离子液体溴代1-丁基-3-甲基咪唑盐合成的红外光谱分析

本实验建立以红外光谱法,利用特征吸收频率处的红外吸收率测得合成离子液体1-丁基-3-甲基咪唑六氟磷酸盐的中间产物溴代1-丁基-3-甲基咪唑盐的含量,应用于探索1-丁基-3-甲基溴代咪唑盐合成的最佳反应条件,结果表明反应温度为65℃,时间50分钟时产物得率高。     

离子液体溴代1-丁基-3-甲基咪唑盐合成的红外光谱分析

本实验建立以红外光谱法,利用特征吸收频率处的红外吸收率测得合成离子液体1-丁基-3-甲基咪唑六氟磷酸盐的中间产物溴代1-丁基-3-甲基咪唑盐的含量,应用于探索1-丁基-3-甲基溴代咪唑盐合成的最佳反应条件,结果表明反应温度为65℃,时间50分钟时产物得率高.     

桐油酸咪唑啉衍生物的合成及其缓蚀性能

桐油能自干成膜但水溶性差,在缓蚀剂中的应用有局限性。为此,以桐油为原料合成了桐油酸,将其与二乙烯三胺反应后,产物再与甲基丙烯酸甲酯反应制成桐油酸咪唑啉衍生物,利用红外光谱分析了合成产物的分子结构,利用失重法和动电位极化曲线考察了合成产物在盐酸溶液中对N80钢的缓蚀性能。结果表明:合成的桐油酸咪唑啉衍生物为以阴极抑制为主的混合型缓蚀剂,能有效抑制N80钢在盐酸介质中的腐蚀;随着桐油酸咪唑啉衍生物浓度的增大以及腐蚀介质温度和浓度的降低,N80钢的腐蚀速率下降,缓蚀效率上升。     

MDS-6制备离子液体最佳条件探索

以N-甲基咪唑,溴代正丁烷,四氟硼酸钠为原料,采用两步法合成咪唑基离子液体1-丁基-3-甲基咪唑四氟硼酸盐(bmimBF4),重点对产物的最佳合成方法、最佳反应时间、最佳反应温度进行了探索。实验结果表明,使用微波消解仪(MDS-6)能快速有效地合成离子液体,且最佳的合成条件为:当微波功率400W,甲基咪唑与溴代正丁烷的摩尔比为1∶1.1,反应时间45min,微波反应温度80℃时,中间体bmimBr的合成最理想;当bmimBr与NaBF4的摩尔比1∶1.2,微波反应温度65℃,反应时间60min时,离子液体bmimBF4产率达到90%左右。试验产物用IR进行了确认。所制备的离子液体为后面制备四氧化三铁纳米空心球做准备。     

新型肉桂基咪唑啉缓蚀剂的合成及其对盐酸介质中Q235钢的缓蚀性能

目前,有关用肉桂酸和有机胺合成咪唑啉衍生物及其合成产物的缓蚀性能与机理研究未见介绍。利用肉桂酸和二乙烯三胺脱水反应生成咪唑啉衍生物,采用失重法、电化学方法、量子化学计算研究了合成缓蚀剂对Q235钢的缓蚀性能和机理。结果表明,新型肉桂基咪唑啉的缓蚀率随缓蚀剂浓度的增大而升高,＂-31mol／LHCl中缓蚀剂浓度为800m...     

研究具有新骨架的青发色性化合物——吡唑骈咪唑吡啶

从合成两种吡唑骈咪唑吡啶:1-H-吡唑[5’,1’:2,3]咪唑[4,5-b]吡啶（PIP-A）及1-H吡唑[1’,5’:1,2]咪唑[4,5-c]吡啶（PIP-B）的研究结果,认为这两种化合物结构式3位具有活性亚甲基能与醌二亚胺（QDI）偶合反应,而且形成的青发色染料（PIP-A-Dye）和（PIP-B-Dye）具有类似的光谱吸收特性,如与前苯酚系青成色剂形成的染料相比,具有1）最大吸收波长稍短波化,2）光谱吸收曲线形状非常锋利,3）暗褪色性好,还原电位低弱。     

