折流式旋转床（RZB）微观混合和液—液传质性能及其应用研究

发布时间：2018-07-02 10:44

本文选题：折流式旋转床 + RZB　；参考：《浙江工业大学》2017年硕士论文

【摘要】：作为最受关注的过程强化技术之一,超重力技术已经成为化学工程学科研究的前沿和热点方向之一。与普通的旋转填料床相比,折流式旋转床具有诸多优点。其中,独特的动静转子结构有利于改善液体进口处的“端效应区”,使得折流式旋转床具有更优异的微观混合性能和液-液传质强化性能,使其在“受传质和分子混合限制”的化学反应制备化学品的应用领域具有巨大潜力。本文从折流式旋转床的微观混合和液-液传质强化两个特性研究出发,开展实验研究,并且第一次将其应用于羟醛缩合制备化学品的过程强化中。主要工作和研究结果如下:1、采用碘化物-碘酸盐平行竞争反应体系,对折流式旋转床(RZB)的微观混合性能进行研究,分别考察了超重力因子β、液体入口总流量uin、H+浓度、反应物体积流量比VA/VB对RZB反应器离集指数Xs的影响;并与三通混合装置、旋转填料床(RPB)对离集指数Xs的影响进行对比。实验结果表明:在本实验范围内,折流式旋转床实验所得到的离集指数XS在0.01~0.05之间,显示出了较三通混合装置优越的微观混合性能;另外,由实验结果可知RZB反应器的微观混合性能略优于RPB反应器。2、以大豆油-异丙醇-水为实验体系,研究了折流式旋转床(RZB)强化物理萃取传质的性能。考察了超重力因子β、液体入口总流量uin和水油两相体积流量比?等主要操作参数对萃取级效率η影响;并在相同操作条件下,进一步探究了折流式旋转床(RZB)萃取传质性能与微观混合性能之间的定量关系。实验结果表明:对比于传统搅拌萃取装置,折流式旋转床萃取性能更加优异。它能够使液滴粒径瞬间达到微米级水平,具有优异的微观混合特性,能有效的强化物理萃取传质过程。在折流式旋转床(RZB)反应器内,萃取传质性能与微观混合性能密切相关。在实验操作条件下,超重力因子β逐渐增加到263时,离集指数Xs减小为0.020,对应的萃取级效率η逐渐增加到94.2%,萃取级效率η随离集指数Xs的减小而逐渐增加,说明随RZB着反应器微观混合效果的提高,萃取传质效果也逐渐提高,但两者并不呈线性关系。3、采用异戊醛和丙酮进行羟醛缩合反应制备甲基庚烯酮的生产工艺,将折流式旋转床反应器用于强化反应过程。考察了超重力因子β、反应温度T、碱浓度?和异戊醛与丙酮物质的量比?等操作条件对异戊醛转化率X、甲基庚烯酮选择性S和收率Y的影响,并对目的产物甲基庚烯酮(MHK)进行了核磁共振氢谱(1H-NMR)、核磁共振碳谱(13 CNMR)和GC-MS的表征,以确定其分子结构。实验结果表明:RZB反应器可以有效强化异戊醛和丙酮羟醛缩合反应,当碱性催化剂用量为物料的40%,循环流量为150L/h时,控制适当温度和异戊醛丙酮物质的量比,碱性催化剂浓度为4.2%,超重力因子为263时,异戊醛转化率为88.6%,甲基庚烯酮的选择性和收率分别达到93.3%和82.7%。相同操作条件下,与机械搅拌装置强化效果对比,RZB反应器强化下的异戊醛转化率提高了20%,选择性提高了30%。
[Abstract]:As one of the most concerned process strengthening techniques, supergravity technology has become one of the frontiers and hot topics in the research of chemical engineering. Compared with the ordinary rotating packed bed, the baffled rotary bed has many advantages. The rotary bed has a more excellent micro mixing performance and liquid liquid mass transfer enhancement. It has great potential in the application field of chemical reaction preparation of "mass transfer and molecular mixing restriction". In this paper, two characteristics of micro mixing and liquid to liquid mass transfer enhancement in a baffled rotating bed are studied, and the experimental study is carried out. The main work and research results are as follows: 1, the micro mixing properties of the RZB are studied by the iodide iodate parallel competitive reaction system, and the supergravity factor beta, the total flow rate UIN, H+ concentration and the reaction object are investigated. The effect of VA/VB on the off set index Xs of the RZB reactor and the effect of the three pass mixing device and the rotating packed bed (RPB) on the off set index Xs are compared. The experimental results show that in the experimental range, the off set index XS obtained by the baffle rotary bed experiment is between 0.01~0.05, which shows the superior microstructure of the three pass mixing device. In addition, the experimental results show that the micro mixing performance of the RZB reactor is slightly better than that of the RPB reactor.2. With the soybean oil isopropanol water as the experimental system, the properties of the mass transfer in the physical extraction of the baffled rotating bed (RZB) are studied. The supergravity factor beta, the total flow rate UIN of the liquid inlet and the volume flow ratio of the water and oil two phase are investigated. The effect of the operating parameters on the extraction efficiency was investigated. The quantitative relationship between the mass transfer performance and the micro mixing performance of the RZB was further investigated under the same operating conditions. The experimental results showed that the performance of the baffled rotary bed was better than that of the traditional stirred extraction device. At the micron level, with excellent micro mixing characteristics, it can effectively strengthen the mass transfer process of physical extraction. In a baffled rotary bed (RZB) reactor, the mass transfer performance is closely related to the micro mixing performance. Under the experimental operating conditions, the supergravity factor beta is gradually increased to 263, the off set index Xs is reduced to 0.020, the corresponding extraction grade The efficiency ETA gradually increased to 94.2%, the extraction efficiency was gradually increased with the decrease of the separation index Xs, indicating that the mass transfer effect of the extraction was gradually increased with the increase of the micro mixing effect of the RZB reactor, but they did not have a linear relationship.3. The production process of methyl heptanone by isovalaraldehyde and acetone was used to prepare methyl heptanone. The flow type rotating bed reactor was used to strengthen the reaction process. The effects of the supergravity factor beta, the reaction temperature T, the concentration of the alkali and the ratio of the isovalaraldehyde to acetone were investigated, such as the conversion of isovaleral X, the selective S of methyl hepenone and the yield Y, and the nuclear magnetic resonance hydrogen spectrum (1H-NMR) was carried out for the target product of methyl heptanone (MHK). The molecular structure of the magnetic resonance carbon spectrum (13 CNMR) and GC-MS is determined. The experimental results show that the RZB reactor can effectively strengthen the condensation reaction of Isoamyl aldehyde and acetone hydroxyaldehyde. When the amount of the basic catalyst is 40% of the material and the circulation flow is 150L/h, the ratio of the appropriate temperature to the isovalaraldehyde acetone is controlled, and the concentration of the alkaline catalyst is 4.2%, When the supergravity factor was 263, the conversion rate of isovaleral was 88.6%. The selectivity and yield of methyl hepenone were 93.3% and 82.7%., respectively, under the same operating conditions, compared with the mechanical agitator, the conversion of isovaleral under the RZB reactor was increased by 20%, and 30%. was selectively raised.
【学位授予单位】：浙江工业大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TQ051.1

【参考文献】