同位素标记敌百虫-甲氧基-D_6和敌敌畏-甲氧基-D_6的合成

以CD3OD为同位素源,经与三氯化磷酯化得到亚磷酸二甲酯,再进一步与三氯乙醛加成得到敌百虫-甲氧基-D6,碱解脱去氯化氢分子,重排后生成敌敌畏-甲氧基-D6。以消耗CD3OD计算稳定同位素标记敌百虫-甲氧基-D6和敌敌畏-甲氧基-D6提纯后总收率分别为57.7%和47.3%。产物经高效液相色谱(HPLC)、质谱(MS)和核磁(NMR)等仪器的鉴定为目标物质,化学纯度大于98.0%,同位素丰度高于98.0%,可作为食品安全领域检测用同位素内标试剂。     

纳米级亚磷酸铅及纳米二盐基亚磷酸铅的制备与表征

用微液相合成法制备了PbHPO_3超细粉末。得到的产物经粉末X射线衍射(XRD)和透射电镜(TEM)检测表明为纯净的PbHPO_3和2PbO·PbHPO_3·0.5H_2O。PbHPO_3粒子为均匀球形,尺度范围30nm～60nm,2PbO·PbHPO_3·0.5H_2O粒子为棒状,尺度范围(20～40)nm×(50～200)nm。     

Synthesis of alkynyl phosphite ligands and its application in the preparation of high stability one-component heat-curable silicone rubber

Hydrosilylation reaction is one of the main ways to obtain silicone rubber vulcanized products in the industry. However, it still remains a challenge for the currently used catalyst to obtain one-component silicone rubbers with Karstedt's catalyst. In this work, we synthesize a series of phosphite ligands by transesterification, which are further used in combination with Karstedt's catalyst to prepare one-component silicone rubber. The structure of the ligand is characterized by Fourier transform infrared spectroscopy and nuclear magnetic resonance and the vulcanization properties of silicone rubber are investigated by rotorless vulcanizer, differential scanning calorimeter (DSC) and rotational viscometer. It is found that the complex catalysts have low catalytic activity at ambient temperature when the ratio of P:Pt exceeds 1:1. The viscosity growth results show that the prepared silicone rubber has a storage time of more than 30 days at 25°C, and can be completely cured within 10 min at 150°C. The DSC results indicate that one of the prepared catalysts exhibited relatively strong catalytic activity only above 110.7°C. Moreover, the prepared complex catalyst can effectively avoid the production of colloidal platinum and prolong the storage stability of the catalyst.     

用扫描电镜研究亚磷酸钙无毒防锈涂料的防锈机理

用扫描电镜研究了水对亚磷酸钙醇酸树脂有机涂层结构的影响，并用能谱仪和Ｘ射线衍射仪分析了水化后金属表面的状况．提出了亚磷酸钙醇酸树脂防锈涂料可能的防锈机理。