【作者】 邵利；

【导师】 周明；

【作者基本信息】 天津大学 ， 化学工程， 2006， 硕士

【摘要】 以甲缩醛催化精馏合成技术为研究背景,在总结催化精馏塔结构、模型与模拟方法的基础上,本文提出了浆料催化精馏制备甲缩醛的新工艺,浆料催化精馏将催化剂磨成微粒或超微颗粒,使其与液相形成浆料在塔内流动,并循环使用。本文采用细粉状的强酸性阳离子交换树脂做催化剂,在内径为76mm的玻璃复合塔内,对浆料催化精馏工艺制备甲缩醛进行了实验研究,考察了这一新工艺的可行性。本文考察了回流比、催化剂浓度、进料总流量和进料醇醛比等条件对浆料催化精馏过程的影响。实验结果表明:回流比对甲缩醛收率和塔顶甲缩醛纯度的影响不同于一般的精馏过程,存在一个最优回流比,本过程最佳回流比在1-2之间;提高催化剂浓度,甲缩醛收率和塔顶甲缩醛纯度均增加;提高进料醇醛摩尔比也会提高甲缩醛收率;进料总流量对甲缩醛的收率的影响十分明显,进料总流量减少可以使甲缩醛的收率得到明显提高。采用平衡级模型,应用Aspen Plus软件对实验过程操作参数及塔内各参数对过程的影响进行模拟,模拟结果与实验结果吻合较好。结果揭示了过程各参数在塔内的变化规律,及塔内各参数对过程的影响规律,为今后工艺和塔的设计提供依据。最后,对浆料催化精馏工艺在缩合反应中的应用前景进行了探讨。与普通的催化精馏相比,浆料催化精馏具有不需要制作催化剂原件、不需要停车更换催化剂、不需要固液分离、催化剂效率高和易于工业化生产等优点,具有很好的研究与开发的前景。更多还原

【Abstract】 On the basis of the research of synthesis of methylal with catalytic distillation and reviewing tower structures, models and simulation methods for catalytic distillation process, a novel technology of preparation of methylal with slurry catalytic distillation was studied in this paper. A fine particulate catalyst is slurried in one of the reactant streams and fed into a distillation column reactor and is recycled. In this paper, the slurry catalytic distillation process was experimentally studied on the preparation of methylal from methanol and formaldehyde and the feasibility of this novel technology was studied. The experiments were carried out in a glass column with an inner diameter of 76mm and the catalyst was particle of acidic cation ion-exchange resin.The effects of reflux ratio, catalyst concentration, feed mole ratio of methanol to formaldehyde and total feed flow on the process were experimentally investigated. The experiment results indicate that: the increases of catalyst concentration, feed mole ratio of methanol to formaldehyde and the decrease of total feed flow can increase the yield of methylal; the concentration of methylal in distillate also increases with the increase of catalyst concentration; that the effects of reflux ratio on the yield and concentration of methylal in distillate are different from conventional distillation process, an optimal value of reflux ratio exists between 1 and 2 for this process.Based on equilibrium stage model, the effects of parameters of operation and tower on process were simulated by using Aspen Plus software. The simulation results show that the calculated results agree satisfactorily with the experiment data, and provide also the basis for designing process and column of slurry catalytic distillation.Compared with conventional catalytic distillation, slurry catalytic distillation holds more advantages, such as: simpler column structure, easier to operate and control, higher efficiency of reaction and separation, more suitable to large scale production, etc. The slurry catalytic distillation process is worth researching and developing.更多还原