【摘要】：滲透蒸發(fā)是一種高效節(jié)能的膜分離技術(shù),尤其對于有機物中少量水的脫除或恒沸物體系及近沸物體系分離,與傳統(tǒng)精餾、吸附、萃取等分離技術(shù)相比優(yōu)勢明顯。強親水性的NaA沸石膜在有機物脫水方面表現(xiàn)出優(yōu)異的滲透蒸發(fā)性能,已經(jīng)被市場化應(yīng)用,但其弱的耐酸性限制了其應(yīng)用范圍。T型沸石膜親水性稍弱于NaA沸石膜,但耐酸性較好,在一定強度酸性環(huán)境中具有良好的滲透蒸發(fā)性能,探索高性能T型沸石膜的成熟制備工藝,進而工業(yè)化應(yīng)用具有重要意義。本文面向T型沸石膜的實際應(yīng)用,以多孔粗糙的廉價氧化鋁管為載體,制備了高性能T型沸石膜,進行了實驗室規(guī)模放大制備,探究了其在有機物脫水方面滲透蒸發(fā)性能,主要工作內(nèi)容如下：(1)以模板劑配方1 SiO2:0.055Al2O3:0.23Na2O:0.0825K2O:xTMAOH:11.68H2O(x=0.045或0.1)水熱合成了2gm和0.4μm兩種尺寸的結(jié)晶度高、粒徑分布均勻的T型沸石分子篩；采用大小品種匹配-變溫熱浸漬法在粗糙的大孔廉價載體表面引入高質(zhì)量晶種層,在摩爾配比為1 SiO2:0.055Al2O3:0.23Na2O:0.08K2O:30H2O的凝膠體系中水熱法合成T型沸石膜,考察了晶化溫度和晶化時間對膜的形貌及性能的影響,結(jié)果表明：晶化溫度150℃晶化4h為較理想的合成條件,合成的T型沸石膜在75℃分離90wt.%異丙醇/10wt.%水,滲透通量為2.84 kg-m-2.h-1,分離系數(shù)為1766。(2)理想條件合成的T型沸石膜對各種90wt.%有機溶劑/10wt.%水體系具有良好的滲透蒸發(fā)分離性能；酸浸泡試驗表明高濃度的酸對T型沸石膜有較強腐蝕作用；對pH=4的90wt.%異丙醇/10wt.%水體系進行長時間(120h)滲透蒸發(fā)測試表明滲透通量大于1.00kg.m-2.h-1,分離系數(shù)變化不大,說明T性沸石膜具有一定耐酸穩(wěn)定性。(3)基于長為80cm的載體管進行了T型沸石膜放大制備,從晶化時間、晶化溫度及晶化方式等進行條件優(yōu)化,表明晶化溫度為170℃晶化時間為6h旋轉(zhuǎn)晶化為最佳成膜條件,放大制備的T型沸石膜滲透通量大于1.50 kg·m-2.h-1,分離系數(shù)大于10000；T型沸石膜滲透蒸發(fā)中試測試結(jié)果表明操作條件(進料溫度、進料流量、進料組成)對膜的滲透蒸發(fā)性能均有不同程度的影響,高溫連續(xù)滲透蒸發(fā)將異丙醇料液含水量由10%降至0.5%,平均滲透通量為1.90 kg·m-2·h-1,分離系數(shù)大于3000。
[Abstract]:Osmotic evaporation is an efficient and energy saving membrane separation technology, especially for the removal of a small amount of water from organic matter or the separation of azeotrope system and near-boiling system, which is superior to the traditional separation techniques such as distillation, adsorption, extraction and so on. The strong hydrophilic NaA zeolite membrane has shown excellent pervaporation performance in organic dehydration and has been marketed, but its weak acid resistance limits its application scope. The hydrophilicity of T-type zeolite membrane is slightly weaker than that of NaA zeolite membrane. But the acid resistance is good, and it has good pervaporation performance in a certain strong acidic environment. It is of great significance to explore the mature preparation process of high performance T-type zeolite membrane and then to apply it to industry. For the practical application of T zeolite membrane, high performance T zeolite membrane was prepared with porous and rough cheap alumina tube as the carrier. The laboratory scale was enlarged to investigate its pervaporation performance in the dehydration of organic matter. The main contents are as follows: (1) 2gm and 0.4 渭 m were synthesized by hydrothermal synthesis of 2gm and 0.4 渭 m with the template formulation 1 SiO2:0.055Al2O3:0.23Na2O:0.0825K2O:xTMAOH:11.68H2O (x0. 045 or 0. 1). T-type zeolite with uniform particle size distribution; T zeolite membrane was synthesized by hydrothermal method in gel system with 1 SiO2:0.055Al2O3:0.23Na2O:0.08K2O:30H2O molar ratio by introducing high quality seed layer on the rough surface of macroporous cheap carrier by varietal matching and variable temperature hot impregnation. The effects of crystallization temperature and crystallization time on the morphology and properties of the films were investigated. The results showed that crystallization temperature at 150 鈩，

本文編號：2405578