本文選題：超重力反應(yīng)器　切入點(diǎn)：縮合　出處：《北京化工大學(xué)》2015年碩士論文　論文類型：學(xué)位論文

【摘要】：羥醛縮合反應(yīng)在工業(yè)上具有十分廣泛的應(yīng)用。然而,縮合反應(yīng)過程復(fù)雜,副反應(yīng)產(chǎn)物多,從文獻(xiàn)報(bào)道來看,物料間的混合程度對(duì)產(chǎn)品質(zhì)量的影響比較顯著。作為化工過程強(qiáng)化技術(shù)的代表之一,超重力技術(shù)能極大地強(qiáng)化混合和傳遞過程,減少停留時(shí)間,抑制副反應(yīng)的發(fā)生,大幅提高產(chǎn)品質(zhì)量。為此,本文以某羥基酮化合物(H)的合成為例,分別在攪拌釜(STR)反應(yīng)器以及超重力組合反應(yīng)器(RPB+STR)中系統(tǒng)研究了各種工藝參數(shù)對(duì)原料轉(zhuǎn)化率、目標(biāo)產(chǎn)品選擇性和收率的影響,并采用氣質(zhì)聯(lián)用儀(GC-MS)、紅外光譜儀(IR)、核磁共振儀(NMR)等檢測儀器對(duì)產(chǎn)品結(jié)構(gòu)進(jìn)行了表征。同時(shí),采用Gauss View軟件,模擬了該主反應(yīng)的反應(yīng)焓。研究結(jié)果表明：1、采用攪拌反應(yīng)釜為縮合反應(yīng)器,考察了反應(yīng)時(shí)間(t)、溫度(T)、醛醇比(θ)、醛酮比(e)、醛堿比(β)、攪拌釜轉(zhuǎn)速(n)等對(duì)原料轉(zhuǎn)化率及反應(yīng)產(chǎn)物H收率的影響。當(dāng)醛酮比為1：4時(shí),最佳反應(yīng)條件為：溫度40℃、醛堿比1：0.15、醛醇比1：10、攪拌槳轉(zhuǎn)速1000 rpm、反應(yīng)時(shí)間25 min。2、使用超重力組合反應(yīng)器對(duì)縮合過程進(jìn)行強(qiáng)化。當(dāng)醛酮比為1：4時(shí),最佳反應(yīng)條件為：溫度40℃、醛堿比1：0.10、醛醇比1：7.40、轉(zhuǎn)子轉(zhuǎn)速2840rpm、反應(yīng)時(shí)間12 min。3、超重力組合反應(yīng)器能加快反應(yīng)速率,縮短反應(yīng)時(shí)間,減少催化劑(減少33%)和溶劑(減少26%)使用量,將目標(biāo)產(chǎn)物收率提高5%-10%。4、在攪拌釜反應(yīng)器內(nèi)研究了該縮合反應(yīng)的宏觀動(dòng)力學(xué)。在本文的操作條件下,該反應(yīng)符合擬一級(jí)動(dòng)力學(xué)反應(yīng)規(guī)律。指前因子為3.47×1010L·mol-1·min-1,表觀活化能為60.99 kJ·mol-1,進(jìn)一步推導(dǎo)出了該主反應(yīng)的宏觀反應(yīng)動(dòng)力學(xué)方程,表示如下：d[H]/dt]=k'[A]=3.47×1010 exp[-6.099×104/(RT)][C][OH-][A]/[H2O]
[Abstract]:Aldol condensation reaction has been widely used in industry. However, the condensation process is complex and the byproducts are many. As one of the representatives of chemical process strengthening technology, hypergravity technology can greatly enhance the mixing and transfer process, reduce residence time, and inhibit the occurrence of side effects. Therefore, taking the synthesis of a hydroxy ketone compound (H) as an example, the feedstock conversion rate of various process parameters was systematically studied in stirred tank reactor (STR) reactor and high gravity combined reactor (HPB STR), respectively. The influence of selectivity and yield of the target product was studied. The structure of the product was characterized by GC-MSX, IR, NMR, and Gauss View software. The reaction enthalpy of the main reaction was simulated. The effects of reaction time, temperature, ratio of aldehyde to alcohol (胃), ratio of aldehyde to kettle, ratio of aldehyde to base (尾), rotating speed of stirred kettle on the conversion of raw materials and H yield of reaction products were investigated. When the ratio of aldehyde to ketone was 1: 4, the optimum reaction conditions were as follows: temperature 40 鈩，

本文編號(hào)：1610682