的GD随过氧化苯甲酰(BPO)用量增加先上升后下降,随NDAM用量单调上升;而LDPE-g-NDAM的MFI随BPO用量增加而下降,随NDAM用量增加而上升；同时,利用液体石蜡、油酸很好地抑制了反应挤出过程中的交联反应。与LDPE相比,LDPE-g-NDAM的Tm略有下降,Tc小幅上升,且热稳定性变化不大。利用共混纺丝工艺制得的LDPE-g-NDAM纳米纤维的平均直径为486nm,活性氯含量最高可达35μg/g LDPE-g-NDAM纳米纤维,且氯漂可再生性较好。
在iPP-g-NDAM的研究中,利用红外光谱表征了接枝反应的发生,iPP-g-NDAM的GD随着DCP用量增加而上升,随NDAM用量增加而上升；而iPP-g-NDAM的MFI随DCP用量增加而明显上升,随NDAM用量增加而缓慢下降；与iPP相比,iPP-g-NDAM未发生晶型转变,Tm略有下降,Tc明显上升,且热稳定性提高。利用共混纺丝工艺制得的iPP-g-NDAM纳米纤维的平均直径为317nm,活性氯含量最高可达700μg/g iPP-g-NDAM纳米纤维,且氯漂可再生性较好。
As the most widely used thermoplastic polymer materials at present, the applications of polyolefin, particularly polypropylene and polyethylene, are restricted to some extent due to nonpolar and semicrystallization. Polar or functional lateral groups can be grafted onto nonpolar molecular chains of polyolefin via reactive extrusion, enduing it with special functions and making it applicable for more extensive fields. Meanwhile, melt-blown spinning and blended spinning are two important methods to prepare micro/nano fibers, which can be employed to applications of functional polyolefin.
In this paper, on the basis of present researches on the applications of functional polyolefin both in China and abroad, with melt-blown polypropylene (PP), low density polyethylene (LDPE) and isotactic polypropylene (iPP) selected as the representative polyolefin, and N,N-Diallylmelamine as the functional monomer, the grafting modification of polyolefin via reactive extrusion was taken on a twin-screw extruder. Consequently, melt-blown polypropylene grafted N,N-Diallylmelamine (PP-g-NDAM), low density polyethylene grafted N,N-Diallylmelamine (LDPE-g-NDAM), and isotactic polypropylene grafted N,N-Diallylmelamine (iPP-g-NDAM) were obtained. On the basis of previous study, PP-g-NDAM melt-blown fibers were prepared via melt-blown spinning, cellulose acetate butyrate (CAB)/LDPE-g-NDAM and CAB/iPP-g-NDAM binary hybrids melt extruded, obtaining corresponding nano-fibers via blended spinning.
In the study of PP-g-NDAM, the FTIR spectra illustrate that NDAM was successfully grafted onto PP backbone. The grafting degree (GD) of PP-g-NDAM increased firstly, then decreased with the increase of dicumyl peroxide (DCP) concentration, whereas the GD increased fast originally and then increased gently with the increase of NDAM concentration. However, the melt flow index (MFI) of PP-g-NDAM decreased originally, and then increased with increasing DCP concentration, and decreased slightly with the increase of NDAM concentration. Meanwhile, the degradation of PP was restrained and the thermal stability of PP-g-NDAM was improved after using the antioxygen Irganox1010/Irgafosl68 blends. No crystal tranformation occurred in PP-g-NDAM, as compared with PP, while its melting temperature (Tm) decreased slightly, crystallization temperature (Tc) increased obviously, and thermal stability was enhanced. The PP-g-NDAM melt-blown fibers prepared with the best weight ratio of raw material had an average diameter of 3.1μm. The elongation at break of obtained melt-blown fibers decreased, the air permeability was improved. The active chlorine content was 380μg/g PP-g-NDAM melt-blown fibers at the maximum, and PP-g-NDAM melt-blown fibers had excellent rechargeability of chlorine bleaching.
In the study of LDPE-g-NDAM, the FTIR spectra showed NDAM was successfully grafted on the backbone of LDPE. The GD of LDPE-g-NDAM increased firstly then decreased as the BPO concentration increased, and increased as the NDAM concentration increased. However, MFI of LDPE-g-NDAM decreased as the BPO concentration increased, and increased slightly as the NDAM concentration increased. Meanwhile, the crosslinking reaction of LDPE was restrained under using the liquid paraffin and oleic acid. Compared with LDPE, Tm of LDPE-g-NDAM decreased slightly, Tc increased, and thermal stability changed little. The LDPE-g-NDAM nano-fibers, which were prepared via blended spinning, had an average diameter of 486nm. The active chlorine content was 350μg/g LDPE-g-NDAM nano-fibers at the maximum, and LDPE-g-NDAM nano-fibers had excellent rechargeability of chlorine bleaching.
In the study of iPP-g-NDAM, the FTIR spectra showed NDAM was successfully grafted onto iPP backbone. The GD of iPP-g-NDAM increased as the DCP concentration increased, and increased as the NDAM concentration increased. However, MFI of iPP-g-NDAM increased as the DCP concentration increased, and increased slowly as the NDAM concentration increased. Compared with iPP, no crystal tranformation occurred in PP-g-NDAM, its Tm decreased slightly, Tc increased obviously, and thermal stability was enhanced. The iPP-g-NDAM nanofibers, which were prepared via combined spinning, had an average diameter of 317nm. The active chlorine content was 700μg/g iPP-g-NDAM nanofibers at the maximum, and iPP-g-NDAM nano-fibers had excellent rechargeability of chlorine bleaching.
引文
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