功能化离子液体的合成及对环氧树脂的改性

首先采用阳离子开环聚合法合成端羟基聚环氧氯丙烷(PECH),然后将其与N-乙基咪唑反应,制备咪唑型聚醚离子液体(PIIL),并用红外和核磁谱图对其结构进行表征。再将咪唑型聚醚离子液体与通用型环氧树脂(EP)进行共混,在苯胺固化剂作用下固化成型。用凝胶渗透色谱测定了PECH的相对分子质量及其分布,用红外光谱和差示扫描量热仪对离子液体与环氧树脂复合产物(PIIL/EP)进行了结构表征及热性能测试,研究了PECH相对分子质量及聚醚离子液体的含量对EP冲击强度的影响。结果表明,合成的咪唑型聚醚离子液体是目标产物,当PECH相对分子质量为1000左右时,冲击强度较好。随着PIIL含量的增加,改性后的EP冲击强度大幅度提高,当PIIL用量为EP的50%时,冲击强度高达14.86kJ/m2,固化后的EP明显具有橡胶的弹性。     

离子液体[Amim]PF_6的水相法合成与表征

以N-甲基咪唑、烯丙基氯为原料,采用回流法制备中间体氯化-1-烯丙基-3-甲基咪唑离子液体([AMIM]Cl),进而采用水相法,通过离子交换制备了疏水型离子液体1-烯丙基-3-甲基咪唑六氟磷酸盐([Amim]PF6),考察了合成温度、中间体与六氟磷酸钾的摩尔配比对其产率的影响,以红外光谱、核磁共振波谱进行结构表征。结果表明,水相法能够有效地合成目标产物,大大缩短合成时间;当温度为30℃,物料比n([Amim]Cl)∶n(KPF6)为1∶1.2,反应10min可以得到产率为87%的[Amim]PF6。     

金属锌功能化离子液体催化PET聚酯醇解反应

合成了一种热稳定性良好、具有Brφnsted酸和Lewis酸双重酸性的金属锌功能化离子液体N-甲基丁基咪唑三溴化锌([Bmim]ZnBr3),并将其用于催化PET聚酯在乙二醇中的醇解反应。研究结果发现[Bmim]ZnBr3催化活性明显高于溴代N-甲基丁基咪唑([Bmim]Br)和ZnBr2,反应温度和催化剂的浓度均是影响PET聚酯乙二醇醇解的重要因素。本文中合成的催化剂对常见的五种PET制品均有良好的催化降解作用,经FTIR和1H-NMR分析表明,降解产物是对苯二甲酸乙二醇酯(BHET)。推测的反应机理是:[Bmim]ZnBr3通过与聚酯分子形成环状过渡态完成催化历程。     

溴化1-乙基-3-甲基咪唑氯化锌离子液体的合成、表征及催化性能

采用溴代乙烷与N-甲基咪唑为原料合成了中间体溴化1-乙基-3甲基咪唑,并与氯化锌反应制备了1-乙基-3-甲基溴化咪唑氯化锌盐。分别经1 HNMR、FT-IR、TG、DSC对离子液体进行了结构表征及热分析。将该离子液体用于尿素醇解合成碳酸二乙酯反应体系,考查了[EMIM][Br][Zn2Cl4]离子液体的催化性能,碳酸二乙酯的收率超过25%。     

The Solubility of Salicylic Acid in Supercritical Carbon Dioxide

The possibility of using the method of supercritical fluid extraction for purifying the product of synthesis of salicylic acid is revealed and confirmed experimentally. A continuous-flow experimental setup is used to investigate the solubility of salicylic acid and phenol in supercritical CO₂ and to purify the product of synthesis of salicylic acid at a temperature of 308 K in the pressure range from 7.8 to 12 MPa. The salicylic acid content of the resultant product conforms to the requirements of the State Pharmacopoeia.     

500t/a纳米TiO2的生产工艺设计方案

提出了以硫酸法钛白生产的中间产物偏钛酸为原料均匀沉淀法工业生产纳米TiO2的工艺路线,生产规模确定为500t/a,产品品种为锐钛矿型和金红石型.介绍了间歇搅拌釜式水解工艺、多孔陶瓷膜洗涤、隔膜压滤机过滤、旋流动态煅烧炉-旋转闪蒸干燥组合煅烧的工艺设计方案和主要设备的选型,对存在的问题进行了讨论.     

