苯基三甲氧基硅烷制备工艺

由苯基三氯硅烷（ＰｈＳｉＣｌ３）和甲醇（ＣＨ３ＯＨ）醇解制备苯基三甲氧基硅烷[Ｐ ｈＳｉ（ＯＣＨ３）３]过程中，采取及时驱除氯化氢（ＨＣｌ）的方法，控制副反应发生 ，可提高ＰｈＳｉ（ＯＣＨ３）３的质量，收率达８０％以上。     

聚二甲基硅氧烷—苯基倍半硅氧烷共聚物及其弹性体 Ⅱ共聚物流动性和硫化胶力学性能的影响因素

羟基封端的聚二甲基硅氧烷和苯基三甲氧基硅烷在有机溶剂中进行碱催化水解缩合反应，形成了聚二甲基硅氧烷—苯基倍半硅氧烷共聚物。在有机锡催化剂存在下，共聚物于室温可硫化成力学性能优良的有机硅弹性体。通过考察各种反应因素对共聚物流动性及硫化胶力学性能的影响，发现Ｈ２Ｏ与ＰｈＳｉ（ＯＣＨ３）３的摩尔比、１０７胶与ＰｈＳｉ（ＯＣＨ３）３的重量比、１０７胶分子量、甲苯用量对共聚物粘度和硫化胶力学性能有较大的影响，其中Ｈ２Ｏ与ＰｈＳｉ（ＯＣＨ３）３的摩尔比是决定共聚物及其硫化胶基本性能的关键因素。     

聚二甲基硅氧烷一苯基倍半硅氧烷共聚物及其弹性体

以苯基三甲氧基硅烷和羟基封端的聚二甲基硅氧烷为原料，在有机溶剂中进行碱催化水解、缩合反应，形成了聚二甲基硅氧烷－苯基倍半硅氧烷共聚物，当Ｈ２Ｏ与ＰｈＳｉ（ＯＣＨ３）３的摩尔比Ｒｗ／ｓｉ〉１．５时，形成的共聚物发生分层或交联；在０．８〈Ｒｗ／Ｓｉ〈１．５的情况下，共聚物为一种白色有机硅流体。通过ＦＴＩＲ和＾１Ｈ－ＮＭＲ光谱研究表明，这种可流动的共聚物是由聚二甲基硅氧烷链段和具有不完整梯形结构的苯基倍     

硅烷（CH3）m（C6H5）nSiCL4—m—n的Rochow合成

用高效ＲＳＰ－Ｓｕ３Ｓｉ合金催化剂，气化的氯苯ＰｈＣｌ与氯甲烷在４００℃同时经过催化剂ＲＳＰ－Ｃｕ３Ｓｉ可制得重要硅烷化试剂（ＣＨ３）ｍＰｈｎＳｉＣｌ４－ｍ－ｎｏ讨论了反应的最佳条件及速度。     

直接法合成甲基（氢）二氯硅烷新工艺研究

本文通过催化作用原理研究，提出了以Ｓｉ、ＣＨ＿３Ｃｌ为原料，直接法合成ＣＨ＿３ＳｉＨＣｌ＿２的新工艺．采用ＣｕＣｌ－Ｎｉ－Ｚｎ催化体系不但能使ＣＨ＿３Ｃｌ适量分解产生ＨＣｌ．而且还能促进ＨＣｌ与Ｓｉ、ＣＨ＿３Ｃｌ反应并有效地转化为目的产物ＣＨ＿３ＳｉＨＣｌ＿２，由小试和４００ｍｍ流化床中试所得的混合单体中，ＣＨ＿３ＳｉＨＣｌ＿２含量＞１５％，（ＣＨ＿３）＿２ＳｉＣｌ＿２＞５０％，为工业化生产有机硅含氢单体开辟了新的途径。     

甲基（γ—氯丙基）二氯硅烷和甲基丙基二氯硅烷定性分析

通过色质联用定性地分析了甲基（γ－氯丙基）二氯硅烷（Ｃｌ（ＣＨ２）３Ｓｉ（ＣＨ３）Ｃｌ２）和甲基丙基二氯硅烷（ＣＨ３（ＣＨ２）Ｓｉ（ＣＨ３）Ｃｌ２）的色谱质谱特征，测定了它们的色谱保留时间。     

聚二甲基硅氧烷—苯基倍半硅氧烷共聚物及其弹性体

以苯基三甲氧基硅烷和羟基封端的聚二甲基硅氧烷为原料，在有机溶剂中进行碱催化水解、缩合反应．形成了聚二甲基硅氧烷－苯基倍半硅氧烷共聚物．当Ｈ２Ｏ与ＰｈＳｉ（ＯＣＨ３）３的摩尔比ＲＷ／Ｓｉ＞１．５时．形成的共聚物发生分层或交联；在０．８＜ＲＷ／Ｓｉ＜１．５的情况下，共聚物为一种白色有机硅流体。通过ＦＴＩＲ和１Ｈ—ＮＭＲ光谱研究表明，这种可流动的共聚物是由聚二甲基硅氧烷链段和具有不完整梯形结构的苯基倍半硅氧烷链组成的．它能够在室温下硫化成力学性能优异的有机硅弹性体。     

