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新型橡塑硫化助剂的合成
引用本文:陈雷,陈国辉,江文辉.新型橡塑硫化助剂的合成[J].应用化工,2011,40(11).
作者姓名:陈雷  陈国辉  江文辉
作者单位:中南大学化学化工学院,湖南长沙,410083
摘    要: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。

关 键 词:双-(γ-三乙氧基硅丙基)二硫化物  硅烷偶联剂  无水合成

Synthesis of new rubber vulcanization agent
CHEN Lei,CHEN Guo-hui,JIANG Wen-hui.Synthesis of new rubber vulcanization agent[J].Applied chemical industry,2011,40(11).
Authors:CHEN Lei  CHEN Guo-hui  JIANG Wen-hui
Affiliation:CHEN Lei,CHEN Guo-hui,JIANG Wen-hui(Department of Chemistry and Chemical Engineering,Central South University,Changsha 410083,China)
Abstract: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.
Keywords:bis-[γ-(triethoxysilyl)propyl]disulfide  silane coupling agent  anhydrous synthesis
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