Knowledge integration and sharing for complex product development

Product development is a highly creative and knowledge-intensive process that involves extensive information and knowledge exchange and sharing among geographically distributed teams and developers. How to best integrate such heterogeneous product knowledge has become an extremely important knowledge management (KM) subject associated with product development. Product development knowledge integration and sharing is becoming a key issue in the enterprise KM. This paper addresses the challenges of product development knowledge integration and sharing during product development. The aim of this research work effort is to develop a method to enhance the integration and sharing of product knowledge during the development phase. This study presents a systematic approach to developing knowledge integration and sharing for product development. The proposed approach includes the steps for designing a framework of product development knowledge sharing, developing representation model for product development knowledge, designing product development knowledge sharing process, designing product development knowledge integration ontology, developing knowledge integration and sharing method for product development based on ontology, and implementation of product development knowledge integration and sharing method. The proposed method could bring out an efficient and proactive way for knowledge integration and sharing among product developers in the product development process.     

High Performance Liquid Chromatographic Method for the Determination of Diphenhydramine in Liquid and Solid Drug Dosage Forms and Its Application to Stability Testing

Abstract

A simple, precise, rugged, stability-indicating method for diphenhydramine in liquid and solid drug preparations based on reversed phase ion-pair HPLC is described. The eluent used with the C8-bonded phase column, was acetonitrile/0.005 M aq. hexanesulfonic acid/acetic acid (70/30/1,v/v). The liquid product was simply dissolved in acetonitrile/water/acetic acid (70/30/1,v/v) and filtered; the solid product was briefly ground, dissolved in the same solvent, and filtered. The precision (rsd) of the method for diphenhydramine in the liquid sample is 0.52%, and 0.50% for the solid sample. The method is linear up to 200 μg/mL. Based on spiking studies, the recoveries are 100.1% for the liquid sample, and 99.2% for the solid sample. The method was applied to the study of the thermal stability of the drug by following the degradation of diphenhydramine in the two products at temperatures in the 42°C to 62°C range for up to 16 weeks. Shelf lives of the products were determined assuming zero and first order kinetics of decomposition, and are at least 163 days for the liquid product, and at least 255 days for the solid product.     

Rapid high-resolution characterization of functionally important monoclonal antibody N-glycans by capillary electrophoresis

Characterization of the N-glycosylation present in the Fc region of therapeutic monoclonal antibodies requires rapid, high-resolution separation methods to guarantee product safety and efficacy during all stages of process development. Determination of fucosylated oligosaccharides is particularly important during clone selection, product characterization, and lot release as fucose has been shown to adversely affect the ability of mAbs to induce antibody dependent cellular cytotoxicity (ADCC). Here, we apply a general capillary electrophoresis optimization strategy to separate functionally relevant fucosylated and afucosylated glycans on mononclonal antibody products in the presence of several high mannose oligosaccharides. The N-glycans chosen represent those most commonly reported on CHO cell derived therapeutic antibodies. A rapid (<7 min) high-resolution separation of 12 commonly reported and functionally important IgG glycans was developed by systematically evaluating the effects of selectivity (boric acid) and efficiency (linear polyacrylamide) enhancing additives. The approach can be used to rapidly optimize capillary electrophoresis separation of other glycan mixtures. Following optimization, the method was applied to overnight sample processing for automated 96 well plate-based glycosylation analyses of two nonproprietary therapeutic monoclonal antibodies, demonstrating ruggedness and suitability for high-throughput process and product monitoring applications.     