硅烷（CH_3）_m（C_6H_5）_nSiCl_（4－m－n）的Rochow合

用高效ＲＳＰ－Ｃｕ_３Ｓｉ合金催化剂，气化的氯苯ＰｈＣｌ与氯甲烷在４００℃同时经过催化剂ＲＳＰ－Ｃｕ_Ｓｉ可制得重要硅烷化试剂（ＣＨ_３）_ｍＰｈ_ｎＳｉＣｌ_（４－ｍ－ｎ）讨论了反应的最佳条件及速度。     

甲基(γ-氯丙基)二氯硅烷和甲基丙基二氯硅烷定性分析

通过色质联用定性地分析了甲基（γ－氯丙基）二氯硅烷［Ｃｌ（ＣＨ２）３Ｓｉ（ＣＨ３）Ｃｌ２］和甲基丙基二氯硅烷［ＣＨ３（ＣＨ２）２Ｓｉ（ＣＨ３）Ｃｌ２］的色谱质谱特征，测定了它们的色谱保留时间。     

具有生物活性的含硅有机锡化合物研究

作者合成了一系列含硅有机锡化合物，对其结构进行了表征。化台物的生物选择性主要取决于硅原子上的取代基（Ｍｅ和／或Ｐｈ）．生物活性实验表明其规律为：（Ｍｅ＿３ＳｏＣＨ＿２）＿３ＳｎＹ＞（ＰｈＭｅ＿２ＳｉＣＨ＿２）＿３ＳｎＹ＞＞（Ｐｈ＿２ＭｅＳｉＣＨ＿２）＿３ＳｎＹ并且不受阴离子Ｙ的影响。     

血样中血小板污染对凝聚胺抗体筛检和交叉配血的影响

目的探讨血小板污染对凝聚胺抗体筛检和交叉配血试验的干扰。方法应用自然沉降和离心方法去除血液标本中的血小板,用凝聚胺方法进行血小板去除前后抗体筛检和交叉配血试验。瑞氏染色显微镜下观察血小板聚集。结果自然沉降的标本有大量的絮状团块,镜下可见血小板聚集,而非红细胞凝块。不同离心力去除血小板污染的程度不同,离心力越大,血小板聚集越少,离心力达2200g,可完全去除血小板污染,对凝聚胺抗体筛检和交叉配血试验的干扰消失。结论血浆标本中血小板污染可对凝聚胺抗体筛检和交叉配血试验产生干扰,但可以采用离心法去除。     

两种不同培养工艺制备森林脑炎灭活疫苗的免疫原性及安全性评价

目的评价细胞工厂工艺制备森林脑炎灭活疫苗的免疫原性及安全性。方法利用10 L转瓶和细胞工厂两种工艺在地鼠肾细胞上培养森林脑炎病毒(tick-borne encephalitis virus,TBEV),收获病毒液,经病毒灭活、超滤浓缩、柱层析纯化、除菌过滤后,制备森林脑炎灭活疫苗。采用透射电子显微镜及SDS-PAGE对病毒进行形态观察及鉴定。将两种工艺共制备的6批疫苗免疫小白鼠,评价疫苗的免疫原性;通过家兔刺激试验及豚鼠主动过敏性试验评价疫苗的安全性。结果两种工艺共制备的6批疫苗原液,透射电镜下观察均可见约为50 nm的圆形病毒颗粒,SDS-PAGE分析均可见相对分子质量分别为50 000和40 000~45 000的蛋白条带,病毒形态及蛋白条带大小均与TBEV相符;免疫保护指数均大于1. 0×10~5,符合《中国药典》三部(2015版)标准;家兔刺激试验对注射部位无刺激性,豚鼠主动过敏试验无小鼠出现过敏性反应。结论细胞工厂工艺和10 L转瓶工艺制备的森林脑炎灭活疫苗均具有良好的免疫原性及安全性。     

两工艺流程对高藻原水中微量有机物的去除特性

试验以高藻水源水为处理对象,就两工艺流程(溶气气浮 活性炭过滤,溶气气浮 砂滤 活性炭过滤)对高藻原水中微量有机物的去除特性进行了考察。试验采用了强化混凝,气浮单元对有机物有一定去除效果,对DOC的去除率高于其它处理单元,而对于BDOC、AOC、HAAsFP,气浮单元的去除效果均弱于两流程的炭滤柱。流程2砂滤柱对有机物去除效果较差。对于试验考察的微量有机物,流程1的去除效果优于流程2,并且起主导作用的处理单元均为炭滤柱,而流程1炭滤柱的去除效果优于流程2炭滤柱。     

Dilatometric study of the baking behaviour of pitch bonded carbon artifacts

A dilatometric apparatus was developed for studying the baking behaviour of pitch bonded green carbon artifacts in situ. This technique resulted in an excellent complement to the thermogravimetric method used by us before in many studies of the baking process. The release of frozen stresses, the collapse of the bodies by the softening of the binder or their swelling due to the formation of volatile products in the body, the bulk shrinkage caused by the crack formation during the pyrolysis of the solidified binder can be clearly analyzed. These effects are shown to be strongly affected by orientation parameters, by the type of filler material, by the binder content and by other factors.     

