SSP装置制备结晶切片工艺优化

为使产品的黏度短时间达到要求的范围,以及防止切片在主反应器内发生结块现象,针对制备结晶切片的工艺过程进行了优化。经过工艺优化有效减少了物料降等数量,提高了切片结晶度,缩短了装置开车时间。     

杀虫单结晶工艺的优化初探

研究了－10℃和50℃下杀虫单－氯化-水三元体系相图,根据获得的相平衡结果,对现有杀虫单生产工艺提出了改进措施,同时考察了添加剂对杀虫单结晶形态的影响。工业实验表明,采用本文提出的改进措施,杀虫单产率和产品质量都有较大的提高。     

盐酸林可霉素结晶工艺研究

探索盐酸林可霉素共沸结晶工艺,与丙酮结晶工艺进行对比研究。     

头孢拉定连续结晶工艺研究

采用三级混合悬浮混合产品出料结晶器(MSMPR),搭建了头孢拉定连续结晶实验装置。通过单因素实验研究了养晶pH值、晶种添加量、原料液浓度、停留时间、结晶系统温度及搅拌速率等结晶工艺条件对头孢拉定连续结晶产品收率及粒度分布的影响,优化了头孢拉定连续结晶工艺参数。通过实验获得优化结晶工艺参数：结晶温度293.15 K,搅拌速率180 r·min^-1,养晶pH=2.85,晶种添加量为3%(质量分数),头孢拉定原料液浓度11%(质量分数),停留时间33.3 min,此条件下可以获得平均粒径为85.3μm,收率为76.53%的头孢拉定连续结晶产品。     

衣康酸精制品结晶工艺研究

通过结晶基本理论分析，在工业装置上对精制品衣康酸结晶过程进行了研究，得到了结晶降温控制优化工艺方案。     

响应曲面法优化碳酸锂反应结晶工艺

碳酸锂是制备各种锂化合物的基础锂盐,碳酸锂的制备是锂产业链当中的承前启后的关键技术。以察尔汗盐湖老卤为原料,采用响应曲面法中的central composite design（CCD）设计实验,分别考察了温度、碳酸钠加料速度、碳酸钠浓度和锂离子浓度4个因素及交互作用对反应结晶工艺中碳酸锂的收率和粒度的影响,并分别建立了响应值与影响因素之间的回归方程。响应预测最佳值为：碳酸锂收率93.68%、粒径（d₅₀）16.73 μm;相应的实验值分别为94.01%和16.91 μm。预测值与实验值接近,误差较小,说明响应曲面法建立的预测碳酸锂反应结晶的模型可靠,在最佳工艺条件下分析所制得的产品,用ICP-AES分析纯度为99.52%,用XRD分析基本无杂峰,说明反应结晶生成Li₂CO₃晶体,其主要晶面为（-1 1 0）、（-2 2 0）和（0 0 2）。     

动态熔融结晶工艺

浅谈动态熔融结晶特点及其工艺过程和工艺原理。     

超声在结晶中的应用与进展

超声结晶是一种新的结晶分离技术,将超声应用到结晶过程可以产生显著的效果。引入超声可以缩短诱导期,促进成核,降低结晶产品的粒径;在有的体系中还会影响结晶收率,晶形,产品的流动性等。文章综述了超声结晶在无机盐、制药、食品领域的应用以及研究进展。     

水合氯醛结晶工艺研究

对水合氯醛结晶工艺进行了研究,经实验确定了水合氯醛结晶的最佳工艺条件,获得了符合“BP93”标准的水合氯醛产品,产率达85％左右,结晶时间约为3．5h。     

美伐他汀结晶纯化工艺研究

目的:分析并总结优化美伐他汀提取工艺.方法:以相同质量美伐他汀粗品为原料,采用丙酮、乙酸乙酯、乙醇和异丙醇4种溶剂结晶.结果:脱水美伐杂质去除效果顺序为乙酸乙酯>丙酮>乙醇>异丙醇;双氢美伐杂质去除效果顺序为异丙醇>乙醇>乙酸乙酯>丙酮;低温浸泡(≤5℃)去除蛋白效果较好.结论:综合考虑应选择异丙醇溶剂作为结晶溶剂;在...     