基于可靠性的设计门限值的分析与确定

针对设计过程中所需确定的产品主要参数的可靠性设计门限值进行了分析。通过采用蒙特卡洛仿真方法和性能性参数可靠性评定方法,实现了随机变量的综合分析和可靠性设计门限值的确定,从而提出了产品设计过程中保证可靠性指标的实现途径,并为产品的制造验收和使用检测提供了定量依据。     

A new approach to LiFePO4/C synthesis: The use of complex carbon source without ball milling

A new approach to synthesize LiFePO₄/C composite without the need of ball milling was developed by using complex carbon source. The esterification reaction between citric acid and sucrose during the drying process fosters the well-mixing of precursor materials, which contributes to the small particle size, porous network, large surface area and good electrochemical performances of LiFePO₄/C composite. The ratio of sucrose to citric acid affects the morphology and electrochemical performance of LiFePO₄/C. This study offers a new method to optimize the morphology of LiFePO₄/C composite by controlling the interaction between different precursors during precursor treatment, such as the esterification reaction between carboxylic acid and sugar. The method developed is simple, requires inexpensive starting materials and the final product gives good electrochemical performance; therefore, it may be of great interest in the mass production of LiFePO₄/C cathode material.     

A neutral loss activation method for improved phosphopeptide sequence analysis by quadrupole ion trap mass spectrometry

Recent advances in phosphopeptide enrichment prior to mass spectrometric analysis show genuine promise for characterization of phosphoproteomes. Tandem mass spectrometry of phosphopeptide ions, using collision-activated dissociation (CAD), often produces product ions dominated by the neutral loss of phosphoric acid. Here we describe a novel method, termed Pseudo MS(n), for phosphopeptide ion dissociation in quadrupole ion trap mass spectrometers. The method induces collisional activation of product ions, those resulting from neutral loss(es) of phosphoric acid, following activation of the precursor ion. Thus, the principal neutral loss product ions are converted into a variety of structurally informative species. Since product ions from both the original precursor activation and all subsequent neutral loss product activations are simultaneously stored, the method generates a "composite" spectrum containing fragments derived from multiple precursors. In comparison to analysis by conventional MS/MS (CAD), Pseudo MS(n) shows improved phosphopeptide ion dissociation for 7 out of 10 synthetic phosphopeptides, as judged by an automated search algorithm (TurboSEQUEST). A similar overall improvement was observed upon application of Pseudo MS(n) to peptides generated by enzymatic digestion of a single phosphoprotein. Finally, when applied to a complex phosphopeptide mixture, several phosphopeptides mis-assigned by TurboSEQUEST under the conventional CAD approach were successfully identified after analysis by Pseudo MS(n).     

伦理关怀视角下的核酸检测试剂盒改良设计

目的 在疫情常态化背景下,为避免核酸检测试剂盒在使用与回收周期中,对传染源处理不当造成二次污染,因此进行试剂盒改良设计,以构建良好的伦理关怀关系。方法 首先分析了当下核酸检测产品所存在的弊端,获取功能需求,确定了所属设计类型,运用AD理论对功能需求进行分解,然后对初步设计方案进行耦合判断,运用TRIZ进行解耦,最终得到设计方案。结果 采用集成AD和TRIZ的设计方法,从伦理关怀的视角下,对核酸检测试剂盒的安全消毒模块进行设计,将核酸检测试剂盒改良为一体化结构,并增添消毒灭菌模块,最终设计方案可有效解决二次污染问题并实现伦理关怀。结论 方案通过集成AD和TRIZ的设计方法,从功能结构上对核酸检测试剂盒进行改良设计,解决了现有产品存在的诸多问题。在设计中注重产品使用感受,帮助人们在使用产品时舒缓紧张感并构建信任,同时为产品新功能模块的创新设计提供思路和参考。     

Electrometric methods of analyses applied to process and product control at the ab bofors nitroglycerine plant

Spent acid from the injector process for the production of nitroglycerine contains 2 to 3 per cent of nitroglycerine. This may later separate from theThe nitroglycerine content in the nitrating acid spent acids is determined polarographically in an aqueous solution containing 3 per cent ammonium acetThe nitroglycerine process is controlled by measurement of the redox potential of the spent acid. The purity of the product nitroglycerine is determineResults and experiences from the above mentioned methods of process and product control at the AB Bofors nitroglycerine plant will be discussed.A polagraphic method for the determination of nitrate esters other than nitroglycerine, $\text{e.}$$\text{g.}$ mixtures of nitroglycol acid nitroglycerin