生漆多糖的分离和分析

由云南镇雄采取新鲜生漆,经丙酮除去漆酚,沸水浴提取,三氯醋酸—正丁醇除杂蛋白,乙醇沉淀。再应用CTAB络合法进一步精制,得到生漆漆多糖精制品,含糖量占90％以上,经纸层析,醋酶纤维素薄膜电泳、琼脂糖电泳分析表明,其组成为单一斑点。经分析,分子中含有已糖醛酸、阿拉伯糖、鼠李糖、半乳糖和葡萄糖。组成中不含蛋白和核酸类物质。     

芳杂环聚合物质子交换膜的制备

引言直接甲醇燃料电池(direct methanol fuel cell,DMFC)由于无需将甲醇转变为氢气,直接使用液体燃料甲醇,与氢氧燃料电池相比,省去许多辅助设备,体积小,成为了便携式电源的最佳候选者,特别适合用于可移动电源,如移动电话、笔记本电脑和照相机等。质子交换膜是直接甲醇燃料电池的核心组成之一,其性能好坏直接影响电池的性能和     

The electrochemistry of nitrate-amide melts: Reactions of nickel and copper in nitrate-amide melts

Copper and nickel may be electrodeposited from their ions in solution in nitrate-amide melts at room temperature. In the ammonium nitrate-acetamide-urea melt at 23°C, the reduction to the metal competes with the corrosion reaction at low rates and with the reduction of the ammonium and nitrate ions of the melt at high current densities. Two distinct types of nickel complexes are found in solution. The nickel complex formed by the corrosion reaction is bound by at least one ammonia ligand. Nickel complexes formed by dissolving the halide in the melt show evidence of coordination by less strongly bounding ligands, probably by amides. Similarly, the visible spectra of copper chloride in solution suggest that the cupric ions are coordinated primarily by amides. The copper corrosion reaction produces a complex with a spectra distinctly different from that of cupric chloride in solution. The shift in absorption maxima suggests that the copper complex formed by the corrosion reaction has at least one ammonia ligand in the coordination sphere.     

铝电解槽内电解质运动的数值模拟

通过适当的简化,建立了铝电解槽内电解质运动的物理模型和数学模型,以商业CFD软件为平台,分别对电磁力作用、阳极气体作用以及电磁力和阳极气体共同作用3种情况下的电解质运动进行了数值模拟. 研究结果表明,电磁力作用时,电解质以水平运动为主,半槽的电解质流场基本上呈现一个大涡的结构;阳极气体作用时,电解质运动主要是以每个阳极周围的小循环为主;电磁力和阳极气体共同作用时,电解质流场与阳极气体作用时几乎完全相同,这说明阳极气体对电解质流场起主要作用.     

Tryptophan H33 plays an important role in pyrimidine (6-4) pyrimidone photoproduct binding by a high-affinity antibody

The importance of Trp H33 in antibody recognition of DNA containinga central pyrimidine (6–4) pyrimidone photoproduct wasinvestigated. This residue was replaced by Tyr, Phe and Alaand the binding abilities of these mutants were determined bysurface plasmon resonance and fluorescence spectroscopy. Conservativesubstitution of Trp H33 by Tyr or Phe resulted in moderate lossesof binding affinity; however, replacement by Ala had a significantlylarger impact. The fluorescence properties of DNA containinga (6–4) photoproduct were strongly affected by the identityof the H33 residue. DNA binding by both the wild-type and theW-H33-Y mutant was accompanied by a small degree of fluorescencequenching; by contrast, binding by the W-H33-F and W-H33-A mutantsproduced large fluorescence increases. Taken together, thesevariations in binding and fluorescence properties with the identityof the H33 residue are consistent with a role in photoproductrecognition by Trp H33 in the high-affinity antibody 64M5.     

Moisture absorption by PVC plastisol components

Moisture can be absorbed from the air by PVC plastisols and by the fused product. Water in plastisols can contribute to defects in films, sheet goods and foam products, usually in the form of depressions or craters. Water absorbed by thermoformable foam PVC sheets can result in defects in the molded product, often appearing as wrinkles. Correlation between the sum of the water absorbed by individual PVC plastisol components and the water absorbed by a fused thermoformable foam sheet suggests that moisture sensitivity of the product can be minimized by selecting plasticizers and PVC resins having low moisture absorption.