PP无纺布上功能分子的固定及其吸附性能研究
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摘要
本论文以聚环氧氯丙烷(PECH)、聚氯乙烯(PVC)和氯醋树脂为原料,利用取代反应在其高分子骨架上引入叠氮基团后制得三种高分子叠氮化合物,聚叠氮缩水甘油醚(GAP)、叠氮聚氯乙烯以及叠氮氯醋树脂。探讨和优化了反应条件对高分子叠氮化合物合成的影响,并对部分叠氮化合物进行了FTIR、XPS和热分析,证明叠氮基团确被引入相应的高分子链上。以所得高分子叠氮化合物为光偶联剂,在UV辐照下将明胶分子固定到PP无纺布上,制得了相应的PP无纺布UV光固定明胶。用单因素实验对光固定反应条件进行了优化。实验结果表明,GAP的UV光固定反应优化后条件为：GAP(3)浓度为8.3g/L和12.5g/L,涂覆工艺为1+1方式,UV辐照30min,明胶固载量可达到9.33g/g(L)和3.59g/g(R)。叠氮PVC的UV光固定反应优化后条件为：叠氮PVC(4)浓度为10g/L,涂覆工艺为1+1方式,UV辐照30min,同样条件下明胶固载量可达到7.89g/g(L)和3.81g/g(R)。叠氮氯醋树脂的UV光固定反应优化后条件为：叠氮氯醋树脂(4)浓度为10g/L,涂覆工艺为1+1方式,UV辐照30min,同样条件下明胶固载量可达到6.10g/g(L)和3.41g/g(R)。
本文利用茚三酮—氨基酸显色分光光度法对PP无纺布上所固定的明胶量进行了测定,研究了PP无纺布光固定明胶的吸水溶胀性能,探讨了光固定明胶固载量对固定率、吸水率和氨基酸固载量的影响,发现明胶固定率及氨基酸固载量与固载量呈正相关,光固定产物上明胶固载量越大,吸水率越低。
本文对PP无纺布UV光固定明胶的单宁酸吸附性能进行了研究。在20℃下,50mL200mg/L的单宁酸吸附原液中,固载量为0.79g/g(R)的GAP光固定明胶0.2g,搅拌下吸附3h,单宁酸脱出率可达到92.4%,吸附量Q为0.0492g/g。同样条件下,固载量为3.12g/g(R)的叠氮PVC光固定明胶对单宁酸的脱出率可达到96.6%,吸附量Q为0.0514g/g。在室温下,100mL 200mg/L的单宁酸吸附原液中,固载量为2.34g/g(L)的叠氮氯醋树脂光固定明胶0.2g搅拌下吸附24h,对单宁酸脱出率可达到97.7%,吸附量Q为0.1300g/g。吸附实验结果表明,明胶固载量n对吸附性能的影响具有明显规律性,单宁酸吸附原液浓度越低,吸附时间越长,PP无纺布光固定明胶投料量越大,对单宁酸的吸附量也越大。
本文还对部分PP无纺布UV光固定明胶及其吸附后样品进行了FTIR分析、扫描电镜(SEM)分析、X光电子能谱(XPS)分析以及热分析。FTIR结果表明,PP无纺布UV辐照光固定明胶上2100cm-1附近的叠氮基团含量明显减少甚至消失,从XPS结果可推测出各样品上元素的贡献源基团及含量,对热分析中TG、DTG、DTA曲线及数据的分析表明明胶分子已被固定到PP无纺布上,其吸附后样品上单宁结构基团的出现证明对单宁酸吸附的实现。SEM照片中清晰地揭示了PP纤维表面形貌在光固定明胶后发生了较大变化,PP纤维间隙被固定明胶所填充,在吸附单宁酸后PP纤维直径进一步变粗,表面被一层吸附质所包裹,证实单宁酸已被吸附到光固定明胶表面。
In this paper, with polyepichlorohydrin (PECH), polyvinyl chloride (PVC) and Vinyl chloride-acetate as the raw materials, the azide group was introduced into corresponding polymer chains by substitution of chloride atom, and three kinds of polymeric azides were prepared. Several effect factors of the azidation were investigated, and some of azidated polymers were characterized by using FTIR、XPS and Thermal analysis, The results revealed that the azide group was indeed introduced into polymer chains. Gelatin was immobilized onto PP non-woven fabrics(PNF) with polymeric azides as photolinker assisted by UV radiation. the optimum condition of immobilization could be given as follow:①concentration of GAP(3) solution 8.3g/L and 12.5g/L, coating process 1+1, UV radiation for 30min, the immobilization quantity can reach 9.33g/g(L) and 3.59g/g(R), respectively.②concentration of azidated PVC(4) 10g/L, coating process 1+1, UV radiation for 30min, the immobilization quantity can reach 7.89g/g(L) and 3.81g/g(R), respectively.③concentrain of azidated Vinyl chloride-acetate(4) 10g/L, coating process 1+1, UV radiation for 30min, the immobilization quantity can reach 6.10g/g(L) and 3.41g/g(R), respectively.
