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磁性四氧化三鐵復(fù)合顆粒的制備及其在吸附金屬離子方面的應(yīng)用

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  本文關(guān)鍵詞: 四氧化三鐵 復(fù)合粉體 改性 重金屬離子 吸附 出處:《中國海洋大學(xué)》2015年碩士論文 論文類型:學(xué)位論文


【摘要】:四氧化三鐵因為具備良好的物理化學(xué)穩(wěn)定性、生物兼容性和特殊的磁性能,使它在磁分離、催化劑、磁流體、生物醫(yī)學(xué)和環(huán)境治理等領(lǐng)域得到廣泛應(yīng)用。本文采用沉淀法和溶劑熱法兩種方法制備出磁性納米Fe304顆粒,并探討了不同制備方法、反應(yīng)時間和溫度對Fe304顆粒晶型和性狀的影響。通過改進的Stober法和沉淀聚合法在四氧化三鐵顆粒表面包覆二氧化硅和聚甲基丙烯酸酯(PMMA),并在氨基改性后進行了重金屬離子的吸附測試。具體研究內(nèi)容如下:(1)利用共沉淀法和溶劑熱法分別制備出純度較高的納米四氧化三鐵顆粒,通過XRD、 SEM和VSM等測試手段進行表征。結(jié)果顯示,共沉淀法制得的Fe304顆粒粒徑較小,但團聚比較嚴(yán)重:溶劑熱法制備出的Fe304顆粒分散性比較好,形狀規(guī)則,具有良好的超順磁性能。因此,我們選用溶劑熱法制備的納米Fe304顆粒作為后期實驗的核心粒子,而且此方法在無水環(huán)境下反應(yīng),避免了Fe304的氧化問題,操作簡單可行。(2)利用改進的Stober法在納米Fe304顆粒表面包覆上一層SiO2,討論了正硅酸乙酯(TEOS)的加入量對包覆結(jié)果的影響。通過XRD、SEM、TEM等檢測方法進行表征,得出最佳包覆的配比,制備出顆粒粒徑均勻、形狀規(guī)則、分散性較好的Fe3O4@SiO2復(fù)合顆粒。(3)利用懸浮聚合法在Fe3O4@SiO2復(fù)合顆粒表面包覆PMMA。討論了預(yù)先用硅烷偶聯(lián)劑(KH-570)處理對包覆結(jié)果的影響。通過XRD、SEM、TG和FT-IR等測試方法對樣品表征,實驗表明,在預(yù)先將Fe3O4@SiO2復(fù)合顆粒用KH-570處理后,得到的Fe3O4@SiO2@PMMA復(fù)合顆粒形狀更加規(guī)則圓整而且表面光滑。(4)利用氨基化的方法對Fe3O4@SiO2@PMMA復(fù)合顆粒進行修飾,由FT-IR分析可知,Fe3O4@SiO2@PMMA復(fù)合顆粒表面接上氨基。(5)用氨基化的Fe3O4@SiO2@PMMA復(fù)合顆粒進行Cu2+和Ni2+的吸附試驗。將復(fù)合顆粒分別加入到Cu2+溶液和Ni2+的溶液中,通過紫外-可見分光光度計測量吸附量的大小。討論了吸附量隨反應(yīng)時間和pH值的變化。結(jié)果表明,當(dāng)pH=5.5時,復(fù)合顆粒在2.5 h時,對Cu2+的最大吸附量約為170 mg/g;當(dāng)pH=7時,復(fù)合顆粒在2h時對Ni2+的最大吸附量達(dá)到72 mg/g。
[Abstract]:Due to its good physical and chemical stability, biological compatibility and special magnetic properties, iron trioxide makes it in magnetic separation, catalyst, magnetic fluid, In this paper, magnetic Fe304 nanoparticles were prepared by precipitation method and solvothermal method, and different preparation methods were discussed. The effects of reaction time and temperature on the crystal shape and properties of Fe304 particles were studied. Silica and PMMA were coated on the surface of Fe _ 2O _ 4 particles by modified Stober method and precipitation polymerization method, and heavy gold was prepared after modification by amino groups. The specific contents of the study are as follows: 1) Nano-sized iron trioxide particles with high purity were prepared by co-precipitation method and solvothermal method respectively. The results showed that the particle size of Fe304 prepared by co-precipitation method was small, but the agglomeration was serious. The Fe304 particles prepared by solvothermal method had good dispersion and regular shape. Therefore, Fe304 nanoparticles prepared by solvothermal method were chosen as the core particles in the later experiment, and the reaction in anhydrous environment avoided the problem of Fe304 oxidation. The effect of the content of tetraethylorthosilicate (TEOS) on the coating results was discussed. The optimum coating ratio was obtained by means of XRDX SEMTEM and other methods. The particle size is uniform and the shape is regular. Fe3O4@SiO2 composite particles with good dispersion were coated on the surface of Fe3O4@SiO2 composite particles by suspension polymerization. The effect of pre-treatment with silane coupling agent (KH-570) on the coating results was discussed. The samples were characterized by XRD-SEMTG and FT-IR. After the Fe3O4@SiO2 composite particles were treated with KH-570 in advance, the shape of the Fe3O4@SiO2@PMMA composite particles was more regular and round and the surface was smooth. 4) the Fe3O4@SiO2@PMMA composite particles were modified by amino method. FT-IR analysis showed that Fe3O4SiO2PMMA composite particles were coated with amino groups. (5) Aminated Fe3O4@SiO2@PMMA composite particles were used to adsorb Cu2 and Ni2. The composite particles were added to Cu2 solution and Ni2 solution, respectively. The adsorption capacity was measured by UV-Vis spectrophotometer. The change of adsorption capacity with reaction time and pH value was discussed. The results showed that the maximum adsorption capacity of Cu2 was about 170mg / g when pH=5.5 was 2.5 h, and when pH = 7:00, the maximum adsorption capacity of Cu2 was about 170mg / g. The maximum amount of Ni2 adsorbed by the composite particles at 2h was 72 mg / g.
【學(xué)位授予單位】:中國海洋大學(xué)
【學(xué)位級別】:碩士
【學(xué)位授予年份】:2015
【分類號】:TQ138.11;O647.3

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