負(fù)載ZnO復(fù)合納米纖維膜的制備及其光催化性能研究
發(fā)布時(shí)間:2018-07-11 12:12
本文選題:靜電紡絲 + 聚丙烯腈。 參考:《浙江理工大學(xué)》2017年碩士論文
【摘要】:本文以聚丙烯腈(PAN)與氯化鋅(ZnCl_2)作為前驅(qū)物,采用靜電紡絲工藝和溶液浸漬法相結(jié)合的方法,制備出了復(fù)合納米纖維膜R-11/1、R-7/1、R-5/1、和S-5/1。以亞甲基藍(lán)為污染物模型,評(píng)價(jià)其光催化降解性能,研究了紡絲液配比與不同的溶液浸漬方法對(duì)復(fù)合納米纖維膜結(jié)構(gòu)以及光催化性能的影響。將復(fù)合納米纖維膜進(jìn)行預(yù)氧化、碳化處理,提高其光催化降解性能。(1)以DMF作為溶劑,用聚丙烯腈配得紡絲液,得到了最優(yōu)的靜電紡絲工藝參數(shù):紡絲液濃度12wt%、電壓18kV、紡絲速率為0.7mL/h。采用靜電紡絲和溶液浸漬法制備出了復(fù)合納米纖維膜R-11/1、R-7/1、R-5/1、和S-5/1,其中R表示采用多次冷熱交替浸漬法,S表示采用單次冷熱靜置浸漬法。利用掃描電鏡(SEM)、傅里葉紅外光譜(FT-IR)、X-射線衍射(XRD)、X-射線能量色散光譜(XPS)和熱重分析(TG)對(duì)復(fù)合納米纖維膜的表面形貌和微結(jié)構(gòu)進(jìn)行了表征,研究了不同的紡絲液配比和溶液浸漬法對(duì)復(fù)合納米纖維膜性能的影響。結(jié)果表明:當(dāng)PAN(g)/ZnCl_2(g)=7/1時(shí),通過多次冷熱浸漬法處理的復(fù)合納米纖維膜ZnO含量較高,結(jié)晶性能較好。通過比較樣品R-5/1與S-5/1可知,多次冷熱浸漬法要比單次冷熱靜置法更有利于ZnO粒子負(fù)載在納米纖維上。(2)以亞甲藍(lán)溶液為污染物模型,研究了紡絲液配比和不同的溶液浸漬方法對(duì)復(fù)合納米纖維膜光催化性能的影響。研究表明當(dāng)PAN(g)/ZnCl_2(g)=7/1時(shí),降解性能最優(yōu);多次冷熱交替浸漬法比單次冷熱靜置浸漬法更容易使ZnO粒子負(fù)載在納米纖維上。對(duì)樣品R-7/1與S-5/1進(jìn)行3次循環(huán)使用的光催化降解試驗(yàn),證明了復(fù)合納米纖維膜可以回收進(jìn)行多次重復(fù)利用,具有很好的光催化性能穩(wěn)定性。其次研究了影響光催化性能的因素,結(jié)果表明,MB溶液初始濃度越小,催化劑用量越多,染料溶液呈堿性時(shí)復(fù)合納米纖維膜催化效率越高。(3)研究了預(yù)氧化時(shí)間和溫度、碳化溫度對(duì)PAN/ZnO復(fù)合納米纖維膜形貌的影響,確定了最優(yōu)的碳化工藝:預(yù)氧化時(shí)間60 min、預(yù)氧化溫度200℃、碳化溫度1000℃。按照最優(yōu)碳化工藝對(duì)復(fù)合納米纖維膜PAN/ZnO進(jìn)行處理,發(fā)現(xiàn)樣品R-11/1與R-7/1纖維直徑減小,但表面ZnO粒子脫落嚴(yán)重;而樣品R-5/1與S-5/1纖維直徑?jīng)]有比較明顯的變化,且表面負(fù)載的ZnO粒子脫落較少。經(jīng)過碳化工藝處理后的復(fù)合納米纖維膜光催化性能均得到一定程度的改善。
[Abstract]:In this paper, using polyacrylonitrile (pan) and zinc chloride (ZnCl2) as precursors, the composite nanofiber membranes R-11 / 1 / 7 / 1 / 1 R-5 / 1 and S-5 / 1 were prepared by using electrospinning process and solution impregnation method. The photocatalytic degradation of methylene blue was evaluated using methylene blue as a pollutant model. The effects of spinning solution ratio and different solution impregnation methods on the structure and photocatalytic properties of composite nanofibers were studied. The composite nanofiber membrane was preoxidized and carbonized to improve its photocatalytic degradation. (1) the spinning solution was prepared with polyacrylonitrile (pan) and DMF as solvent. The optimum parameters of electrostatic spinning were obtained: spinning solution concentration 12 wts, voltage 18kV, spinning rate 0.7mL / h. Composite nanofiber membranes R-11 / 1 / 7 / 7 R-5 / 1 and S-5 / 1 were prepared by electrospinning and solution impregnation. The surface morphology and microstructure of composite nanofibers were characterized by scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) X-ray diffraction (XRD), X-ray energy dispersive spectroscopy (XPS) and thermogravimetric analysis (TG). The effects of different ratio of spinning solution and solution impregnation on the properties of composite nanofibers were studied. The results show that when pan / ZnCl _ 2 (g) / 7 / 1, the content of ZnO is higher and the crystallinity is better. By comparing R-5 / 1 with S-5 / 1, we can see that the multiple cold and hot impregnation method is more favorable than the single cold and hot static method to the ZnO particle loading on the nanofibers. (2) the methylene blue solution is used as the pollutant model. The effects of spinning solution ratio and different solution impregnation methods on the photocatalytic properties of composite nanofibers were studied. The results show that when pan / ZnCl _ 2 (g) / 7 / 1, the degradation performance is the best, and the alternative cold and hot impregnation is easier than the single cold and thermal static impregnation to make the particles loaded on the nanofibers. The photocatalytic degradation tests of R-7 / 1 and S-5 / 1 were carried out for three times. It was proved that the composite nanofiber membrane could be recycled for many times and had good photocatalytic stability. Secondly, the factors influencing the photocatalytic performance were studied. The results showed that the lower the initial concentration of MB solution, the more the amount of catalyst was, the higher the catalytic efficiency of composite nanofiber membrane was when the dye solution was alkaline. (3) the pre-oxidation time and temperature were studied. The effect of carbonization temperature on the morphology of pan / ZnO composite nanofiber film was studied. The optimum carbonization process was determined as follows: preoxidation time 60 min, preoxidation temperature 200 鈩,
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