微乳液模板法制備色氨酸分子印跡膜及其性能研究
發(fā)布時(shí)間:2018-07-10 12:26
本文選題:分子印跡膜 + 微乳液聚合; 參考:《福州大學(xué)》2011年碩士論文
【摘要】:本文將微乳液聚合和分子印跡技術(shù)相結(jié)合,提出微乳液模板法制備分子印跡膜(MIM)的新方法。采用L-色氨酸(L-trp)為模板分子,以雙連續(xù)相微乳液為孔穴模板,并在較低溫下引發(fā)聚合制備MIM?疾炝擞绊慚IM選擇吸附性能和膜孔結(jié)構(gòu)的因素,研究MIM的膜孔形態(tài)及分離過程識(shí)別機(jī)理。 對(duì)微乳液擬三元相圖和電導(dǎo)率研究,發(fā)現(xiàn)L-trp和丙烯酰胺(AM)對(duì)體系具有助乳化效果,且L-trp有助于雙連續(xù)相微乳液的形成。油相單體中MMA/BA的比對(duì)反相微乳液區(qū)影響較大。確定微乳液印跡體系為MMA-BA/AA/H2O/L-trp,體系通過KPS/TMEDA氧化還原引發(fā)劑引發(fā)聚合成膜,考察了影響MIM的選擇吸附性能和膜孔結(jié)構(gòu)的因素。結(jié)果表明,交聯(lián)劑EGDMA的加入,能維持MIM的印跡孔穴形態(tài)和膜孔結(jié)構(gòu)的穩(wěn)定性。隨著微乳液印跡體系中水相分率的提高,MIM的吸附量Q和水通量F增加,但水相分率過高容易引起聚合過程發(fā)生的微觀相分離,導(dǎo)致MIM中的印跡層和膜孔結(jié)構(gòu)的破壞。AA與MIM結(jié)合位點(diǎn)和膜孔大小密切相關(guān),AA含量過多會(huì)降低選擇吸附性能和水通量,AA/MMA-BA比控制在2.5,既能維持微乳液聚合的穩(wěn)定性,同時(shí)又能確保MIM較好的性能。MMA能夠維持印跡孔穴的剛性結(jié)構(gòu),但MMA含量過多則會(huì)影響孔穴的空間構(gòu)型。隨著L-trp增加,MIM的水通量F提高,但過量L-trp使印跡位點(diǎn)的利用率下降,選擇吸附性能相應(yīng)下降。所以,當(dāng)EGDMA的含量在2.0%,水相分率為40%,AA/MMA-BA為2.5,MMA/BA為2.0,L-trp含量為0.9%時(shí),,分離因子α和水通量F較大,表現(xiàn)為較佳的選擇識(shí)別性能和膜孔結(jié)構(gòu)。 通過SEM觀察,MIM的孔道維持了雙連續(xù)相的海綿狀孔道結(jié)構(gòu)。MIM的膜孔徑和對(duì)L-trp的滲透量隨著水相分率的提高都增大。MIM對(duì)L-trp吸附在120min內(nèi)可達(dá)到吸附平衡,結(jié)合MIM滲透過程和紅外譜圖分析,發(fā)現(xiàn)L-trp與MIM中的結(jié)合位點(diǎn)存在氫鍵作用,且MIM對(duì)L-trp的滲透是一個(gè)優(yōu)先吸附并逐步透過的過程。MIM耐酸性能較好,但耐堿性較差,在堿溶液中發(fā)生不可逆溶脹。熱重結(jié)果表明MIM具有較好的熱穩(wěn)定性。MIM在20~50℃的熱處理會(huì)引起膜的致密,滲透性能降低;但溫度達(dá)60℃則會(huì)引起膜孔結(jié)構(gòu)的破壞。
[Abstract]:In this paper, a new method of preparing MIM by microemulsion template was proposed by combining microemulsion polymerization with molecular imprinting. Using L-Tryptophan (L-trp) as template molecule and double continuous microemulsion as pore template, Mims were prepared by polymerization at low temperature. The factors affecting the selective adsorption properties and membrane pore structure of MIM were investigated, and the membrane pore morphology and separation process identification mechanism of MIM were studied. The pseudo-ternary phase diagram and electrical conductivity of microemulsion were studied. It was found that L-trp and acrylamide (AM) could help emulsify the microemulsion, and L-trp was helpful to the formation of double-continuous microemulsion. The ratio of MMA / BA in oil phase monomer has a great influence on the area of inverse microemulsion. The microemulsion imprinting system was determined as MMA-BA / A / H _ 2O / H _ 2O _ L-trp.The system was polymerized by KPS / TMEDA redox initiator. The factors affecting the selective adsorption properties and pore structure of MIM were investigated. The results showed that the addition of crosslinking agent EGDMA could maintain the stability of MIM imprinted pore morphology and membrane structure. With the increase of water phase separation rate in microemulsion imprinted system, the adsorption capacity Q and water flux F of MIM increase, but the high water phase separation rate easily leads to the microphase separation in the polymerization process. As a result of the destruction of the imprinted layer and membrane pore structure in MIM. AA is closely related to MIM binding sites and membrane pore size. Excessive AA content will reduce the selective adsorption performance and the water flux ratio of AA / MMA-BA to 2.5, which can maintain the stability of microemulsion polymerization. At the same time, it can ensure the better performance of MIM. MMA can maintain the rigid structure of imprinted pores, but too much MMA content will affect the spatial configuration of the pores. With the increase of L-trp, the water flux F of MIM increased, but excessive L-trp decreased the utilization of imprinted sites and the selective adsorption ability. Therefore, when the content of EGDMA is 2.0 and the water phase separation rate is 40. 5% MMA-BA is 2.5% MMA / BA is 2.0% L-trp content is 0.9, the separation factor 偽 and water flux F are larger, showing better selective recognition performance and membrane pore structure. It was observed by SEM that the membrane pore size and the permeability to L-trp increased with the increase of water phase separation. The adsorption equilibrium of L-trp adsorbed in 120min was achieved. Combined with MIM osmotic process and IR spectrum analysis, it was found that the binding sites of L-trp and MIM had hydrogen bond interaction, and the permeation of L-trp by MIM was a preferential adsorption and gradual permeation process. MIM had good acid resistance, but poor alkali resistance. Irreversible swelling occurs in alkali solution. The thermogravimetric results show that MIM has good thermal stability. The heat treatment of MIM at 20 ~ 50 鈩
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