甲硫基乙醛肟的合成进展

评述了甲硫基乙醛肟的主要合成方法和工艺,分别从乙醛的肟化和乙醛肟的氯化两个过程介绍乙醛法合成甲硫基乙醛肟的研究和进展。分子筛催化乙醛肟化的乙醛肟收率90%以上;在适宜的氯化条件下,甲硫基乙醛肟的收率95%左右。     

甲硫基乙醛肟的合成工艺研究

本文研究了以乙醛肟为原料合成甲硫基乙醛肟的工艺。对各种因素对产品收率的影响进行了试验，找出了最佳工艺条件。经过工业性试验，证明本工艺安全可靠，收率稳定，产品质量好，经济效益高。     

乙醛肟合成方法的改进

改进了乙醛肟的合成工艺。以盐酸羟胺为原料,滴加乙醛,反应1h后,调节pH值,然后加入自制强酸弱碱盐进行中和,将反应产物蒸馏得到乙醛肟。当盐酸羟胺和乙醛的摩尔比为1∶1 05～1 07、盐酸羟胺和水质量比为1∶1～1∶1 2、反应温度控制在10±2℃、反应体系的pH值控制在6～6 5时,乙醛肟的收率和纯度分别为94 1%和96 2%。     

亚硝酸钠法合成乙醛肟新工艺研究

介绍以亚硝酸钠为主要原料合成农药中间体乙醛肟的工艺路线,对影响收率及产品质量的主要因素进行了系统研究,确定了最佳的工艺路线的操作参数,该工艺肟化收率在９０％以上,产品中乙醛肟含量大于３５％,相对纯度高于９５％。     

无水乙醛肟的制备

乙醇肟是生产农药灭多威的中间体,也是重要的有机合成试剂和分析试剂[1]。用于有机合成的乙醛后有时必须要求无水（如：与酰氯和异氰酸酯的反应）,而目前国内市场提供的乙醇肟为含量40％左右的水溶液,不能满足需要,为此,我们对无水乙醛股的制备做了研究。无水乙醛肟可由相应乙醛肟水溶液制备。乙醛肟水溶液由盐酸羟胺或硫酸羟胺与乙醛反应而得。本文用盐酸羟胺和乙醛反应所得已醛肟水溶液经萃取、分离、蒸馏制备无水乙酸肟,取得了较好的结果。1实验部分1.1试剂与仪器．乙醛为分析纯;盐酸羟胺、氢氧化钢和二氯甲烷均为化学纯。CR－3…     

农药中间体乙醛肟合成新工艺研究

本文介绍了亚硝酸钠为主要原料合成乙醛肟的工艺路线，对影响合成收率及产品纯度的有关因素进行了较系统研究，确定了最佳合成路线及操作参数，为其工业化生产提供了依据。     

乙醛肟的气相色谱分析

本文介绍用１０％ＰＥＧ２０Ｍ,长３ｍ内径３ｍｍ的不锈钢填充柱,以正庚醇为内标物,在１２０℃的柱温下用ＦＩＤ检测器对乙醛肟进行定量分析。该法的变异系数为０．７６％,平均回收率９９．８７％,线性相关系数０．９９９７。     

乙醛肟的化学分析法

本文介绍了灭多威中间体乙醛肟的化学分析法，其准确度和精心精密度符合定量分析要求。．     

乙醛肟气相色谱分析测试研究

本文通过气相色谱法,用ＴＣＤ检测器,对乙醛肟进行了分析,该方法在０～１２０ｇ／Ｌ范围内其相关系数Ｒ２＝０．９９９９,标准偏差为０．１％,平均回收率为９９．５％。本文还对ＧＣ方法与ＨＰＬＣ方法做了比较。     

Synthesis and characterization of polyimides from divalent metal salts of p-aminobenzoic acid

Some 50 metal-containing polyimides with the metallic elements (Mg, Ca, Sr, Ba, Pb, Co, Ni) in the main chain were prepared first by reacting pyromellitic dianhydride (PMDA) with the mixture of divalent metal salts of p-aminobenzoic acid [ABA(M)] and 4, 4'-diaminodiphenylmethane (MDA) to form polyamic acid salts, and then the desired polyimides were obtained in high yield by separating the polyamic acid salts from the solvent and heating them under the imidization conditions. The structures of the samples were characterized by ¹H-NMR and IR, and the thermal properties of polyimides were measured by TG-DTA. It was found that the thermooxidative stability of polyimides decreased as a small amount of a metal element was introduced, and the stability of polymer varied slightly or tends to constancy as the metal content increased to a certain degree. In addition, the inherent viscosity of the polyamic acid salt solutions also decreased markedly with the increase of the metal content. © 1996 John Wiley & Sons, Inc.     

