文章摘要
四乙基氢氧化铵改性聚偏氟乙烯接枝二氧化硅油水分离膜的研制
Preparation and Characterization of Oil/Water Separation Membranes via Grafting Silica Dioxide onto Poly(vinylidene fluoride) Modified by Tetraethyl Ammonium
  
DOI:10.16865/j.cnki.1000-7555.2018.02.024
中文关键词: 油水分离膜  聚偏氟乙烯  本体改性  四乙基氢氧化铵  二氧化硅
英文关键词: oil/water separation membrane  poly (vinylidene fluoride)  bulk modification  tetraethyl ammonium hydroxide  silica dioxide
基金项目:国家自然科学基金资助项目(21463016);内蒙古自治区自然科学基金资助项目(2017MS(LH)0515);内蒙古科技大学李保卫科技创新基金(2015112);高等学校科学研究项目(NJZY18148)
作者单位
黄 强1,郭贵宝1,安胜利2,高 军1 1.内蒙古科技大学 化学与化工学院
2.内蒙古科技大学 材料与冶金学院,内蒙古 包头 014010 
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中文摘要:
      利用四乙基氢氧化铵(TEAH)和酸性高锰酸钾对聚偏氟乙烯(PVDF)粉体进行改性,得到含有羟基改性的PVDF,再将四氯化硅(SiCl4)水解后的原硅酸通过分子内脱水缩合的方法接枝到改性PVDF骨架上,通过浸没沉淀相转移法制得聚偏氟乙烯接枝二氧化硅(PVDF-g-SiO2)油水分离膜。研究了TEAH 含量对PVDF粉体接枝二氧化硅(SiO2)的接枝率和油水分离膜性能的影响,同时采用傅里叶变换红外光谱、扫描电镜-X射线能谱和视频光学接触角测量仪测试了膜的结构和表面接触角。结果表明,TEAH 使PVDF脱去部分氟化氢(HF)产生碳碳双键,双键经酸性高锰酸钾(KMnO4)氧化生成羟基,SiO2 接枝到改性的PVDF粉体,硅元素均匀地分散在分离膜中。PVDF粉体接枝SiO2 的接枝率随着TEAH 的含量增加而升高,分离膜的水通量随接枝率的升高先增加后降低。TEAH 质量分数为1.4%,分离膜的接触角降低到62.8°,膜中SiO2 的接枝率和水通量分别为6.25%、889.5L/(m2·h),截留率和水通量恢复率分别达到94.3%和90.4%,衰减率为9.6%。
英文摘要:
      Poly (vinylidene fluoride)-graft-silica dioxide(SiO2) (PVDF-g-SiO2) polymer membranes were synthesized via grafting silica dioxide onto PVDF. The PVDF was initially modified by tetraethyl ammonium hydroxide (TEAH) and H+-KMnO4 solution and generated C-OH bonds on PVDF chains. The orthosilicate produced by hydrolysis of SiCl4 was grafted onto the modified PVDF framework through the dehydration condensation method. Finally, the PVDF-g-SiO2 oil/water separation membranes were synthesized via the immersion phase inversion method. The effects of the TEAH concentration on the grafting degree of PVDF powders of SiO2, the effects of the grafting degree on water flux of oil/water separation membranes were examined. Simultaneously, the structure and performance of as-prepared were characterized by Fourier transform infrared spectroscopy, scanning electron microscopy/energy dispersive X-ray spectroscopy and filtration experiments. The results indicate that the C=C double bonds in PVDF are formed, following dehydrofluorination by TEAH. The C=C double bonds are oxidized by H+-KMnO4 solution and generated C-OH bonds. SiO2 is grafted onto the modified PVDF powders. Silicon evenly disperses in the separation membranes. The grafting degree of PVDF powders of SiO2 increases with the increasing of TEAH content. Water flux of PVDF-g-SiO2 membranes rises with the increasing of grafting degree, then it is reduced. When the content of TEAH is 1.4%(Mass fraction), the contact angle of PVDF-g-SiO2 membranes reduces to 62.8°, the largest water flux of the membranes is 889.5 L/(m2·h), the grafting degree of PVDF powders of SiO2 is 6.25%, rejection ratio and flux recovery ratio of PVDF-g-SiO2 membranes are up to 94.3% and 90.4%, respectively. The water flux attenuation rate is 9.6%.
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