本文關(guān)鍵詞： 酸洗廢液 納米氧化鐵 烷基化反應(yīng) N-芐基苯胺 鄰芐基苯酚 對(duì)芐基苯酚　出處：《哈爾濱師范大學(xué)》2015年碩士論文　論文類型：學(xué)位論文

【摘要】：在鋼鐵制品的加工過程中,通常要用鹽酸酸洗處理其表面的氧化膜,從而產(chǎn)生大量的酸洗廢液。其主要是由氯化氫、氯化亞鐵、水及少量其他雜質(zhì)組成。這些酸洗廢液直接排放會(huì)造成環(huán)境的污染。本文采用溶膠-凝膠法以工業(yè)酸洗廢液為原料可控制備了不同形貌與尺寸的納米氧化鐵材料。利用XRD、UV-Vis、SEM、TEM、FT-IR和ICP-MS等技術(shù)對(duì)其進(jìn)行了表征。實(shí)驗(yàn)結(jié)果表明,在控制pH及其他制備條件下可以得到納米尺寸25 nm、網(wǎng)狀的(Fe-w)、45 nm直徑棒狀的(Fe-r)和50 nm葉寬的黃花菜狀(Fe-l)等的α-Fe2O3粉體材料。研究了溶液pH、超聲處理時(shí)間等因素對(duì)氧化鐵的影響。進(jìn)而得出以聚乙二醇作為分散劑,反應(yīng)溫度85℃,反應(yīng)8小時(shí),500℃下煅燒2小時(shí)的工藝制備條件。選擇最佳條件下制得的納米氧化鐵α-Fe2O3,并將其作為催化劑用來催化苯胺和氯化芐的烷基化反應(yīng)合成N-芐基苯胺。實(shí)驗(yàn)結(jié)果表明,納米氧化鐵α-Fe2O3粒子同樣具有很高的催化活性,其轉(zhuǎn)化頻率TOF為65.1 h-1。優(yōu)化了反應(yīng)溫度、時(shí)間、苯胺和氯化芐的摩爾比和催化劑的用量等條件,確定了最佳的反應(yīng)工藝條件是:反應(yīng)溫度為60℃,反應(yīng)時(shí)間為1h,納米氧化鐵的用量0.1 g,苯胺和氯化芐物質(zhì)的量之比為4:1,該條件下氯化芐的轉(zhuǎn)化率為99.69%,N-芐基苯胺的選擇性為92.54%。另外,研究了催化劑的重復(fù)利用的性能,重復(fù)使用三次后,催化劑的催化活性基本未變。同時(shí),研究了納米α-Fe2O3作為催化劑用于催化苯酚和氯化芐的烷基化反應(yīng)合成鄰芐基苯酚和對(duì)芐基苯酚。實(shí)驗(yàn)結(jié)果表明,納米氧化鐵α-Fe2O3粒子表現(xiàn)出很高的催化活性,其轉(zhuǎn)化頻率TOF為33.3 h-1。對(duì)反應(yīng)溫度、時(shí)間、苯酚和氯化芐的摩爾比和催化劑的用量等條件進(jìn)行了研究,確定了最佳的反應(yīng)工藝條件是:反應(yīng)溫度為60℃,反應(yīng)時(shí)間為1h,苯酚和氯化芐物質(zhì)的量之比為3:1,納米氧化鐵的用量0.1 g,該條件下氯化芐的轉(zhuǎn)化率為97.09%,鄰芐基苯酚的選擇性為42.85%,對(duì)芐基苯酚的選擇性為42.16%。研究了催化劑的重復(fù)利用的性能,重復(fù)使用三次后,催化劑的催化活性基本未變,說明此催化劑具有很好的的工業(yè)應(yīng)用前景。另外,根據(jù)文獻(xiàn)報(bào)道及實(shí)驗(yàn)中所得到的結(jié)果,探討了苯胺及苯酚與氯化芐的烷基化反應(yīng)的機(jī)理。
[Abstract]:In the process of processing iron and steel products, the oxidation film on the surface of iron and steel products is usually treated with hydrochloric acid to produce a large amount of acid pickling waste liquid, which is mainly composed of hydrogen chloride and ferrous chloride. Water and a small amount of other impurities. The direct discharge of these acid pickling waste liquor will cause environmental pollution. In this paper, nanometer ferric oxide materials with different morphology and size can be controlled by sol-gel method using industrial pickling waste liquid as raw material. Using XRD. It was characterized by UV-Vis-SEMMA-TEMT-IR and ICP-MS. Under the conditions of pH control and other preparation conditions, the nanocrystalline size of 25 nm, netted Fe Fe w) can be obtained. 偽 -Fe _ 2O _ 3 powders with a diameter of 45 nm rod shape and a leaf width of 50 nm were investigated. The pH of the solution was studied. The effect of ultrasonic treatment time on ferric oxide was studied. The results showed that polyethylene glycol was used as dispersant, reaction temperature was 85 鈩，

本文編號(hào)：1451579