果糖结晶过程优化

通过实验筛选得到适合果糖结晶的混合溶剂,利用中通量结晶仪器Crystalline测定了果糖在水-乙醇（水的摩尔分数为0.39）混合溶剂中的溶解度和介稳区,采用Apelblat方程拟合了溶解度数据。基于热力学数据设计了晶种引晶的果糖冷却结晶工艺,过程优化得到的产品收率可达78.2%以上,纯度可达99%以上,晶体形貌规则,表面光滑,粒度分布窄。当晶体粒径大于100 μm时,利用粒度无关生长的粒数衡算方程建立了果糖连续结晶过程的动力学模型,模型表明晶体生长级数大于成核级数。     

Optimization and control of crystal shape and size in protein crystallization process

Large molecule protein crystals have shown significant benefits in the delivery of biopharmaceuticals to achieve high stability, high concentration of active pharmaceutical ingredients (API), and controlled release of API. However, among the about 150 biopharmaceuticals on the market by 2004, only insulin has been marketed in crystalline form. A major technological challenge is that protein crystallization has a very complicated environment and is affected by many factors. There is currently a lack of knowledge on large scale production of protein crystals. In contrast to the majority of previous work on protein crystallization that was centered on single crystal scale, the current research is focused on computational study of protein crystallization at process scale, investigating the growth behavior of a population of crystals in a crystallizer. Using a newly developed morphological population balance model that can simulate the multidimensional size distributions of a population of crystals, known as shape distribution, an optimization technique is applied to optimize the growth of individual faces with the aim of obtaining desired crystal shape and size distributions. Using a target shape as the objective function, optimal temperature and supersaturation profiles leading to the desired crystal shape were derived. Genetic algorithm was investigated and found to be an effective optimization technique for the current application. Since tracking an optimum temperature or supersaturation trajectory can be easily implemented by manipulating the coolant flowrate in the reactor jacket, the methodology provides a feasible closed-loop mechanism for protein crystal shape tailoring and control.     

舒巴坦钠溶析结晶工艺优化

目前舒巴坦钠粗品的提纯采用还原成舒巴坦酸后再经反应结晶合成舒巴坦钠的方式,耗时耗力且所需药品、试剂种类较多,不节能环保。针对该问题,采用正交实验 L_{27} \left(3^{13}\right) 对舒巴坦钠的溶析结晶工艺进行优化,探明了6个因素6个交互作用对粒度、纯度以及两者的综合评分的影响,包括养晶时间（A）、溶析剂用量（B）、溶析剂中乙醇的体积分数（C）、溶析剂的滴加速率（D）、搅拌速率（E）、温度（F）以及养晶时间分别与溶析剂用量（A×B）、与溶析剂中乙醇的体积分数（A×C）的交互作用、溶析剂用量与溶析剂中乙醇的体积分数的交互作用（B×C）,并得到了一组最优方案A ₂ B ₂ C ₁ D ₃ E ₃ F ₂。通过该方案可获得纯度x>97%,体积平均粒度D[4,3]≈290μm,质量收率约为84%的舒巴坦钠产品,并发现杂质舒巴坦青霉胺对舒巴坦钠的粒度分布有一定的影响。在解决原有问题的基础上,合适粒度分布的舒巴坦钠产品也可为后续制剂工艺提供方便。     

制药结晶中的先进过程控制

结晶作为固-液分离的重要手段,是实现医药产品高端高值化的关键技术。药物结晶过程的精准控制决定了晶体产品的多晶型、晶习、粒度及粒度分布等诸多特性,对生产效率和产品质量的提升具有重要的意义。基于国内外对药物结晶过程控制的研究现状,结合相关案例,系统总结了制药结晶中先进过程控制的理论模型、监测手段和控制策略,重点分析讨论了过程控制在产品工程中的应用并对其发展趋势进行了展望。     

高效膜蒸馏结晶过程的研究进展

全球性的水资源短缺及环境污染问题,使得工业废水处理、海水淡化、高价值溶质综合利用的需求日益迫切。膜蒸馏结晶过程可以充分利用低品质热源,实现高纯度水溶剂分离、盐分结晶制备,对于实现分离过程零排放和协同增效有重要意义。同时,膜蒸馏结晶也可以与多级闪蒸,多效精馏、纳滤、正向渗透、反渗透等过程进行耦合,进一步提高整体分离效率。此外,该过程对于调控晶体外部形貌,制备晶体尺寸分布集中、流动性好的晶体产品也有积极作用。基于此,针对膜蒸馏结晶原理、过程调控机制以及创新过程应用几个方面开展论述,总结了膜蒸馏结晶技术在高效分离、结晶过程精准控制等领域的关键问题和发展趋势。     