The content of gelatin immobilized on PNF were determined by using 3-dioxohydrindene-amino acid color spectorphotometry, and its water absorption was studied, The influence of immobilization quantity on immobilization rate, water absorption and amino acid immobilization quantity were discussed as well. It was found that the immobilization rate and amino acid immobilization quantity increase with immobilization quantity meeted positive correlation, and water absorption was reduced as the immobilization quantity increased. The adsorption of tannin by gelatin immobilized on PNF was studied in this work. When stirring 3h in 50mL tannin solution (200mg/L) at 20℃by using 0.2g GAP immobilization products(immobilization quantity 0.79g/g(R)) as adsorbent, the removal percentage of tannin and adsorption quantity Q can reach 92.4% and 0.0492g/g respectively, in the same condition,96.6% and 0.0514g/g can be achieved by using 0.2g azidated PVC immobilization products(immobilization quantity 3.12g/g(R)) as adsorbent,97.7% and 0.1300g/g by using 0.2g azidated Vinyl chloride-acetate(immobilization quantity 2.34g/g(R)) as adsorbent, but stirring for 24h at room temperature. The results show that the the adsorption quantity has obvious regularity in adsorptivity. The result indicates that the adsorption quality could be increased by the lower concentration of tannin solution, the longer adsorption time and the higher quantity of immobilization products.
The gelatin immobilized on PNF and their adsorbed sample were also characterized by using FTIR, SEM, XPS and thermal analysis. The results showed that the content of azide groups(corresponding FTIR adsorbance at 2100cm-1) were significantly reduced or even disappeared after UV radiation. Chemical composition and its contribution groups were determined by XPS. The results from TG、DTG and DTA revealed that the gelatin molecules had been immobilized onto PNF. The emergence of tannin structure on the adsorbed sample confirmed that tannin had been adsorbed on the surface of gelatin immobilized on PNF. The surface morphology of PNF had been changed greatly after immobilization of gelatin, gelatin filled between PP fibers and PP fibers became thicker after adsorption, its surface was covered with adsorbate. These results revealed that tannin has been adsorbed on the surface of immobilization product.
本文利用茚三酮—氨基酸显色分光光度法对PP无纺布上所固定的明胶量进行了测定,研究了PP无纺布光固定明胶的吸水溶胀性能,探讨了光固定明胶固载量对固定率、吸水率和氨基酸固载量的影响,发现明胶固定率及氨基酸固载量与固载量呈正相关,光固定产物上明胶固载量越大,吸水率越低。
本文对PP无纺布UV光固定明胶的单宁酸吸附性能进行了研究。在20℃下,50mL200mg/L的单宁酸吸附原液中,固载量为0.79g/g(R)的GAP光固定明胶0.2g,搅拌下吸附3h,单宁酸脱出率可达到92.4%,吸附量Q为0.0492g/g。同样条件下,固载量为3.12g/g(R)的叠氮PVC光固定明胶对单宁酸的脱出率可达到96.6%,吸附量Q为0.0514g/g。在室温下,100mL 200mg/L的单宁酸吸附原液中,固载量为2.34g/g(L)的叠氮氯醋树脂光固定明胶0.2g搅拌下吸附24h,对单宁酸脱出率可达到97.7%,吸附量Q为0.1300g/g。吸附实验结果表明,明胶固载量n对吸附性能的影响具有明显规律性,单宁酸吸附原液浓度越低,吸附时间越长,PP无纺布光固定明胶投料量越大,对单宁酸的吸附量也越大。
本文还对部分PP无纺布UV光固定明胶及其吸附后样品进行了FTIR分析、扫描电镜(SEM)分析、X光电子能谱(XPS)分析以及热分析。FTIR结果表明,PP无纺布UV辐照光固定明胶上2100cm-1附近的叠氮基团含量明显减少甚至消失,从XPS结果可推测出各样品上元素的贡献源基团及含量,对热分析中TG、DTG、DTA曲线及数据的分析表明明胶分子已被固定到PP无纺布上,其吸附后样品上单宁结构基团的出现证明对单宁酸吸附的实现。SEM照片中清晰地揭示了PP纤维表面形貌在光固定明胶后发生了较大变化,PP纤维间隙被固定明胶所填充,在吸附单宁酸后PP纤维直径进一步变粗,表面被一层吸附质所包裹,证实单宁酸已被吸附到光固定明胶表面。
