多级间歇分步结晶过程的研究

对间歇参数泵分步结晶过程进行了研究,此过程由结晶、发汗和熔化三步组成.研究表明,影响该过程的主要参数有鼓气速率、结晶降温速率、结晶时间、发汗升温速率及发汗时间等.在管长2m,内径50mm的结晶管内对萘-硫茚混合物进行了结晶发汗实验,取得上述因素对参数泵结晶过程的影响规律.     

熔融结晶法提纯对苯二胺

对粗对苯二胺用熔融结晶的方法进行提纯,考察了降温结晶速率、结晶终温、发汗升温速率、发汗终温对晶体纯度和产品收率的影响,并确定了最佳工艺条件:降温结晶速率为0.05℃/min,结晶终温为124℃,发汗升温速率为0.035℃/min,发汗终温为139℃。在最佳工艺条件下,通过单级熔融结晶从质量分数为92%的粗对苯二胺中得到纯度为99.5%以上的精对苯二胺,产品收率大于70%。     

氯酸钠真空结晶工艺粒度控制

氯酸钠晶体粒度是用户最为关注的一项质量指标。介绍了氯酸钠真空结晶的工艺过程;着重研究氯酸钠真空结晶工艺结晶机理及生产过程中影响晶体成核速率和晶体生长速率的各项因素。详细叙述了结晶区间、外循环速率、晶种、小循环方式对晶体成核速率的影响,以及结晶器内液位高度、液体密度、温度对晶体生长速率与生长时间的影响。得到了真空结晶工艺生产粒度较大且均匀的氯酸钠晶体的具体操作方案。     

熔融结晶法提纯2-氯-5-三氟甲基吡啶

对2-氯-5-三氟甲基吡啶使用熔融结晶的方法进行提纯,考察了结晶过程中的降温速率、结晶终温以及发汗过程中的升温速率、发汗终温等因素对产品收率和纯度的影响,并确定最佳工艺条件:降温结晶速率为0.071℃/min,结晶终温为16~19℃,发汗升温速率为0.062~0.083℃/min,发汗终温为28~30℃。在此条件下,通过单次结晶可得到纯度为99%的2-氯-5-三氟甲基吡啶产品。     

利用熔融结晶技术提纯对苯二甲酰氯

利用熔融结晶技术对粗对苯二甲酰氯进行提纯,考察了结晶终温、发汗终温、降温速率和升温速率对产品纯度和结晶收率的影响,最终确定最佳工艺条件为:降温速率为0.05℃/min,结晶终温为64℃,升温速率为0.1℃/min,发汗终温为76℃,所得产品纯度在99.8%以上。     

蒸馏-结晶耦合过程熔融结晶部分中发汗对产品纯度的影响

主要研究发汗在蒸馏.结晶耦合工艺中分离乙酸.氯苯共沸体系的应用.以发汗温度和发汗时间为工艺控制条件,通过对乙酸纯度、结晶率、发汗率,产品提纯能力等工艺参数的考察,来阐述发汗对于结晶过程的重要意义.通过实验得出最佳发汗温度为2℃,发汗时间为2.5 h.     

熔融分步结晶提纯L-丙交酯

以实验室制备的粗丙交酯为原料,采用熔融分步结晶法对提纯丙交酯进行了实验研究,考察了熔融分步结晶过程中结晶时间、结晶温差、发汗时间等参数对产品质量分数、结晶率、母液质量分数、组分收率以及提纯能力的影响,同时,对结晶和发汗过程的提纯能力进行了对比研究。结果表明:在给定的原料组成下,较适宜的结晶时间为60 min,结晶温差为20℃,发汗时间为50 min,发汗过程提纯能力是结晶过程的1.77倍。     

高纯对甲酚分步结晶控制系统软件开发

阐述了工业控制微机系统在千吨级对甲酚分步结晶装置中的应用，分析了对甲酚精制的加料、结晶、发汗和熔化等间歇过程的控制策略及软件设计方法。     

熔融结晶分离对硝基氯苯温度控制方案的设计与应用

介绍了对硝基氯苯熔融结晶分离的过程,并在结晶器温度控制方案中通过采用HONEYWELL公司的TPS系统的CL程序和RAMP/SOAK算法来满足熔融结晶的工艺控制要求,提高了结晶工序的控制性能.     

用精馏-降膜结晶耦合技术提纯对二氯苯

用精馏-降膜结晶耦合工艺分离对二氯苯。考察了降膜结晶操作中冷却剂温度、发汗升温速率对产品的影响,结果表明,冷却剂的温度为38℃,发汗速率为0. 5℃/min,可使w(对二氯苯)≥99 7%,单程收率>58%。与使用精馏工艺相比,总能耗下降71 7%。     

Effects of sweating time and cooling strategy on purification of N-vinyl-2-pyrrolidinone using a melt crystallizer

A melt crystallization process is proposed to produce high-purity n-vinyl-2-pyrrolidinone (NVP). To produce high purity products, operation strategy plays key role in the melt crystallizer. We investigated the cooling strategy and optimal sweating time using a batch-type melt crystallizer. A slow cooling followed by a slow heating was found to be an effective temperature profile to produce high purity of NVP. The optimal sweating time was found to be about 20 minutes. For industrial application, a cascade melt crystallizer which consists of four stages was constructed and the proposed crystallization/sweating scheme was applied. Using the new melt crystallizer, NVP more than 99.99% purity can be produced in semi-continuous mode.     

