非均相光催化水处理管式反应器的放大设计

研究了非均相光催化反应器在放大过程中光辐射能衰减和流体返混对其放大过程设计的影响。结果表明,光辐射能随着光源和反应管的中心距的增加急剧衰减,两者呈1 56次方反比关系;管式反应器中流体的返混程度远小于相同反应体积的环型反应器,这有利于提高水中有机污染物的降解率。建立了一套由3组管式反应器串联且光接触面与光源的距离小于10cm的连续光催化水处理中试装置,并对印染废水进行处理。化学需氧量可从150～180mg/L降至50mg/L以下,处理量为50L/h时的出水优于国家一级排放标准。     

On Improving Scale-Up Procedures for Dense-Phase Pneumatic Conveying of Powders

This article presents results of an ongoing effort toward improving the modeling and scale-up procedures for the dense-phase pneumatic conveying of fine powders through pipes. Two new approaches are employed in this study. One approach, derived by modifying an existing reliable dilute-phase model to make it suitable for the dense-phase, has resulted in relatively stable predictions for diameter and length scale-up for two types of fly ash, ESP dust, pulverized brown coal and fly ash/cement mixture. Although some over-predictions still remain for the cases of diameter scale-up, there seems to be a substantial relative improvement in the overall accuracy of predictions (compared to the existing design methods). Another method has been derived using the concept of “two-layer” slurry flow modeling (suspension flow occurring on top of a non-suspension moving layer), and this has also resulted in similar improvements. Although the “two-layer” technique is believed to be more representative of the actual flow conditions under dense-phase conveying, the simpler “modified” method appears to be adequate for practical design purposes.     

4-氯代邻苯二甲酸酐合成的中试研究

以苯酐为原料,水为介质,先用氢氧化钠中和生成邻苯二甲酸单钠盐,再向混合体系通氯气,亲电取代得纯度大于72%(HPLC)的4-氯邻苯二甲酸单钠盐.然后经酸化、脱水、精馏.中试规模制备了纯度大于98.5%(HPLC)的4-氯邻苯二甲酸酐.探索了反应条件对转化率和选择性的影响.结果表明,最佳反应条件为:体系的pH 4.5～5.5、水/苯酐质量比2.0～2.2、反应温度55～65℃、通氯速度30～50 L/min,反应时间180～220 min.苯酐转化率84.4%,总收率50%～60%.     

中试规模合成青霉烯和碳青霉烯类抗生素关键中间体4-AA

该文研究了青霉烯和碳青霉烯关键中间体4-AA的生产工艺。在-5℃,L-苏氨酸与亚硝酸钠、盐酸、氢氧化钠发生重氮化、分子内亲核取代反应生成(2R,3R)-2,3-环氧丁酸(中间体A),收率74.5%。A再与对甲氧苯氨基乙酸乙酯(中间体B)反应5～6 h制得(2R,3R)-N-乙氧羰甲基-N-(4-甲氧基苯基)-2,3-环氧丁酰胺(中间体C),收率94.3%。中间体C在六甲基二硅氮烷、氨基锂作用下环合成(3S,4S)-3-[(1R)-1-羟乙基]-4-乙氧羰基-1-对甲氧苯基-2-氮杂环丁酮(中间体D),收率72.1%。最后中间体D经羟基保护、水解、氧化脱羧、臭氧化脱保护基制得4-AA{(3R,4R)-3-[(1R)-叔丁基二甲基硅氧乙基]-4-乙酰氧基-2-氮杂环丁酮}。总收率达到34.5%,4-AA液相色谱纯度达到99.34%。     

反胶团法制备ZrO2超细粉末过程的放大模型

使用喷射 -搅拌混合器 ,使油水两相可以快速而且充分接触 ,从而利用反胶团法得到粒度分布均匀的ZrO2 超细粉末 .首先利用模型预测了不同转速和不同相比下两相传质的结果 ,然后用实验验证了模型的准确性 ,建议利用该模型进行放大研究     

橡胶防老剂4020合成新工艺的工业化研究

以研究成功的橡胶防老剂4020合成新工艺的小试和中试条件为依据,完成了工业化生产的研究。在常压下从较小的分子出发,即以对氨基苯酚、甲基异丁基酮、甲酸、苯胺为原料,分3步反应合成4020。用两台反应釜并联,差时半个生产周期分别开动,用一台同体积的蒸馏釜与之配套,实现了节省时间的最佳组合,同时减少了其它配套设备的尺寸和投资。在3台釜中都加入冷却蛇管,大大缩短了冷却时间。生产过程安全平稳,产品收率达90 1%,为4020的工业化生产提供了一条新的途径。     

Scale-up of functional properties of pressure-sensitive adhesive from laboratory to industrial plant production: from monomers to label

A waterborne acrylic pressure-sensitive adhesive produced in a commercial plant to label market was successfully developed. In order to reach the required functional properties (i.e. holding time, peel, and loop tack strengths), glass transition temperature, functional monomer content, type of surfactant, and reaction temperature were optimized. A proper balance of wetting and thickening agents content was found taking into consideration their significant unfavorable effect on functional properties.     

Study of granule growth kinetics during in situ fluid bed melt granulation using in-line FBRM and SFT probes

Objective: The aim of this work was to study the granule growth kinetics during in situ fluid bed melt granulation process using real-time particle size measurement techniques. In addition, the usefulness of these techniques during scale-up of melt granulation was evaluated.

Materials and methods: Focused beam reflectance measurement (FBRM) and spatial filtering technique (SFT) probes were used within the process chamber of fluid bed granulator for real-time in-line granule size analysis.

Results: The results demonstrated that the use of in-line particle size probes in fluid bed granulator during the process offers an insightful view of granule growth and allows in-process monitoring of granule chord length changes. The effect of selected critical parameters (binder content, inlet air temperature and product endpoint temperature) on the granule growth was clearly presented by in-line measurements in a laboratory scale. A comparison of granule size measurements from both FBRM and SFT probes showed similar particle growth trends, which were in close correlation to the product temperature. Comparable trends in end granule particle size were observed when comparing different in-line, at-line and off-line particle size measurements.

Conclusion: The in-line FBRM and SFT probes were successfully employed in in situ fluid bed melt granulation process to study the influence of critical formulation/process parameters on the granule growth kinetics. The scale-up experiment confirmed the potential of these in-line granule size measurement techniques as a viable tool for process monitoring during the transfer of granulation to the larger scale or another manufacturing site/equipment.     

Hot-melt extrusion – basic principles and pharmaceutical applications

Originally adapted from the plastics industry, the use of hot-melt extrusion has gained favor in drug delivery applications both in academia and the pharmaceutical industry. Several commercial products made by hot-melt extrusion have been approved by the FDA, demonstrating its commercial feasibility for pharmaceutical processing. A significant number of research articles have reported on advances made regarding the pharmaceutical applications of the hot-melt extrusion processing; however, only limited articles have been focused on general principles regarding formulation and process development. This review provides an in-depth analysis and discussion of the formulation and processing aspects of hot-melt extrusion. The impact of physicochemical properties of drug substances and excipients on formulation development using a hot-melt extrusion process is discussed from a material science point of view. Hot-melt extrusion process development, scale-up, and the interplay of formulation and process attributes are also discussed. Finally, recent applications of hot-melt extrusion to a variety of dosage forms and drug substances have also been addressed.