本文選題：微波輔助 + 反相乳液聚合　； 參考：《太原理工大學(xué)》2017年碩士論文

【摘要】：鎘是一種具有致癌、致畸的有毒重金屬,可以對環(huán)境和人體造成嚴(yán)重的危害。離子印跡聚合物具有高選擇性、良好的穩(wěn)定性、良好的循環(huán)使用能力及應(yīng)用范圍廣等優(yōu)點,作為一種新型的吸附材料可以被用來分離和去除水中的重金屬離子。制備印跡聚合物過程中采用微波輔助法可以縮短聚合時間,加快反應(yīng)的進行。本文通過微波輔助兩種聚合方法、選擇不同的功能單體分別制備了兩種不同的鎘離子印跡聚合物并用于水中鎘離子的吸附和固相萃取。以β-環(huán)糊精和丙烯酰胺作為功能單體、環(huán)氧氯丙烷作為交聯(lián)劑、過硫酸銨作為引發(fā)劑通過微波輔助反相乳液聚合法制備鎘離子印跡聚合物(IEIIP)。用SEM、FTIR和TG對IEIIP進行結(jié)構(gòu)表征。研究了Cd(Ⅱ)的初始濃度、溶液p H值、反應(yīng)溫度、時間和競爭離子對IEIIP吸附量的影響。在最佳吸附條件下,IEIIP的吸附量達到107mg/g。非印跡聚合物的吸附量比印跡聚合物的吸附量小52.4mg/g。選擇性研究表明,IEIIP對Cd~(2+)/Pb~(2+)、Cd~(2+)/Cu~(2+)和Cd~(2+)/Zn~(2+)的選擇性系數(shù)分別為2.7624、3.8154和1.1500。而IENIP的選擇性系數(shù)k分別為0.4521、0.5024和0.3747,說明IEIIP對溶液中的鎘離子有較好的選擇性。此外,用準(zhǔn)一級、準(zhǔn)二級動力學(xué)模型和顆粒內(nèi)擴散模型描述IEIIP對鎘的吸附動力學(xué)行為。結(jié)果表明準(zhǔn)二級動力學(xué)方程能很好地描述IEIIP的吸附行為。Langmuir等溫線模型符合IEIIP對溶液中Cd(Ⅱ)的吸附行為,表明吸附過程是以單層吸附為主。Scatchard分析得到的離解常數(shù)KD和最大表觀結(jié)合能力Qmax分別為72.99mg/L和130mg/g,說明IEIIP對Cd(Ⅱ)的吸附位點是等價的。熱力學(xué)參數(shù)ΔG00、ΔH00和ΔS00表明吸附過程是自發(fā)的、吸熱的。采用IEIIP作為固相萃取吸附劑,研究了洗脫液濃度、Cd(Ⅱ)初始濃度、p H值和競爭離子對萃取效率的影響,并對IEIIP固相萃取柱的重復(fù)性和精密度進行檢驗。結(jié)果表明,洗脫液甲醇:乙酸為7:1時富集效果最好,Cd(Ⅱ)的濃度為10μg/L,溶液p H值為7時萃取效率最高。IEIIP固相萃取柱在重復(fù)使用5次后萃取效率在70%以上。IEIIP固相萃取柱對離子混合溶液中Cd(Ⅱ)的萃取效率要高于其他競爭離子,這是因為IEIIP具有良好的選擇性。通過IEIIP固相萃取柱平行分析11次標(biāo)準(zhǔn)溶液來檢驗方法的精密度,相對標(biāo)準(zhǔn)偏差(RSD)為2.699%,檢出限3σ為0.8094μg/L(n=11)。對實際廢水樣本中Cd(Ⅱ)的加標(biāo)回收率在93.58%到101%之間。以席夫堿作為功能單體、EGDMA作為交聯(lián)劑、AIBN作為引發(fā)劑通過微波輔助反相乳液-懸浮聚合制備了鎘離子印跡聚合物(IESIIP)。采用SEM、FTIR對IESIIP進行結(jié)構(gòu)表征。通過靜態(tài)吸附實驗和競爭吸附實驗研究IESIIP對溶液中Cd(Ⅱ)的吸附能力,研究了不同的影響因素包括Cd(Ⅱ)的初始濃度、溶液p H值、溫度、時間和競爭離子對IESIIP吸附效果的影響。在最佳吸附條件下,IESIIP的吸附量為179.04mg/g。Cd~(2+)/Pb~(2+)、Cd~(2+)/Cu~(2+)和Cd~(2+)/Zn~(2+)的相對選擇性系數(shù)k'分別為2.1061、4.7306和4.5602表明IESIIP對鎘的選擇性要遠大于IESNIP的選擇性。IESIIP的吸附過程符合準(zhǔn)二級動力學(xué)方程和Langmuir等溫線模型(R20.99)。Scatchard模型計算得到IESIIP上兩類結(jié)合位點的離解常數(shù)KD分別為16.89mg/L和39.84mg/L,最大表觀吸附量Qmax分別為105.15mg/g和171.84mg/g。熱力學(xué)參數(shù)表明吸附可以自發(fā)進行,并且是吸熱過程。IESIIP作為固相萃取柱填料時研究洗脫劑濃度、Cd(Ⅱ)初始濃度、p H值和競爭離子對萃取效率的影響。并評價固相萃取柱的穩(wěn)定性和精密度。結(jié)果表明最佳的洗脫條件為0.5mol/L鹽酸,萃取效率隨著Cd(Ⅱ)濃度的增大而減小,最佳的p H條件為7。該固相萃取柱經(jīng)5次重復(fù)使用后萃取效率僅僅下降了9.9%,說明該萃取柱具有良好的重復(fù)使用能力。將含有競爭離子的溶液通過固相萃取柱時,IESIIP對Cd(Ⅱ)的萃取效率明顯高于其他的競爭離子。該方法的相對標(biāo)準(zhǔn)偏差(RSD)為2.699%,檢出限3σ為0.288μg/L(n=11)。在最佳固相萃取條件下,對實際廢水樣本中Cd(Ⅱ)的加標(biāo)回收率為95.22%-104%。
[Abstract]:Cadmium is a toxic heavy metal which is carcinogenic and teratogenic. It can cause serious harm to the environment and human body. The ion imprinted polymer has the advantages of high selectivity, good stability, good recycling ability and wide application. As a new type of adsorption material, it can be used to separate and remove heavy metal ions in water. In the process of preparing imprinted polymer, microwave assisted method can shorten the polymerization time and accelerate the reaction. In this paper, two different cadmium ion imprinted polymers were prepared by microwave assisted two polymerization methods and used to adsorb cadmium ion and solid phase extraction in water. Amine is used as a functional monomer, epichlorohydrin as a crosslinker and ammonium persulfate as an initiator to prepare cadmium ion imprinted polymer (IEIIP) by microwave assisted reverse phase emulsion polymerization. The structure of IEIIP is characterized by SEM, FTIR and TG. The initial concentration of Cd (II), the solution P H value, reaction temperature, time and competitive ions to IEIIP adsorption amount are studied. Under the optimal adsorption conditions, the adsorption capacity of IEIIP is less than that of the imprinted polymer, which is smaller than that of the imprinted polymer. The selective coefficient of the IEIIP to Cd~ (2+) /Pb~ (2+), Cd~ (2+) /Cu~ (2+) and IEIIP is respectively the selectivity coefficient respectively. For 0.4521,0.5024 and 0.3747, it is shown that IEIIP has good selectivity for cadmium ions in the solution. In addition, the adsorption kinetics of cadmium by IEIIP is described by quasi first order, quasi two kinetics model and