药用氨基酸复合盐的合成研究

氨基酸复合盐是一类具有独特药学作用的氨基酸衍生物.以氨基酸单体为原料研究了L-鸟氨酸L-天冬氨酸盐、L-精氨酸L-谷氨酸盐、L-精氨酸L-焦谷氨酸、L-赖氨酸L-谷氨酸盐等7种氨基酸复合盐的合成方法、结晶条件.产品的转化率均在80%以上,质量符合AJI97等相关标准,工艺适合工业化生产.     

Novel gallium and indium salts of the 12-tungstophosphoric acid: Synthesis,characterization and catalytic properties

The objective of this study was the preparation, characterization and testing of the catalytic properties of the GaPW₁₂O₄₀ and InPW₁₂O₄₀ salts of 12-tungstophosphoric heteropolyacid (HPW). The samples were characterized by XRD, IR, SEM, and ³¹P and ¹H MAS NMR spectroscopy. The acid properties of the solids were directly accounted for by applying ¹H MAS NMR. The salts were screened in the etherification of 1-phenylethanol with C₁–C₄ alkanols in dichloromethane as a solvent to yield the corresponding C₆H₅CH(OR)CH₃ unsymmetrical ethers. In comparison with pure HPW, the new salts revealed generally a higher selectivity of ethers formation at 65 °C.     

Keggin结构的钨钴杂多酸盐的合成与表征

由Ｎａ２ＷＯ４·２Ｈ２Ｏ和Ｃｏ（ＮＯ３）２·６Ｈ２Ｏ在不同条件下合成了两种钨钴杂多酸盐，并对它们的结构和性质进行了表征。     

Synthesis and characterization of water-soluble diazonium salts as contrast-enhancement materials

Water soluble aromatic diazonium double salts, p-diazodiphenylamine chloride zinc chloride (DZS-1) and p-diazoanisol chloride zinc chloride (DZS-2), have been evaluated as photobleachable dyes for contrast enhancement lithography. After testing the bleaching characteristics, aqueous solutions of DZS-1 and poly(vinyl alcohol) were used as a contrast enhancement material. Thermal stability, resist contrast, exposure parameters and other bleaching characteristics of the photobleachable membranes were investigated. A. commercial i-line photoresist was used to evaluate the contrast ratio of the DZS-1/PVA CEL layer. The contrast ratio obtained in this investigation is 1.67.     

Synthesis and characterization of antimicrobial cationic surfactants: Aminopyridinium salts

Three antimicrobial 4-aminopyridinium salts were synthesized using two different processes in an effort to develop antimicrobial surface treatment agents for wool fibers. The structures of the salts were fully characterized using Fourier transform infrared, ¹H nuclear magnetic resonance (NMR), and ¹³C NMR analysis. In addition, their thermal stability was determined using differential scanning calorimetry and thermogravimetric analysis. The antimicrobial efficacy of these compounds was evaluated using minimum inhibitory concentration as an indicator. All of the synthesized aminopyridinium salts showed antimicrobial activity against gram-negative bacteria, but in different levels depending on their structures. The salts possessing longer alkyl chains demonstrated better antimicrobial function. The melting points of the salts decreases as the alkyl chain length increases.     

铌酸的合成与表征

采用氢氧化钾熔融法以不同无机酸处理合成了铌酸。利用傅立叶变换红外光谱仪,热重分析仪和紫外-可见-近红外光谱仪对合成的铌酸分别进行了表征。结果表明,经冰醋酸处理合成的铌酸纯度较高,用硫酸和硝酸处理合成的铌酸含有少量杂质,而磷酸处理后没有得到铌酸。     

聚天冬氨酸的合成与表征

介绍了以L -天冬氨酸为原料 ,热缩合成聚天冬氨酸酐 ,水解得到聚天冬氨酸的合成工艺。采用凝胶色谱法测定了聚天冬氨酸的分子量 ,并用核磁共振对其进行了表征。     

二环烷基次膦酸的合成与表征

以一水合次膦酸钠和环烯烃为主要原料,在醋酸溶剂中,用二叔丁基过氧化物为引发剂,经自由基加成反应合成二环烷基次膦酸,收率90%以上,结构经1HNMR、13CNMR、31PNMR、ESI-MS表征。该反应收率高,易纯化,反应条件温和。提出可能的自由基加成反应机理。     

柠檬酸酐的合成与表征

以无水柠檬酸和乙酸酐为原料合成柠檬酸酐,通过单因素试验利用滴定法考察投料摩尔比、反应温度以及溶剂用量对反应转化率和收率的影响。结果表明:反应温度为52℃,n(乙酸酐)∶n(无水柠檬酸)=1.2∶1,n(乙酸)∶n(无水柠檬酸)=1.0∶1,反应时间为1.5 h时,柠檬酸酐收率达88.8%。利用红外光谱、核磁共振氢谱和质谱表征了合成产物,证明其为五元环状柠檬酸酐。