本文關(guān)鍵詞： 三氫化鋁 α-三氫化鋁 固相真空法 固相甲苯法 漿液法 一步法　出處：《哈爾濱工業(yè)大學(xué)》2015年碩士論文　論文類(lèi)型：學(xué)位論文

【摘要】：本文系統(tǒng)綜述了Al H3的合成及應(yīng)用研究現(xiàn)狀。提出一種改進(jìn)型的制備方法:(1)在制備Al H3乙醚絡(luò)合物過(guò)程中直接用含有Li Cl沉淀的Al H3乙醚絡(luò)合物進(jìn)行脫醚轉(zhuǎn)晶,得到固相產(chǎn)物;(2)對(duì)固相產(chǎn)物進(jìn)行洗滌,除去Li Cl雜質(zhì)并對(duì)α-Al H3進(jìn)行穩(wěn)定化處理。此種不需過(guò)濾Li Cl的方法被我們稱(chēng)為“一鍋法”。根據(jù)Al H3乙醚絡(luò)合物所處的狀態(tài)和環(huán)境,將Al H3的“一鍋法”合成細(xì)化成固相真空法、固相甲苯法以及漿液法并分別進(jìn)行研究。最后還研究了Al H3的“一步法”合成。通過(guò)固相真空法,將含有Li Cl的固體Al H3醚合物在真空條件下進(jìn)行轉(zhuǎn)晶,XRD和IR等測(cè)試結(jié)果表明改變Li BH4用量以及轉(zhuǎn)晶溫度、轉(zhuǎn)晶時(shí)間等反應(yīng)條件,利用固相真空法制備出了單一晶型的α-Al H3:當(dāng)沒(méi)有Li BH4參與反應(yīng)且Li Al H4:Al Cl3摩爾比為4:1時(shí),單一晶型α-Al H3所需的轉(zhuǎn)晶溫度為77~80℃,轉(zhuǎn)晶時(shí)間為2~3 h;當(dāng)有Li BH4參與反應(yīng)且Li Al H4:Al Cl3:Li BH4摩爾比為4:1:0.5時(shí),單一晶型α-Al H3所需的轉(zhuǎn)晶溫度為80~85℃,轉(zhuǎn)晶時(shí)間為1~2 h。通過(guò)固相甲苯法,將含有Li Cl的固體Al H3醚合物在甲苯中進(jìn)行轉(zhuǎn)晶,XRD和IR等測(cè)試結(jié)果表明改變轉(zhuǎn)晶溫度、轉(zhuǎn)晶時(shí)間等反應(yīng)條件,利用固相甲苯法也制備出了單一晶型的α-Al H3:當(dāng)Li Al H4:Al Cl3:Li BH4摩爾比為4:1:1時(shí),理想轉(zhuǎn)晶溫度和時(shí)間分別為80~85℃和1.5~2 h。此種方法制備的單一晶型的α-Al H3氫含量為8.8~8.9wt%。通過(guò)漿液法,將Al H3乙醚絡(luò)合物溶液濃縮后,置于甲苯條件下進(jìn)行轉(zhuǎn)晶,改變轉(zhuǎn)晶溫度以及實(shí)驗(yàn)流程,確定了漿液法制備α-Al H3的合適條件。XRD結(jié)果表明產(chǎn)物為單一晶型的α-Al H3;TG測(cè)試表明失重量與理論值10.1wt%相當(dāng),且產(chǎn)物的初始分解溫度高達(dá)176℃。類(lèi)似于漿液法,一步法是直接用Li Al H4和Al Cl3在90~100℃的甲苯中直接制備非溶劑化的α-Al H3。實(shí)驗(yàn)結(jié)果表明樣品是直徑為10~50μm的大顆粒,分解溫度在170℃,含氫量高達(dá)10%。綜合對(duì)比四種方法的結(jié)果,漿液法合成的α-Al H3呈直徑10~50μm的大顆粒,測(cè)試結(jié)果表明制備的α-Al H3的生成熱焓值為11.9 k J/mol,失重率高達(dá)10wt%,均與理論值相一致,因此更適合單一晶型α-Al H3的制備。
[Abstract]:In this paper, the synthesis and application of Al H 3 are reviewed systematically. An improved preparation method: 1) in the process of preparing Al H 3 ether complex, it is directly used to deether transprystallization with Al H 3 ether complex containing Li Cl precipitation. The solid product is washed, the impurity of Li Cl is removed and 偽 -Al H 3 is stabilized. This method, which does not require filtration of Li Cl, is called "one pot process." according to the state and environment of the Al H 3 ether complex, The "one pot" synthesis of Al H 3 was refined into solid phase vacuum method, solid phase toluene method and slurry method, respectively. Finally, the "one step" synthesis of Al H 3 was also studied. The results of XRD and IR measurements of solid Al H 3 ether complexes containing Li Cl in vacuum show that the amount of Li BH4 and the reaction conditions such as temperature and time of transition are changed. The single crystalline 偽 -Al H 3 was prepared by solid phase vacuum method. When there was no Li BH4 in the reaction and the mole ratio of Li Al H 4 to Al Cl3 was 4: 1, the transition temperature of 偽 -Al H 3 was 7780 鈩，

本文編號(hào)：1507953