internal particle diffusion model. The results show that the quasi two order kinetic equation can describe the adsorption behavior of IEIIP with.Langmuir isotherm model conforming to IE well. The adsorption behavior of IIP on Cd (II) in the solution shows that the adsorption process is KD and the maximum apparent binding capacity Qmax of the single layer adsorption.Scatchard analysis 72.99mg/L and 130mg/g respectively. It shows that the adsorption site of IEIIP to Cd (II) is equivalent. The thermodynamic parameter delta G00, Delta H00 and Delta S00 indicate that the adsorption process is spontaneous and endothermic. Using IEIIP as solid phase extraction adsorbent, the effect of eluent concentration, initial concentration of Cd (II), P H value and competitive ion on the extraction efficiency were studied, and the repeatability and precision of IEIIP solid phase extraction column were tested. The results showed that the enrichment effect was best when the eluent was methanol: acetic acid was 7:1, the concentration of Cd (II) was 10 u g/L, and the P H value of the solution. The extraction efficiency of the.IEIIP solid extraction column at 7 time is highest. The extraction efficiency of Cd (II) in the mixed solution of.IEIIP solid extraction column is higher than that of other competitive ions in the mixed solution of 70%.IEIIP after repeated use. This is due to the good selectivity of the IEIIP solid extraction column. The method of parallel analysis of the IEIIP solid phase extraction column for the test of the standard solution The precision, the relative standard deviation (RSD) was 2.699%, the detection limit was 3 Sigma 0.8094 g/L (n=11). The recovery rate of Cd (II) in the actual wastewater samples was between 93.58% and 101%. The Schiff base was used as a functional monomer, EGDMA as a crosslinker, and AIBN was used as a initiator to prepare the cadmium imprinted polymer by microwave assisted reverse phase emulsion suspension polymerization. IESIIP). The structure of IESIIP was characterized by SEM and FTIR. The adsorption capacity of Cd (II) in the solution by IESIIP was studied by static adsorption and competitive adsorption. The influence factors including the initial concentration of Cd (II), the H value of P, temperature, time and the effect of competing ions on the adsorption of IESIIP were studied. Under the optimal adsorption conditions, I The adsorption capacity of ESIIP is 179.04mg/g.Cd~ (2+) /Pb~ (2+), Cd~ (2+) /Cu~ (2+) and Cd~ (2+) /Zn~. The dissociation constant KD of the two binding sites on the IESIIP is 16.89mg/L and 39.84mg/L respectively. The maximum apparent adsorption capacity Qmax is 105.15mg/g and 171.84mg/g. thermodynamics parameters show that adsorption can be carried out spontaneously, and it is the concentration of eluent, Cd (II) initial concentration and P H value when.IESIIP is used as solid phase extraction column for the endothermic process. And the influence of the competitive ion on the extraction efficiency and evaluation of the stability and precision of the solid phase extraction column. The results show that the best elution condition is 0.5mol/L hydrochloric acid, the extraction efficiency decreases with the increase of Cd (II) concentration, the best p H condition is 7., the extraction efficiency of the solid phase extraction column is only 9.9% after the extraction, indicating that the extraction efficiency is only 9.9%. The extraction efficiency of IESIIP for Cd (II) was significantly higher than that of other competitive ions. The relative standard deviation (RSD) of the method was 2.699% and the detection limit was 3 Sigma 0.288 g/L (n=11). Under the optimum solid-phase extraction conditions, Cd (II) in the actual wastewater samples. The recovery rate of the added standard is 95.22%-104%.
【學(xué)位授予單位】：太原理工大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：O631.3;X703

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