新型橡塑硫化助剂的合成

Synthesis of new rubber vulcanization agent

以九水硫化钠、硫粉、γ-氯丙基三乙氧基硅烷为原料,甲苯、乙醇作溶剂,合成了双-(γ-三乙氧基硅丙基)二硫化物。讨论了反应物比例、溶剂用量、反应温度和时间等因素对产率的影响。结果表明,最佳工艺条件:硫与九水硫化钠的物质的量比为1.05:1,甲苯与九水硫化钠的物质的量比为36:1,γ-氯丙基三乙氧基硅烷与过硫化钠的物质的量比为2.1:1,无水乙醇与过硫化钠的物质的量比为5.0:1,反应温度为80℃,反应时间为4 h。最终制得的产品外观为淡黄色,类乙醇香味,产率为95.63%,含硫量达13.8%,产品贮存时间长。

Taking nine water-sodium sulfide,sulfur powder and γ-chloropropyltriethoxysilane as raw materials,the toluene and ethanol as the solvent,the bis-[γ-（triethoxysilyl）propyl]disulfide was synthesized.The influence of reactants ratio,solvent dosage,reaction temperature and time,and other factors on synthetic reaction were discussed.The optimum process condition was obtained as follows：the molar ratio of sulfur powder to nine water-sodium sulfide was 1.05 ∶ 1,the molar ratio of toluene to nine water-sodium sulfide was 36 ∶ 1,the molar ratio of chloropropyltriethoxysilane to polysulfide was 2.1 ∶ 1,the molar ratio of absolute alcohol to polysulfide was 5.0 ∶ 1,the synthesis temperature was 80 ℃,the synthesis time was 4 h.The appearance of obtained product was light yellow with ethanol smell.The yield was 95.63% and the sulfur content was up to 13.8%.It also could be stored for a considerable period of time.