本文關(guān)鍵詞：高比表面積介孔氧化鋁的制備與表征　出處：《沈陽(yáng)工業(yè)大學(xué)》2017年碩士論文　論文類(lèi)型：學(xué)位論文

  更多相關(guān)文章： 沉淀法 介孔氧化鋁 有機(jī)物 摻雜改性 熱穩(wěn)定性

【摘要】：介孔氧化鋁具有較高的比表面積、適宜的孔結(jié)構(gòu)、較高的機(jī)械強(qiáng)度和良好的表面酸性等優(yōu)異性能,在大分子吸附與分離、多相催化、功能材料和陶瓷等領(lǐng)域中得到了廣泛的應(yīng)用,是一種性能優(yōu)異的催化和吸附材料。目前制備的介孔氧化鋁性能較差,尤其在高溫下易轉(zhuǎn)變成熱力學(xué)穩(wěn)定的剛玉相氧化鋁而失去活性,所以研究工藝簡(jiǎn)單、成本低廉且能獲得具有優(yōu)異性能和高熱穩(wěn)定性介孔氧化鋁的工藝方法具有重要的理論與現(xiàn)實(shí)意義。本論文首先對(duì)以硫酸鋁銨為鋁源、碳酸氫銨為沉淀劑采用沉淀法制備介孔氧化鋁的工藝條件進(jìn)行了研究,確定的最佳工藝條件為:pH值為9.5、反應(yīng)溫度為60°C、洗滌液為熱水(90°C蒸餾水),所得產(chǎn)物經(jīng)500°C焙燒后得到的介孔氧化鋁的比表面積、孔容和孔徑分別為571m2/g、0.78cm3/g和6.15nm。其次研究了有機(jī)醇PEG和EDTA對(duì)介孔氧化鋁熱穩(wěn)定性的影響,發(fā)現(xiàn)PEG和EDTA均可以提高其熱穩(wěn)定性。其中PEG可有效抑制γ-Al2O3向α-Al2O3的晶型轉(zhuǎn)變,其最佳添加量為1mol%,改性后制備的樣品經(jīng)500°C焙燒后,其比表面積、孔容和孔徑分別為589m2/g、0.96cm3/g和6.69nm,經(jīng)1100°C焙燒后其比表面積、孔容和孔徑分別為71m2/g、0.56cm3/g和14.69nm。EDTA的最佳添加量為6mol%,改性后的樣品經(jīng)500°C焙燒后其表面積、孔容和孔徑分別為614m2/g、0.97cm3/g和6.69nm。最后通過(guò)沉淀-浸漬法制備了Si和La摻雜介孔氧化鋁,得到了熱穩(wěn)定性能優(yōu)異的介孔氧化鋁。其中Si的最佳摻雜量為12%,改性后的樣品在500°C、700°C、900°C、1000°C、1100°C和1200°C焙燒時(shí)相對(duì)于未添加樣品的比表面積提高率分別為4.9%、12.2%、36.7%、58.47%、69.79%和71.11%,樣品經(jīng)1100°C和1200°C處理后的比表面積、孔容和孔徑分別為149m2/g、0.52cm3/g、8.9nm和45m2/g、0.16cm3/g、7.99nm。稀土元素La的最佳摻雜量為9%,摻雜改性后制備的樣品經(jīng)1100°C焙燒后獲得的比表面積高達(dá)93m2/g,體現(xiàn)了改性后介孔氧化鋁的高熱穩(wěn)定性。
[Abstract]:The mechanical strength of mesoporous alumina with high specific surface area, suitable pore structure, high surface acidity and good performance, has been widely used in the field of macromolecular adsorption and separation, catalysis, functional materials and ceramics, catalysis and adsorption material is a kind of excellent. At present, the preparation of mesoporous alumina with poor performance, especially under high temperature into a thermodynamically stable phase of alumina corundum and so on loss of activity, simple process and low cost and can obtain process with excellent properties and thermal stability of mesoporous alumina has important theoretical and practical significance. Firstly, the ammonium aluminum sulfate as aluminum source and ammonium hydrogen carbonate using technology in the preparation of mesoporous alumina by precipitation as precipitating agent was studied, the optimum preparation conditions were: pH value is 9.5, the reaction temperature is 60 DEG C, washing liquid for hot water (90 degrees C distilled water), medium porous alumina products obtained after calcined at 500 ~ C of surface area, pore and Kong Rong were 571m2/g, 0.78cm3/g and 6.15nm. Secondly, the effect of organic alcohol PEG and EDTA on the thermal stability of mesoporous alumina was studied. It was found that both PEG and EDTA could improve the thermal stability of mesoporous alumina. The PEG can effectively inhibit the gamma -Al2O3 transition to crystalline alpha -Al2O3, the optimal dosage was 1mol%, after calcined at 500 ~ C samples prepared by the modified method, the surface area, pore size and Kong Rong were 589m2/g, 0.96cm3/g and 6.69nm, after calcined at 1100 ~ C, the specific surface area of Kong Rong and the pore size were 71m2/g, 0.56cm3/g and 14.69nm. The optimum addition of EDTA was 6mol%. The surface area, Kong Rong and pore size of the modified samples were 614m2/g, 0.97cm3/g and 6.69nm respectively after 500 degree C roasting. At last, Si and La doped mesoporous alumina were prepared by precipitation impregnation method, and the mesoporous alumina with excellent thermal stability was obtained. The optimal doping amount of Si is 12%, the modified samples in 500 ~ C, 700 ~ C, 900 ~ C, 1000 ~ C, 1100 ~ C and 1200 ~ C was compared to samples without surface area increase rate were 4.9%, 12.2%, 36.7%, 58.47%, 69.79% and 71.11%. The sample was 1100 ~ C and 1200 ~ C after the specific surface area, pore and Kong Rong were 149m2/g, 0.52cm3/g, 8.9nm, 0.16cm3/g, 7.99nm and 45m2/g. The optimum doping amount of rare earth element La is 9%. The surface area of the prepared samples is 93m2/g after 1100 degree C calcination, which indicates the high thermal stability of modified mesoporous alumina.
【學(xué)位授予單位】：沈陽(yáng)工業(yè)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類(lèi)號(hào)】：TQ133.1

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