青霉素钠萃取工艺的优化

针对溶媒萃取工艺生产青霉素钠进行技术研究,并对萃取工艺进行了进一步的创新优化,采用离心机萃取工艺替代传统的罐式萃取工艺,提高对不同物料的操作弹性,提高产品质量和收率.     

高效青霉素萃取助剂的合成研究

对发酵青霉素萃取助剂的种类及效果进行了综述,重点介绍了乙氧基脂肪二胺和脂肪酰胺复配破乳剂,并以牛油二胺和环氧乙烷为原料,氢氧化钾为催化剂,合成了乙氧基脂肪二胺,环氧乙烷反应率可达79.5%;用大豆植物油和三乙醇胺合成了油酰胺,以乙氧基脂肪二胺为主、油酰胺为辅制备了破乳剂,该破乳剂用于青霉素的提取,使用量300ppm,溶解情况良好,萃取液界面清晰,界面层厚度0.9~1.2mm,离心分层时间35s,青霉素提取收率（两步,二次结晶）90.6%,性能优于市售同类产品。     

青霉素RSE—POD机串联萃取工艺探索与应用

RSE离心机（固-液-液三相萃取分离机）为固-液-液三相立式分离机,是德国生产的新型离心机,具有处理量大、分离因数高、能够自动排渣的特点;美国生产的液-液卧式离心分离萃取机（POD机）,具有处理量大、萃取级数高（可达4级）、收率高的特点。在青霉素新萃取工艺开发中,充分利用这2种设备的优点,开发了RSE与POD机串联逆流萃取生产工艺,该工艺具有连续稳定、劳动强度小、产品质量好、收率高等优点。     

醋酸丁酯及二正辛基亚砜萃取青霉素的研究

通过化学分析、计算机数据处理及FT—IR红外光谱的确证,提出了醋酸丁酯及二正辛基亚砜萃取青霉素的萃合反应式及萃合物的键合结构;研究中观察到青霉素在醋酸丁酯中形成了反胶团,胶团半径可达0.6μm.     

用硫酸铝作絮凝剂从发酵滤液中萃取青霉素时破乳效果的研究

本文应用铝离子水溶液的化学特点及蛋白质在溶液中结构变化的特征,研究了用硫酸铝作为青霉素萃取工艺中的破乳剂的作用规律及操作条件.中、小试结果表明,先将硫酸铝溶液与滤液混合30秒,并使混合液的pH值>4.5,萃取平衡的pH值>3.0,0.1～0.3%(mass/v)的硫酸铝即可有较好的破乳效果,但需严格控制溶液的pH值.     

粗叔胺中催化剂组份萃取分离

本文以实验数据为依据，在由脂肪醇催化胺化法生产的粗叔胺中，提出采用液—液萃取法净化技术净化粗叔胺，该法操作简单，收率高。     

煤的溶剂热萃取研究进展

综述了近年来在煤的溶剂热萃取（不小于300℃）的研究进展。讨论了主要影响因素包括极性溶剂、酸处理、萃取时间等对热萃取率的影响。结论表明：酸处理、使用强极性溶剂有利于提高煤的热萃取产率;时间和温度是热萃取的两个重要参数,在不同程度上影响着煤的热萃取率;萃取物活性很高,并且基本无灰,是煤直接液化的极好的原料也可以作为内燃机燃料。     

青霉素制备青霉素亚砜的研究

以青霉素G钾盐与低质量分数过氧乙酸为原料氧化制备青霉素亚砜 ,其最佳工艺条件为 :n(C16 H18N2 O4 SK)∶n(CH3CO3H) =1 .0∶( 1 1～ 1 2 ) ,反应温度 0～ 5℃ ,反应时间 2 .0～ 2 5h ,w(CH3CO3H) =8 5% ,w(CH3CO2 H) =1 0 %。青霉素亚砜收率达 96 8%。同时建立了青霉素亚砜的半定量分析方法 ,以硅胶G为固定相 ,以V(CH3CO2 C4 H9 n)∶V(CH3CO2 H)∶V(NaH2 PO4 -H2 O)∶V(C4 H9OH n) =6.0∶2 .0∶1 .0∶0 5为流动相 ,用TLC法对产品进行半定量分析检测 ,并经IR、MS谱图验证了产品结构。     

盐湖卤水提硼萃取剂的研究进展

溶剂萃取法是一种有工业应用前景的盐湖卤水提硼方法,而萃取分离的核心问题在于萃取剂的选择。为此,本文综述了近几年国内外盐湖卤水提硼萃取剂类型及其萃取效果,按照萃取剂结构和萃取方法将提硼萃取剂划分为脂肪醇（包括一元脂肪醇和二元脂肪醇）、芳香醇、混合醇等三部分加以叙述,着重介绍了应用最广的两种萃取剂,即2-乙基己醇和2-乙基-1,3-己二醇的研究与应用情况。同时介绍了大量新型结构的?-二醇类萃取剂,指出了今后提硼萃取剂的设计合成的发展趋势,为盐湖卤水萃取提硼工艺开发中萃取剂的选择提供重要参考。     

固相微萃取-气相色谱法测定氨苄青霉素中丙酮和异丙醇残留量

本文采用顶空-固相微萃取-气相色谱联用技术测定了氨苄青霉素中丙酮和异丙醇残留量。使用自制萃取头(苯-丙共聚物与SE-30复合),萃取时间为50min,温度为60℃,2m×3mm i.d.不锈钢色谱柱、内填充10%聚丁二酸乙二醇酯/202酸洗红色担体。丙酮测定结果的相对标准偏差(RSD)为0.38%,在0.11~20μg.g-1范围时,色谱峰面积与质量浓度之间相关系数(r2)为0.9897,回收率为98.5%~101%;异丙醇测定结果相对标准偏差(RSD)为0.56%,在0.17~20μg.g-1范围时,色谱峰面积与质量浓度之间的相关系数(r2)为0.9902,回收率为97.9%~102%。     