In this paper, with polyepichlorohydrin (PECH), polyvinyl chloride (PVC) and Vinyl chloride-acetate as the raw materials, the azide group was introduced into corresponding polymer chains by substitution of chloride atom, and three kinds of polymeric azides were prepared. Several effect factors of the azidation were investigated, and some of azidated polymers were characterized by using FTIR、XPS and Thermal analysis, The results revealed that the azide group was indeed introduced into polymer chains. Gelatin was immobilized onto PP non-woven fabrics(PNF) with polymeric azides as photolinker assisted by UV radiation. the optimum condition of immobilization could be given as follow:①concentration of GAP(3) solution 8.3g/L and 12.5g/L, coating process 1+1, UV radiation for 30min, the immobilization quantity can reach 9.33g/g(L) and 3.59g/g(R), respectively.②concentration of azidated PVC(4) 10g/L, coating process 1+1, UV radiation for 30min, the immobilization quantity can reach 7.89g/g(L) and 3.81g/g(R), respectively.③concentrain of azidated Vinyl chloride-acetate(4) 10g/L, coating process 1+1, UV radiation for 30min, the immobilization quantity can reach 6.10g/g(L) and 3.41g/g(R), respectively.
The content of gelatin immobilized on PNF were determined by using 3-dioxohydrindene-amino acid color spectorphotometry, and its water absorption was studied, The influence of immobilization quantity on immobilization rate, water absorption and amino acid immobilization quantity were discussed as well. It was found that the immobilization rate and amino acid immobilization quantity increase with immobilization quantity meeted positive correlation, and water absorption was reduced as the immobilization quantity increased. The adsorption of tannin by gelatin immobilized on PNF was studied in this work. When stirring 3h in 50mL tannin solution (200mg/L) at 20℃by using 0.2g GAP immobilization products(immobilization quantity 0.79g/g(R)) as adsorbent, the removal percentage of tannin and adsorption quantity Q can reach 92.4% and 0.0492g/g respectively, in the same condition,96.6% and 0.0514g/g can be achieved by using 0.2g azidated PVC immobilization products(immobilization quantity 3.12g/g(R)) as adsorbent,97.7% and 0.1300g/g by using 0.2g azidated Vinyl chloride-acetate(immobilization quantity 2.34g/g(R)) as adsorbent, but stirring for 24h at room temperature. The results show that the the adsorption quantity has obvious regularity in adsorptivity. The result indicates that the adsorption quality could be increased by the lower concentration of tannin solution, the longer adsorption time and the higher quantity of immobilization products.
The gelatin immobilized on PNF and their adsorbed sample were also characterized by using FTIR, SEM, XPS and thermal analysis. The results showed that the content of azide groups(corresponding FTIR adsorbance at 2100cm-1) were significantly reduced or even disappeared after UV radiation. Chemical composition and its contribution groups were determined by XPS. The results from TG、DTG and DTA revealed that the gelatin molecules had been immobilized onto PNF. The emergence of tannin structure on the adsorbed sample confirmed that tannin had been adsorbed on the surface of gelatin immobilized on PNF. The surface morphology of PNF had been changed greatly after immobilization of gelatin, gelatin filled between PP fibers and PP fibers became thicker after adsorption, its surface was covered with adsorbate. These results revealed that tannin has been adsorbed on the surface of immobilization product.
引文
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