Research progress of high-efficiency membrane distillation crystallization process

The global shortage of water resources and environmental pollution has made the demands for industrial wastewater treatment, seawater desalination, and comprehensive utilization of high-value solutes increasingly urgent. Membrane distillation crystallization process cannot only make full use of low-quality heat sources, achieve high-purity water-solvent separation, but also achieve salt crystallization preparation, which is of great significance for achieving zero liquid discharge and synergistic efficiency in the separation process. At the same time, membrane distillation crystallization process can also be coupled with multi-stage flash evaporation, multi-effect distillation, nanofiltration, forward infiltration, reverse osmosis and other processes to further improve the overall separation efficiency. In addition, it also has a positive impact on regulating the external morphology of the crystal, preparing crystal products with relatively concentrated crystal size distribution and good flowability. Based on this, this article has discussed several aspects of membrane distillation crystallization principles, process control mechanisms and innovative process applications, and looking forward to the key issues and development trends of membrane distillation crystallization technology in the fields of efficient separation and precise control of the crystallization process.     

结晶精制技术进展

考虑到节能、环保等问题，结晶技术在有机混合物的分离和精制中得到广泛应用。特别是熔融结晶，已引起人们的重视。文中介绍了结晶研究和技术发展概况，以及几种新型的结晶精制装置。     

基于层次分析法优化天然气净化工艺

为了避免杂质腐蚀设备或因低温冻结而堵塞换热器,天然气在进入液化装置前需对其进行净化处理,即脱除天然气中的酸性气体(CO₂、H₂S)和水分。本文选用二乙醇胺(DEA)法脱除天然气中的酸性气体,用三甘醇(TEG)法脱除天然气中的水分,通过耦合DEA法和TEG法得到最终天然气净化工艺,且达到净化指标要求。但由于工程手册只能给出工艺参数的大概范围,尚无法得到最优的工艺方案,因此本文首先应用化工模拟软件HYSYS8.4对天然气工艺过程进行模拟计算,然后在工艺参数推荐范围内设定9组推荐方案,引入系统评价方法中的层次分析法,并基于Matlab程序计算,对9组推荐方案进行多目标综合评价,最终确定最优的净化组合方案。本文可为天然气净化工艺和其他工艺方案的优选提供指导。     

核黄素结晶母液的处理及回收利用

发酵法生产核黄素会产生大量的结晶母液,很难处理。本文首先采用聚丙烯酰胺对结晶母液进行絮凝沉降处理,确定了最佳投料量200mg/L,最优pH 5~6,母液中的化学需氧量（COD）去除率达60%以上。絮凝沉降物采用喷雾干燥法进行回收,对几个主要参数进行了优化,得到了最佳操作参数：进风温度190℃,进样流速3mL/min,β-环糊精添加量1%,产品得率66.95%,含水率2.9%,有效减小了对环境的影响。     

Optimization of solvent crystallization process in obtaining high purity anthracene and carbazole from crude anthracene

Solvent crystallization is the main method used for preparing anthracene and carbazole from the crude anthracene. The key to the optimization of this method is improving the solubility selectivity of the solvent by means of solvent modulating and process optimization. In this study, the solubility of anthracene, phenanthrene, and carbazole in xylene, dimethylformamide (DMF), DMF with amine/amide, isopropanolamine, and chlorobenzene is examined and the solid‐liquid ternary anthracene–carbazole–DMF/(DMF+19.96% isopropanolamine) system phase diagram is determined and applied in the solvent crystallization process. The results showed that the solubility selectivity of xylene increases with increased temperature. Also, selectivity increases with an increase of the amount of isopropanolamine in the mixture of DMF and isopropanolamine, while decreases with increased temperature. Through multiple washings of crude anthracene with xylene, DMF+19.96% isopropanolamine, and chlorobenzene, it was possible to obtain anthracene and carbazole of purity higher than 98 wt %. © 2013 American Institute of Chemical Engineers AIChE J, 60: 275–281, 2014