本文關(guān)鍵詞： 磁性材料 雙酚A 多環(huán)芳烴 重金屬離子 檢測　出處：《中國人民解放軍軍事醫(yī)學科學院》2015年碩士論文　論文類型：學位論文

【摘要】：環(huán)境污染物種類繁多,對人類健康及生態(tài)環(huán)境造成了嚴重的威脅。因此建立環(huán)境污染物檢測技術(shù),對于環(huán)境污染風險防控、保護人類健康及生態(tài)環(huán)境有著重要的意義。由于環(huán)境樣品復雜多樣、環(huán)境污染物檢測項目千差萬別,樣品前處理技術(shù)一直是環(huán)境污染物檢測技術(shù)建立和發(fā)展的關(guān)鍵環(huán)節(jié)之一。功能化磁性材料作為一種新型的SPE材料,具有快速磁響應性、高度生物相容性、易于表面功能化修飾等一系列優(yōu)點,在快速高效富集蛋白、細菌、核酸、病毒等特定目標物等方面均顯示了良好的應用前景。因此,將功能化磁性材料應用于環(huán)境污染物的檢測技術(shù)研究中,對環(huán)境中相關(guān)污染物分析技術(shù)的完善、保護人類健康有重要的意義。1.功能化磁性材料的制備與表征(1)納米四氧化三鐵(Fe3O4)磁性內(nèi)核的制備與表征；(2)二氧化硅磁性微球(Fe3O4@TEOS)的制備與表征；(3)聚酰胺66(PA66)功能化磁性材料的制備與表征；(4)氨基功能化磁性材料(Fe3O4@TEOS@APTES)的制備與表征。2.PA66功能化磁性材料在雙酚A(BPA)檢測中的應用(1)PA66功能化磁性材料對BPA富集條件的優(yōu)化；(2)基于PA66功能化磁性材料的BPA檢測方法的建立；(3)實際樣品檢測。3. Fe3O4@TEOS@APTES在幾種典型環(huán)境污染物檢測中的初步應用(1) Fe3O4@TEOS@APTES對16種多環(huán)芳烴類(PAHs)污染物的吸附效果研究；(2) Fe3O4@TEOS@APTE S對重金屬離子Pb、Cd的吸附效果研究。1.功能化磁性材料的制備及表征(1)納米Fe3O4磁性內(nèi)核的制備及表征：在傳統(tǒng)化學共沉淀法基礎(chǔ)上,通過調(diào)整反應的堿性體系、三價鐵和二價鐵比例,結(jié)合脫氧、陳化等技術(shù)對Fe3O4的制備過程進行優(yōu)化,并以TEM、XRD對合成的Fe3O4進行表征；(2) Fe3O4@TEOS的制備及表征：利用富含硅氧鍵的TEOS對磁性Fe3O4內(nèi)核進行修飾,并以TEM、XRD3寸合成的]Fe3O4@TEOS進行表征；(3)PA66功能化磁性材料的制備及表征：利用反相無水微乳液合成的新方法,完成難溶于水和一般有機相材料在固相親水性磁性微球表面的修飾,并以TEM、FT-IR對合成的PA66功能化磁性材料進行表征；(4)Fe3O4@TEOS@APTES的制備及表征：利用APTES對制備的Fe3O4@TEOS表面進行修飾,并以TEM、XRD、FT-IR對合成的Fe3O4@TEOS@APTES進行表征。2.PA66功能化磁性材料在BPA檢測中的應用(1)探討PA66功能化磁性材料制備過程中相關(guān)影響因素對BPA的預處理效果的影響,并在優(yōu)化好的條件下驗證材料多次重復使用對BPA回收效果的影響；(2)在優(yōu)化好的實驗條件下,建立水中基于PA66功能化磁性材料的BPA檢測方法；(3)將制備的材料應用到實際樣品的檢測中,對海水、河水、地下水、自來水廠出廠水和自來水5種不同的水樣中的BPA進行檢測,采用高(5μg/L)中(10μg/L)低(15μg/L)三個濃度對實際水樣進行加標回收,驗證方法的準確性和不同水體基質(zhì)的適用能力。3.Fe3O4@TEOS@APTES對幾種典型環(huán)境污染物的吸附效果研究(1)結(jié)合HPLC分析技術(shù),初步驗證Fe3O4@TEOS@APTES對16種PAHs的吸附效果；(2)結(jié)合原子吸收分光光度計,初步驗證Fe3O4@TEOS@APTES對水中重金屬離子Pb、Cd的吸附效果。1.功能化磁性材料的制備及表征(1)成功制備了粒徑約為15-20nm的Fe3O4納米磁性內(nèi)核,優(yōu)化后的方法相對于傳統(tǒng)的化學共沉淀法所制得的Fe3O4磁性顆粒形貌更加規(guī)則,粒徑更加均勻；(2)TEOS在Fe3O4表面修飾成功,成功合成了規(guī)則球形、粒徑約為3OOnm的Fe3O4@TEOS;(3)利用反相無水微乳液合成新方法,成功制備了PA66功能化磁性材料,其分散性能好,形貌規(guī)則；(4)成功合成了形貌規(guī)則、粒徑均勻的球形Fe3O4@TEOS@APTES。2.PA66功能化磁性材料在BPA檢測中的應用(1)完成了PA66功能化磁性材料對BPA富集條件的優(yōu)化,并在優(yōu)化好的條件下驗證了材料多次重復使用對BPA回收效果的影響,證實了本材料可至少重復使用10次以上；(2)在優(yōu)化好的實驗條件下,建立了水樣中基于PA66功能化磁性材料的BPA的檢測方法,線性范圍0.20-100.00μg/L,檢出限為0.05μg/L,富集倍數(shù)為250倍；(3)將制備的材料應用到實際樣品的檢測中,對5種不同的水樣中的BPA進行檢測,加標回收率88.54%-104.46%。證實該方法對該5種水體基質(zhì)適用性良好。3. Fe3O4@TEOS@APTES對幾種典型環(huán)境污染物的吸附效果研究(1)該材料對苯并[a]芘、苊、苯并[a]蒽、苯并[b]熒蒽、苯并[k]熒蒽、二苯并[a,h]蒽和茚并芘7種稠環(huán)PAHs具有不同程度的吸附效果,吸附效率在61.0-79.0%之間；(2)該材料對水中Pb(5.0mg/I的吸附效率為94.4Cd(5.0mg/I的吸附效率為94.7%。證實了該材料對水中重金屬離子Pb、Cd具有較好的吸附效果。本研究制備了Fe3O4納米磁性內(nèi)核、二氧化硅磁性微球、PA66功能化磁性材料及氨基功能化磁性材料。確定了PA66功能化磁性材料對BPA吸附的最佳條件,建立了基于PA66功能化磁性材料的BPA檢測方法。利用制備的氨基功能化材料,實現(xiàn)了以苯并[a]芘為代表的7種PAHs的同時定量分析,為進一步的風險防控研究提供了依據(jù)。制備的氨基功能化磁性材料對重金屬離子Pb,Cd的吸附效果較好,為氨基功能化磁性材料在這些重金屬離子的去除及檢測方面的進一步應用提供了一定的理論依據(jù)。本研究所制備的功能化磁性材料在環(huán)境污染物的檢測中具有進一步研究價值和更廣闊的應用前景。
[Abstract]:Many kinds of environmental pollutants, causing a serious threat to human health and ecological environment. Environmental pollutant detection technology is established so for the risk of environmental pollution prevention and control, plays an important role in the protection of human health and ecological environment. Because of complex environmental samples, environmental pollutant detection projects vary, sample pretreatment technology has been one of the key links in establishing environmental pollutant detection technology and the development of functional magnetic materials. As a kind of new SPE materials, with fast magnetic response, high