The Extraction of Penicillin G with Aliphatic Amines in Organic Solvents of Different Polarities

The equilibrium constants of the extraction, the molar ratios of amines to penicillin G in the extract and the bonding structures of the extracted species were studied with chemical analysis and the absorbance shift of FT-IR spectra of the functional groups in penicillin G. Extraction of penicillin G from the filtrate of fermentation broth indicates that amines will be difficult to use as the industrial solvent for the production of penicillin G because of the poor quality of the final crystalline product obtained and the difficulties involved in the stripping and solvent recovery.     

Partition Behavior of Penicillin in Three-liquid-phase Extraction System

Partition behavior of penicillins G and V was studied in a novel three-liquid-phase extraction system, which is composed of butyl acetate (BA), polyethylene glycol (PEG), ammonia sulfate [(NH4)2SO4] and water (H2O). The main components in the top, middle and bottom phases are butyl acetate, polyethylene glycol aqueous solution and ammonia sulfate aqueous solution, respectively. Some parameters such as partition coefficients Di/j and mass fractions Ei of penicillins G and V were determined at the room temperature, respectively. Experimental efforts have been made to investigate the partition behavior of penicillin in the three-liquid-phase extraction system, including initial concentrations of phase-forming components [PEG and (NH4)2SO4], PEG molecular weight, pH, initial concentration of penicillin. The results indicated that penicillins G and V have the similar partition behavior. They preferentially distribute into the middle phase with the increase of initial concentration of phase-forming components and into the top phase with the decrease of pH, while partition coefficient Dm/b is hardly affected by pH value. The variation of PEG molecular weight has little effect on mass fractions of penicillin. The increase of initial concentration of penicillins G and V could lead to the increase of Dt/b, Dm/b and the decrease of Dt/m, while their mass fractions in all phases were almost independent on their initial concentrations.     

Trace-Level Extraction Behavior of Actinide Elements by Aliphatic Alcohol Extractants in Mineral Acids: Insights into the Trace Solution Chemistry of Protactinium

The extraction of actinide elements thorium, protactinium (Pa), uranium, neptunium, and americium by aliphatic alcohols (1-octanol, 2-ethyl-hexanol, and 2,6-dimethyl-4-heptanol) was investigated with solvent extraction and extraction chromatographic techniques from hydrochloric and nitric acid solutions. These systems provide the potential for low-cost, high quality methods for the isolation of Pa from complex matrices. Acid dependency experiments demonstrate the selective extraction of protactinium from hydrochloric and nitric acids, relative to the other actinides explored. Experiments were conducted to elucidate the equilibrium chemical stoichiometry of the protactinium complex that underlies this unique extraction behavior. Slope analysis with respect to the alcohol concentration infers a stoichiometric relationship of 2:1 for the alcohol extractant to the protactinium ion. Slope analysis with respect to the chloride ion (when [H⁺] = 0.1, 1, and 4 M) suggests that the stoichiometric identity of the protactinium chloro-complexes depends on the [H⁺] (0.1 M to 4 M). Extraction of Pa increases as the Pa:Cl ratio increases from 1:2, at low acid concentration, to 1:6 at high acid concentration. With respect to the nitrate ion (when [H⁺] = 1 and 4 M), the stoichiometric relationship was determined to be 2:1 nitrate to protactinium throughout the range investigated. The sum of these findings and observations contribute to a deeper understanding of the unique chemistry of protactinium compared to the other members of the actinide group.     

青霉素钾,青霉素亚砜和青霉素砜的薄层色谱法分离和鉴别

用薄层色谱法分离和鉴别青霉素钾、青霉素亚砜、青霉素砜,斑点清晰,重现性好,可作为中间体的检测。     

脂肪醇味阈值的拓扑研究

基于脂肪醇分子结构特征与化学拓扑环境定义了4种结构参数:距离连接性指数(G)、取代基指数(F)、取代基位置指数(T)和羟季原子指数(Q),其中G、T对脂肪醇分子具有良好的结构选择性。使用这4种参数及路径数(P4)、碳原子数(X)与99种脂肪醇的味阈值进行拟合,建立了令人满意的定量结构-味阈值模型:pOL=2.365-1.2811G+0.480Q+5.356×10-5F-8.176×10-6T+0.494X-0.00231P43,n=99,R=0.886,F=56.119,S=0.505。经Jackkn ife法检验,该模型具有稳健性,它的计算值与实验值较为吻合,优于目前文献的研究结果。这些指数有望广泛应用于物质构效学领域。     

Catalytic Enantioselective Addition of Alkyl Grignard Reagents to Aliphatic Aldehydes

Herein, we report an efficient catalytic system for the enantioselective addition of alkyl Grignard reagents to a broad range of aliphatic aldehydes with good yields and enantioselectivities. Remarkably, the challenging methylmagnesium bromide (MeMgBr) can also be added to a variety of aliphatic aldehydes, providing versatile chiral methyl carbinol units with unprecedented yields and enantioselectivities in a simple one‐pot procedure under mild conditions.     

新型高效破乳剂在青霉素生产中的应用

本文介绍了我国青霉素征税中使用的破乳剂现状，对破乳机理进行了比较详细的阐述，新型高效破乳剂Ｄ９２５ｍ采用了混合的表面活性剂体系，可调性好，适应性强，已受到国内主要青霉素生产厂家的关注。