结晶法提纯N-乙烯基吡咯烷酮的工艺

对于应用于食品和医药等领域的N-乙烯基吡咯烷酮聚合物,要求N-乙烯基吡咯烷酮单体的纯度高于99.9%,但精馏法往往达不到要求。为了解决这个问题,本文采用结晶法对纯度为99.5%的工业级N-乙烯基吡咯烷酮进行提纯以制备纯度高于99.9%的医药级产品。考察了晶种添加量、晶种添加温度、降温速率、结晶终温、养晶时间、升温速率、发汗终温和发汗时间对最终产品的收率和纯度的影响,并确定了较为适宜的工艺条件：晶种添加量为原料质量的0.1%,晶种添加温度为11℃,降温速率为6℃/h,结晶终温为6℃,养晶时间为20min,升温速率为6~8℃/h,发汗终温为12℃,发汗时间为30min。在这些条件下通过单级结晶就可以将纯度为99.5%的N-乙烯基吡咯烷酮原料提纯至99.95%以上,收率大于74.5%。该方法相对其他分离方法具有较为明显的优势。     

具有静态混合单元的气泡分步结晶过程研究

在气泡分步结晶工艺基础上 ,开发了静态混合气泡结晶技术来提纯均四甲苯。实验表明 ,将静态混合单元引入传统气泡结晶器后 ,拓宽了有效鼓泡气速范围 ,明显改善了结晶过程气体均布及压强均布等状况 ,强化了传热、传质过程 ,提高了晶体纯度     

结晶分离技术新进展

概述了结晶分离理论和模拟优化的发展,综述了冷却剂直接接触冷却结晶、反应结晶、蒸馏-结晶耦合、氧化还原-结晶液膜、萃取结晶、磁处理结晶等结晶分离方法.合理设计结晶器及结晶工艺是实现结晶分离工业化的可靠保证,对降膜结晶装置、Bremband结晶工艺和板式结晶器进行评价.指出今后需深入进行新型结晶分离装置与工艺、工艺的工业化、结晶过程传热传质机理方面的研究.     

低温控温结晶法分离提纯1,8-桉叶油素的工艺

采用全结晶工艺对原料桉叶油[w(cineole)=63.24%]进行分离提纯,在无晶种添加下,降温速率4℃/h、结晶终温-30℃、发汗速率5℃/h、发汗终温-19℃时,可将原料油提纯至77.52%。添加晶种后,可有效提高操作温度,缩小结晶温度的操作范围,提高产品的纯度,在降温速率4℃/h、结晶终温-25℃、发汗速率4℃/h、发汗终温-6℃的操作条件下,将原料油提纯至89.63%。实验得到了低温控温添加晶种结晶法分离提纯1,8-桉叶油素的适宜工艺流程和操作参数,该方法相对其他分离方法具有较为明显的优势。     

A process development for the bundling crystallization of aspartame

It is known that rod-like crystals of aspartame, in which several needle crystals appear to be bundled together (bundle-like crystals), have remarkably improved physical properties compared to the crystals obtained from a conventional stirred crystallizer. A crystallization process for obtaining bundle-like crystals has been developed for manufacturing practice. The conditions to obtain the bundle-like crystals are that crystallization must be carried out without stirring, with a high initial concentration of aspartame so that the amount of precipitated solid after cooling is about 10 g litre^?1 or more, and with rapid cooling to produce high supersaturation. A new type of crystallizer was developed for large-scale crystallization under these conditions. The pilot plant work was carried out in a 400-litre crystallizer, and it has been demonstrated that the crystallization process is technically possible and economically successful in the large-scale manufacturing of aspartame.     

降膜结晶分离技术实验研究

采用萘－硫茚物系对新型高效降膜结晶技术的分离提纯机制进行了实验研究．考察了管外降膜结晶过程中结晶时间、料液流量、冷却水初始进口温度、冷却水降温速率及原料浓度对分离提纯效果的影响．实验发现降膜结晶过程中晶层生长并不完全是光滑界面的生长,而在某些条件下表现为粗糙界面的生长,即生长过程在某些条件下表现为两相区界面的生长．进一步对辅助提纯－发汗过程的工艺参数—发汗时间、发汗初始浓度的影响进行了实验研究．实验结果可用于降膜结晶传热传质机理的数值模拟．     

Product quality improvement of batch crystallizers by a batch-to-batch optimization and nonlinear control approach

Batch crystallization is one of the widely used processes for separation and purification in many chemical industries. Dynamic optimization of such a process has recently shown the improvement of final product quality in term of a crystal size distribution (CSD) by determining an optimal operating policy. However, under the presence of unknown or uncertain model parameters, the desired product quality may not be achieved when the calculated optimal control profile is implemented. In this study, a batch-to-batch optimization strategy is proposed for the estimation of uncertain kinetic parameters in the batch crystallization process, choosing the seeded batch crystallizer of potassium sulfate as a case study. The information of the CSD obtained at the end of batch run is employed in such an optimization-based estimation. The updated kinetic parameters are used to modify an optimal operating temperature policy of a crystallizer for a subsequent operation. This optimal temperature policy is then employed as new reference for a temperature controller which is based on a generic model control algorithm to control the crystallizer in a new batch run.