biocompatibility and a series of advantages of easy surface modification, in a fast and efficient enrichment of protein, nucleic acid, bacteria, viruses and other specific target both show a good application prospect. Therefore, will study the detection technology of functional applications of magnetic materials in environmental pollutants, the pollutants in environmental analysis The improvement of the protection of human health, a preparation and characterization of.1. functional magnetic materials important for (1) nano ferroferric oxide (Fe3O4) synthesis and characterization of magnetic core of the system; (2) magnetic silica microspheres (Fe3O4@TEOS) preparation and characterization of polyamide; (3) 66 (PA66) preparation and characterization of functional magnetic materials; (4) the amino functionalized magnetic material (Fe3O4@TEOS@APTES) preparation and characterization of.2.PA66 functional magnetic materials in bisphenol A (BPA) for the detection of PA66 (1) to optimize the functional magnetic materials of BPA enrichment conditions; (2) to establish BPA PA66 method for detection of functional magnetic materials based on the actual application; (3) preliminary sample detection of.3. Fe3O4@TEOS@APTES in the detection of several typical environmental pollutants in Fe3O4@TEOS@APTES (1) of 16 kinds of polycyclic aromatic hydrocarbons (PAHs) on the adsorption effect of pollutants; (2) Fe3O4@TEOS@APTE S of heavy metal Pb, Cd Preparation and characterization of adsorption effects of.1. functional magnetic materials (1) preparation and characterization of nanometer Fe3O4 magnetic core: in the traditional chemical co precipitation method on the basis of system adjustment by alkaline reaction, ferric iron and two valent iron ratio, combined deoxidation, aging technology on the preparation of Fe3O4 process optimization, and in TEM, XRD on the synthesis of Fe3O4 was investigated; (2) preparation and characterization of Fe3O4@TEOS: modification of magnetic Fe3O4 core by using silicon rich oxygen bond TEOS, and TEM, XRD3 inch]Fe3O4@TEOS synthesis characterization; (3) preparation and characterization of PA66 functional magnetic materials. A new method of using reverse microemulsion synthesis of anhydrous, complete insoluble in water and common organic materials in solid phase modification of hydrophilic magnetic microspheres, and to TEM, the PA66 functional magnetic materials synthesis were characterized by FT-IR; (4) preparation and Fe3O4@ TEOS@APTES Sign: modification on the surface of Fe3O4@TEOS prepared by APTES, and in TEM, XRD, FT-IR for the application of functional magnetic materials characterization of.2.PA66 in detection of BPA on the synthesis of Fe3O4@TEOS@APTES (1) the effect of the pretreatment effect related factors of PA66 functional magnetic materials in the preparation process of BPA, and in the optimized conditions to verify materials used repeatedly impact on BPA recovery effect; (2) under the optimized experimental conditions under the established water BPA PA66 detection method based on functional magnetic materials; (3) the preparation of the material applied to the detection of the actual samples of sea water, river water, groundwater the tap water, tap water and 5 kinds of BPA in water samples were detected by high (5 g/L) in (10 g/L) and low (15 g/L) three concentration of water samples spiked, the accuracy of the verification method and different water matrix. Study on adsorption effects of several typical