三氫化鋁干法合成工藝研究
發(fā)布時間：2018-12-09 17:24
【摘要】：傳統(tǒng)化石能源的日趨消耗及其使用過程中引發(fā)的諸多環(huán)境污染問題越來越受到人們的廣泛關(guān)注,人們迫切需要找到一種可再生、清潔能源。氫能以資源豐富、環(huán)保性能好以及經(jīng)濟效益高等優(yōu)點逐漸得到大家的青睞,而儲氫卻成為氫能源開發(fā)與利用的瓶頸。AlH3是典型的金屬儲氫材料,因其具有優(yōu)越儲氫性能——高理論儲氫體積和儲氫密度,而被視為最有發(fā)展和應(yīng)用前景的優(yōu)質(zhì)儲氫材料,在儲氫材料領(lǐng)域備受人們關(guān)注。本論文提出了Al H3的干法合成法,在避免了液相合成法的缺點同時,也克服了直接合成法的限制性因素,主要研究內(nèi)容:利用機械球磨法制備活性很高、晶粒非常小的鋁粉,使用TG、SEM和XRD對球磨得到的鋁粉進行表征;實驗結(jié)果表明該活性鋁粉初始增重溫度是280℃,最大氧化速率是3.43 mg/min,平均晶粒尺寸是20.1 nm;在溶劑甲苯中制備催化劑R2AlH(R代表烷基),利用LiAlH4和Et2AlCl作原料,在95℃下反應(yīng)5 h制備生成Et2AlH;利用LiAlH4與Me3Al作原料,在85℃條件下反應(yīng)3 h制備生成Me2AlH,對制備得到的產(chǎn)物進行核磁共振表征(1H NMR),核磁譜圖分析表明采用以上實驗方法可以制備生成的Et2AlH與Me2AlH,并且二者的純度較高。研究使用二異丁基氫化鋁、二乙基氫化鋁和二甲基氫化鋁催化活性鋁粉與氫氣反應(yīng),通過控制反應(yīng)溫度(90~120℃)和時間(8~12h)進行AlH3合成實驗;對實驗生成的產(chǎn)物分別進行XRD表征,實驗結(jié)果表明使用三種R2AlH催化活性鋁粉與氫氣均可以生成AlH3;利用放氫實驗裝置分別對產(chǎn)物進行放氫實驗,由實驗結(jié)果可知三種催化反應(yīng)中AlH3產(chǎn)率分別為0.90%、1.25%和2.76%;根據(jù)催化反應(yīng)條件及產(chǎn)物產(chǎn)率可知,催化劑活性大小順序為二甲基氫化鋁、二乙基氫化鋁、二異丁基氫化鋁。采用低熱固相法,以LiAlH4與AlCl3作反應(yīng)原料,探究反應(yīng)溫度(65~95℃)、時間(2~5h)以及原料摩爾比(4:1~12:1)對合成AlH3的影響;反應(yīng)產(chǎn)物的XRD表征分析結(jié)果表明:當(dāng)LiAlH4與AlH3摩爾比大于4:1,反應(yīng)溫度高于75℃,反應(yīng)時間大于2 h時,采用低熱固相法可以獲得AlH3;XRD表征結(jié)果與放氫實驗結(jié)果表明低熱固相法合成AlH3的最優(yōu)條件為LiAlH4與AlH3摩爾比為9:1,反應(yīng)溫度為85℃,反應(yīng)時間為4 h,在此反應(yīng)條件下AlH3產(chǎn)率為24.0%。。
[Abstract]:People pay more and more attention to the increasing consumption of traditional fossil energy and many environmental pollution problems caused by its use. People urgently need to find a kind of renewable and clean energy. Hydrogen energy is getting more and more popular because of its rich resources, good environmental performance and high economic benefit, while hydrogen storage has become the bottleneck of hydrogen energy development and utilization. AlH3 is a typical metal hydrogen storage material. Because of its superior hydrogen storage properties, such as high theoretical hydrogen storage volume and hydrogen density, it is regarded as the most promising high quality hydrogen storage material, which has attracted much attention in the field of hydrogen storage materials. In this paper, a dry synthesis method of Al H3 is proposed, which avoids the shortcomings of liquid phase synthesis and overcomes the restrictive factors of direct synthesis. The main research contents are as follows: preparation of aluminum powder with high activity and very small grain by mechanical ball milling method. The Al powder prepared by ball milling was characterized by TG,SEM and XRD. The experimental results show that the initial weight gain temperature is 280 鈩，
本文編號：2369753
[Abstract]:People pay more and more attention to the increasing consumption of traditional fossil energy and many environmental pollution problems caused by its use. People urgently need to find a kind of renewable and clean energy. Hydrogen energy is getting more and more popular because of its rich resources, good environmental performance and high economic benefit, while hydrogen storage has become the bottleneck of hydrogen energy development and utilization. AlH3 is a typical metal hydrogen storage material. Because of its superior hydrogen storage properties, such as high theoretical hydrogen storage volume and hydrogen density, it is regarded as the most promising high quality hydrogen storage material, which has attracted much attention in the field of hydrogen storage materials. In this paper, a dry synthesis method of Al H3 is proposed, which avoids the shortcomings of liquid phase synthesis and overcomes the restrictive factors of direct synthesis. The main research contents are as follows: preparation of aluminum powder with high activity and very small grain by mechanical ball milling method. The Al powder prepared by ball milling was characterized by TG,SEM and XRD. The experimental results show that the initial weight gain temperature is 280 鈩，
本文編號：2369753
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