超重力反应器强化缩合反应新工艺的研究

发布时间：2018-03-14 09:50

  本文选题：超重力反应器　切入点：缩合　出处：《北京化工大学》2015年硕士论文　论文类型：学位论文

【摘要】：羟醛缩合反应在工业上具有十分广泛的应用。然而,缩合反应过程复杂,副反应产物多,从文献报道来看,物料间的混合程度对产品质量的影响比较显著。作为化工过程强化技术的代表之一,超重力技术能极大地强化混合和传递过程,减少停留时间,抑制副反应的发生,大幅提高产品质量。为此,本文以某羟基酮化合物(H)的合成为例,分别在搅拌釜(STR)反应器以及超重力组合反应器(RPB+STR)中系统研究了各种工艺参数对原料转化率、目标产品选择性和收率的影响,并采用气质联用仪(GC-MS)、红外光谱仪(IR)、核磁共振仪(NMR)等检测仪器对产品结构进行了表征。同时,采用Gauss View软件,模拟了该主反应的反应焓。研究结果表明：1、采用搅拌反应釜为缩合反应器,考察了反应时间(t)、温度(T)、醛醇比(θ)、醛酮比(e)、醛碱比(β)、搅拌釜转速(n)等对原料转化率及反应产物H收率的影响。当醛酮比为1：4时,最佳反应条件为：温度40℃、醛碱比1：0.15、醛醇比1：10、搅拌桨转速1000 rpm、反应时间25 min。2、使用超重力组合反应器对缩合过程进行强化。当醛酮比为1：4时,最佳反应条件为：温度40℃、醛碱比1：0.10、醛醇比1：7.40、转子转速2840rpm、反应时间12 min。3、超重力组合反应器能加快反应速率,缩短反应时间,减少催化剂(减少33%)和溶剂(减少26%)使用量,将目标产物收率提高5%-10%。4、在搅拌釜反应器内研究了该缩合反应的宏观动力学。在本文的操作条件下,该反应符合拟一级动力学反应规律。指前因子为3.47×1010L·mol-1·min-1,表观活化能为60.99 kJ·mol-1,进一步推导出了该主反应的宏观反应动力学方程,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，

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