environmental pollutants with the ability of.3.Fe3O4@TEOS@APTES (1) combined with HPLC analysis, preliminary verification of Fe3O4@TEOS@APTES adsorption on 16 PAHs; (2) combined with atomic absorption spectrophotometer, preliminary verification of Fe3O4@TEOS@APTES of water heavy metal ion Pb, adsorption effect of.1. functional magnetic materials preparation and characterization Cd (1) were successfully prepared Fe3O4 nano particle magnetic core size is about 15-20nm, the optimized method of Fe3O4 magnetic particle morphology compared with the traditional chemical precipitation method produced more rules, more uniform particle size; (2) TEOS in Fe3O4 surface modification, synthesis of spherical particles. The size is about 3OOnm Fe3O4@TEOS; (3) by inverse microemulsion anhydrous synthesis method, PA66 functional magnetic materials were prepared successfully, the good dispersion, the rules of morphology; (4) successfully synthesized particle morphology rules The application of spherical Fe3O4@TEOS@APTES.2.PA66 functional magnetic materials with uniform diameter in the detection of BPA (1) completed the optimization of PA66 functional magnetic materials of BPA enrichment conditions, and verify the materials used repeatedly effect on BPA recovery effect in optimized conditions, confirmed that the materials can be reused at least 10 times; (2) under the optimized experimental conditions under the established water detection method of PA66 functional magnetic materials based on BPA, the linear range of g/L 0.20-100.00, the detection limit is 0.05 g/L, the enrichment ratio of 250 times; (3) the preparation of the material applied to the actual samples, detection on 5 kinds of BPA in water samples, the recoveries of 88.54%-104.46%. confirmed the method research on adsorption effect of good.3. Fe3O4@TEOS@APTES on several typical pollutants of the environment for the matrix of 5 kinds of water (1) the material of benzo [a] Acenaphthene, pyrene, benzo [a] anthracene, benzo [b] fluoranthene, benzo [k] fluoranthene, benzo [a anthracene two, h] and Indeno pyrene 7 fused ring PAHs has adsorption effect in different degree, the adsorption efficiency of 61.0-79.0%; (2) the material of Pb (water adsorption efficiency for 5.0mg/I 94.4Cd (5.0mg/I adsorption efficiency of 94.7%. confirmed that the material of heavy metal ions Pb, Cd has better adsorption effect. The preparation of Fe3O4 nano magnetic core, magnetic silica microspheres, PA66 functionalized amino functionalized magnetic materials and magnetic materials. The PA66 functional magnetic materials on BPA adsorption the optimum conditions were established based on the PA66 functional magnetic materials BPA detection method. The preparation of amino functionalized materials, in order to realize the benzo [a] pyrene as the representative of the 7 kinds of PAHs and quantitative analysis, for further research of risk prevention and control provide the basis. The preparation of amino functionalized magnetic Material for heavy metal ions Pb, good absorption effect of the Cd, provides a theoretical basis for the further application of functionalized magnetic materials in the detection and removal of these heavy metal ions. The preparation of functional magnetic materials has application value and broad prospects for further research in the detection of environmental pollutants.

【學位授予單位】：中國人民解放軍軍事醫(yī)學科學院
【學位級別】：碩士
【學位授予年份】：2015
【分類號】：X830

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