聚硅氧烷类油水分离树脂的制备及其性能研究

发布时间：2018-05-13 03:10

  本文选题：聚甲基硅氧烷 + 疏水性　； 参考：《武汉工程大学》2015年硕士论文

【摘要】：石油开采中的溢油、含油污水的排放,都导致环境污染越来越严重,高效清洁的治理材料已成为研究热点。现有材料制备工艺复杂、吸油倍率低、油品回收操作困难和材料可重复利用性差等缺点限制了它们的商业运用。本论文针对上述问题,研究了一种多孔且具有弹性的油水分离材料—聚甲基硅氧烷树脂的制备。本文以醋酸为水解促进剂,尿素为pH调节剂,十六烷基三甲基溴化铵(CTAB)为表面活性剂,将甲基三甲氧基硅烷(MTMS)和二甲基二甲氧基硅烷(DMDMS)用“一步酸碱”溶胶凝胶法,在常温常压下干燥制得块状聚甲基硅氧烷凝胶树脂。考察了醋酸浓度、溶胶反应时间、CTAB的用量、溶液总量、尿素用量、凝胶时间、凝胶温度对聚甲基硅氧烷树脂的吸油性能和疏水性能影响。结果表明最佳合成配方:甲基三甲氧基硅烷(质量分数)12.719%,二甲基二甲氧基硅烷7.813%,十六烷基三甲基溴化铵1.776%,5mmol/L醋酸66.593%、尿素11.099%。最佳工艺条件:常温水解时间1 h,凝胶温度80℃,凝胶时间9 h。最佳工艺操作顺序:将十六烷基三甲基溴化铵和尿素添加在醋酸溶液中,在剧烈搅拌的同时在反应器两侧分别滴加甲基三甲氧基硅烷和二甲基二甲氧基硅烷。滴毕后在常温下反应60 min,将所得溶液转移至强制对流烘箱,在80℃的条件下反应9 h。在此条件下制备得到的树脂接触角高达140°,具有高疏水性,吸油倍率最大,在几秒内吸收自身重量的6.24倍的正己烷,挤压材料使材料体积降至20%时,解吸出自身重量5.06倍的正己烷。重复利用树脂吸收/解吸正己烷,发现其吸油倍率在3次循环利用后降至6.18 g/g,5次循环利用后降至6.09 g/g,之后基本稳定在6.00 g/g。对其他油和有机溶液的吸附能力根据待吸收溶液的密度和粘度不同各有变化。采用扫描电子显微镜(SEM)、热重差热分析(TG/DTA)、红外光谱(IR)、BET比表面积、能谱分析(EDS)等手段分别对树脂的表面形貌、热稳定性、化学成分、比表面积进行了分析和表征。结果表明树脂的内部有大量的大孔结构;树脂的热解温度高达320℃;产物含有Si-O-Si、Si-CH3、CH3-Si-CH3、C-Si-O键,不含有-OH,Si-O-CH3键,说明前体反应完全;树脂中不含N,说明尿素和表面活性剂没有残留;BET比表面积为1.5 m2/g;密度为0.13 g/cm3。本课题研制的聚甲基硅氧烷树脂具有密度比水小、油水选择性高、吸油速率快、吸油倍率高、制备过程简单等特点,为聚甲基硅氧烷树脂的工业化生产及应用奠定了理论基础。
[Abstract]:The oil spills and the discharge of oily sewage in petroleum exploitation cause more and more serious environmental pollution, and efficient and clean treatment materials have become the research hotspot. Their commercial applications are limited by the complex preparation process, low oil absorption ratio, difficult oil recovery operation and poor reusability of materials. In order to solve the above problems, the preparation of polymethylsiloxane resin, a porous and elastic oil and water separation material, was studied in this paper. In this paper, using acetic acid as hydrolysis promoter, urea as pH regulator, cetyltrimethylammonium bromide (CTAB) as surfactant, methyl trimethoxysilane (MTMS) and dimethyl dimethoxysilane (DMDMS) were prepared by one-step acid-base sol-gel method. Bulk polymethylsiloxane gel resin was prepared by drying at room temperature and atmospheric pressure. The effects of acetic acid concentration, sol reaction time, the amount of CTAB, the total amount of solution, the amount of urea, gel time and gel temperature on the oil absorption and hydrophobicity of polymethylsiloxane resin were investigated. The results showed that the optimum synthetic formula was methyl trimethoxysilane (12.719 by mass fraction, dimethyl dimethoxysilane 7.813), cetyltrimethylammonium bromide 1.776 and 5mmol / L acetic acid 66.593and urea 11.09999. The optimum conditions were as follows: hydrolysis time at room temperature 1 h, gel temperature 80 鈩，

本文编号：1881382