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聚硅氧烷類油水分離樹(shù)脂的制備及其性能研究

發(fā)布時(shí)間:2018-05-13 03:10

  本文選題:聚甲基硅氧烷 + 疏水性; 參考:《武漢工程大學(xué)》2015年碩士論文


【摘要】:石油開(kāi)采中的溢油、含油污水的排放,都導(dǎo)致環(huán)境污染越來(lái)越嚴(yán)重,高效清潔的治理材料已成為研究熱點(diǎn)。現(xiàn)有材料制備工藝復(fù)雜、吸油倍率低、油品回收操作困難和材料可重復(fù)利用性差等缺點(diǎn)限制了它們的商業(yè)運(yùn)用。本論文針對(duì)上述問(wèn)題,研究了一種多孔且具有彈性的油水分離材料—聚甲基硅氧烷樹(shù)脂的制備。本文以醋酸為水解促進(jìn)劑,尿素為pH調(diào)節(jié)劑,十六烷基三甲基溴化銨(CTAB)為表面活性劑,將甲基三甲氧基硅烷(MTMS)和二甲基二甲氧基硅烷(DMDMS)用“一步酸堿”溶膠凝膠法,在常溫常壓下干燥制得塊狀聚甲基硅氧烷凝膠樹(shù)脂?疾炝舜姿釢舛、溶膠反應(yīng)時(shí)間、CTAB的用量、溶液總量、尿素用量、凝膠時(shí)間、凝膠溫度對(duì)聚甲基硅氧烷樹(shù)脂的吸油性能和疏水性能影響。結(jié)果表明最佳合成配方:甲基三甲氧基硅烷(質(zhì)量分?jǐn)?shù))12.719%,二甲基二甲氧基硅烷7.813%,十六烷基三甲基溴化銨1.776%,5mmol/L醋酸66.593%、尿素11.099%。最佳工藝條件:常溫水解時(shí)間1 h,凝膠溫度80℃,凝膠時(shí)間9 h。最佳工藝操作順序:將十六烷基三甲基溴化銨和尿素添加在醋酸溶液中,在劇烈攪拌的同時(shí)在反應(yīng)器兩側(cè)分別滴加甲基三甲氧基硅烷和二甲基二甲氧基硅烷。滴畢后在常溫下反應(yīng)60 min,將所得溶液轉(zhuǎn)移至強(qiáng)制對(duì)流烘箱,在80℃的條件下反應(yīng)9 h。在此條件下制備得到的樹(shù)脂接觸角高達(dá)140°,具有高疏水性,吸油倍率最大,在幾秒內(nèi)吸收自身重量的6.24倍的正己烷,擠壓材料使材料體積降至20%時(shí),解吸出自身重量5.06倍的正己烷。重復(fù)利用樹(shù)脂吸收/解吸正己烷,發(fā)現(xiàn)其吸油倍率在3次循環(huán)利用后降至6.18 g/g,5次循環(huán)利用后降至6.09 g/g,之后基本穩(wěn)定在6.00 g/g。對(duì)其他油和有機(jī)溶液的吸附能力根據(jù)待吸收溶液的密度和粘度不同各有變化。采用掃描電子顯微鏡(SEM)、熱重差熱分析(TG/DTA)、紅外光譜(IR)、BET比表面積、能譜分析(EDS)等手段分別對(duì)樹(shù)脂的表面形貌、熱穩(wěn)定性、化學(xué)成分、比表面積進(jìn)行了分析和表征。結(jié)果表明樹(shù)脂的內(nèi)部有大量的大孔結(jié)構(gòu);樹(shù)脂的熱解溫度高達(dá)320℃;產(chǎn)物含有Si-O-Si、Si-CH3、CH3-Si-CH3、C-Si-O鍵,不含有-OH,Si-O-CH3鍵,說(shuō)明前體反應(yīng)完全;樹(shù)脂中不含N,說(shuō)明尿素和表面活性劑沒(méi)有殘留;BET比表面積為1.5 m2/g;密度為0.13 g/cm3。本課題研制的聚甲基硅氧烷樹(shù)脂具有密度比水小、油水選擇性高、吸油速率快、吸油倍率高、制備過(guò)程簡(jiǎn)單等特點(diǎn),為聚甲基硅氧烷樹(shù)脂的工業(yè)化生產(chǎn)及應(yīng)用奠定了理論基礎(chǔ)。
[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,

本文編號(hào):1881382

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