【作者】 王国锋；

【导师】 黄国强；

【作者基本信息】 天津大学 ， 化学工程， 2012， 硕士

【摘要】 针对目前国内多晶硅行业内日益突出的氯硅烷低沸物富集问题，本文在充分调研国内外文献资料基础上，改进原有工艺，利用氯硅烷反歧化反应精馏处理多晶硅生产中产生的氯硅烷低沸物。通过流程模拟计算、设计和工业化应用，达到了理想的效果。本研究从催化剂的对比、优选和预处理工艺着手，从五种催化剂中选取出一种可靠性高、性能优良且价格合理的催化剂。以国内某多晶硅企业的实际需求为目标，在流程模拟计算的基础上，设计了整套工艺，并将利旧设备改造利用，成功工业化运行，操作稳定且DCS转化率超过98.5%，达到预想效果。在已有模拟计算和工业生产数据的基础上，讨论相关设计和操作参数对工艺的影响，包括捆扎包单板持液量、反应段理论板数、精馏段提馏段理论板数、STC和DCS进料位置、STC循环量和STC循环温度。通过分析，当DCS处理量为300kg/h时，确定最优操作条件为捆扎包单板持液量100L，反应段理论板数8块，精馏段提馏段理论板数均12块，STC位于反应段上部进料，DCS位于反应段下部进料，STC循环量控制在4000-8000kg/h，STC循环温度为30℃。在此条件下可以达到节能高效的生产效果。氯硅烷反歧化反应精馏工艺仍存在一定缺陷。本研究考虑将反应精馏与隔板精馏相结合，进一步优化工艺。通过对氯化亚砜物系隔板精馏提纯案例的分析，初步掌握隔板精馏塔的设计思路，在此基础上对氯硅烷反歧化隔板反应精馏塔进行了模拟计算，效果良好，可指导后续的改进工作。更多还原

【Abstract】 Enrichment of low boiling chlorosilane has become increasingly prominent indomestic polysilicon industry. This work would deal with low boiling chlorosilane byredistribution reactive distillation, based on a large number of literature and collectioninformation, to improve the original process. Ideal results have been achieved byprocess simulation, design and industrial applications.This study begins from the comparison, selection and pretreatment of catalyst. Akind of catalyst is selected from five because of its high reliability, excellentperformance and affordable. In order to meet the need of some domestic corporation,the process is designed and industrialized successfully based on simulation,modifying the old equipments. Stable operation and more than98.5%DCSconversion indicate desired effect.On the basis of the existing simulation and industrial data, the effect of designand operating parameters on the process is discussed, including liquid holdup per tray,number of theoretical trays in reaction, rectifying and stripping section, STC and DCSfeeding location, the STC circulation rate and temperature. By analyzing, when thetreatment capacity of DCS is300kg/h, optimal operating conditions are determinedas that liquid holdup per tray is100L, theoretical trays of reaction section is8, whichis both12for rectifying and stripping section, STC is fed in the upper part of thereaction bed, and DCS lower part, STC circulation rate is controlled in4000-8000kg/h, and temperature30℃. Energy saving and efficient production can be achievedunder these conditions.Chlorosilane redistribution reactive distillation process still has some defects. Inthis study, reactive distillation and dividing wall column are considered to combinefor further optimizing. The idea of dividing wall column design is initially studied byanalysing the case of thionyl chloride purification by dividing wall column. Thensome simulations of chlorosilane redistribution reactive dividing wall column aredone on this basis, and the good results can guide the subsequent improvement work.更多还原