橡胶硫化促进剂PZ的合成工艺及微观结构表征  

Synthesis Process and Microstructure Characterization of Rubber Vulcanization Accelerator PZ

作　　者：魏振亮 苗进之 贾太轩[3] 王春艳 李林东 肖莹霞 Wei Zhen-liang;Miao Jin-zhi;Jia Tai-xuan;Wang Chun-yan;Li Lin-dong;Xiao Ying-xia(Human Resources and Social Security Bureau of Hua County,Anyang Henan 456463,China;Henan Kailun Chemical Co.,Ltd.,Anyang Henan 456463,China;College of Chemistry&Environmental Engineering,Anyang institute of technology,Anyang Henan 455000,China)

机构地区：[1]安阳市滑县人力资源和社会保障局,河南安阳456463 [2]河南省开仑化工有限责任公司,河南安阳456463 [3]安阳工学院化学与环境工程学院,河南安阳455000

出　　处：《江西化工》2024年第1期68-71,77,共5页Jiangxi Chemical Industry

基　　金：国家自然科学基金项目(5220020929);河南省中央引导地方科技发展专项跨区域研发合作项目(Z20221343016);安阳市重大科技专项计划项目(2022A02GX008)资助课题。

摘　　要：本研究采用改进后的一步法制备二甲基二硫代氨基甲酸锌(PZ),按照化学计量比m((二甲胺)):m((二硫化碳)):m((非离子表面活性剂)):m((氧化锌)):m((乙醇))=1.0:1.13:0.014:0.53:5.40,滴加氧化锌后搅拌时间20min,反应温度为20℃。非离子表面活性剂化学计量比m(吐温-20):m(辛基酚聚氧乙烯醚):m(脂肪酸聚氧乙烯酯):m(失水山梨醇酯)=4.0:2.0:1.0:1.0,搅拌时间为140min,得到粗品二甲基二硫代氨基甲酸锌(PZ)。经过精制后为白色粉末,对样品的熔点、灰分、加热减量、锌含量、筛余物及收率进行检测,均达到化工行业标准。利用现代仪器对样品进行检测分析,经过对红外图谱的分析,可以初步确定PZ含有C-H键、C-N键、C=S键、C-S键、S-Zn键。使用UV-vis确定紫外最大吸收峰在300 nm处,利用HPLC以甲醇和水为流动相在300nm处对0.001g/mL的样品溶液进行检测,结果显示2个明显吸收峰,分析为杂质和PZ,PZ纯度为96.3%。XRD图谱分析表明PZ的晶胞参数。通过GC-MS测定3.38min、8.11min出现明显的色谱峰,分别由溶剂甲醇和PZ产生。通过^(1)H-NMR确定促进剂PZ中氢原子的数目为12,和PZ分子式C_(6)H_(12)N_(2)S_(4)Zn相吻合,这为确定其结构和开拓应用范围提供了实验依据和基础实验数据。In this study,zinc dimethyl dithiocarbamate(PZ)was prepared by improved one-step method.Raw materal stoichiometric ratio as zinc oxide:ethanol,Dimethylamine:Carbon disulfide,non-ionic surfactant:zinc oxide:ethanolwas 1.0:1.13:0.014:0.53:5.40(weight ratio).Reaction temperature was 20℃,Tween-20:octylphenol polyoxyethylene ether:fatty acid polyoxyethylene ester:dehydrated sorbitol ester weight was 4.0:2.0:1.0:1.0(weight ratio).Crude zinc dimethyl dithiocarbamate(PZ)was synthesized stirring time140 min.After refining,the sample was turned into a white powder.The samples were detected by the melting point,ash content,heating reduction,zinc content,sieve residue,reached the chemical industry standards.The samples were detected and analyzed by using modern instruments.C-H,C-N,C=S,C-S,and S-Zn bonds were contained in PZ through analyzing the infrared spectrum.The maximum UV absorption peak was determined at 300 nm by UV-vis.A sample solution of 0.001 g/mL was detected at 300 nm detected by HPLC with methanol and water as mobile phases.There were two obvious absorption peaks,which were analyzed as impurities and PZ.The purity of PZ was 96.3%.XRD spectrum analysis showed the cell parameters of PZ.Significant chromatographic peaks were observed at 3.38 and 8.11 minutes by GC-MS,generated by the solvents methanol and PZ,respectively.The number of hydrogen atoms in accelerator PZ was determined to be 12 by^(1)H-NMR,which was consistent with PZ molecular formula C_(6)H_(12)N_(2)S_(4)Zn.Experimental basis and basic experimental data were provided in determining its structure and expanding its application range.

关 键 词：二甲基二硫代氨基甲酸锌(PZ) FTIR UV-VIS HPLC XRD GC-MS 1H-NMR 

分 类 号：TQ330.38[化学工程—橡胶工业]