Synthesis Process and Microstructure Characterization of Rubber Vulcanization Accelerator PZ
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 1H-NMR,which was consistent with PZ molecular formula C6H12N2S4Zn.Experimental basis and basic experimental data were provided in determining its structure and expanding its application range.
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