促进剂O,O′-二异丙基二硫代磷酸镧的制备及其对天然橡胶硫化的影响

Preparation of accelerator lanthanum O,O′-diisopropyldithiophosphate and its effect on curing for natural rubber

以无水乙醇为溶剂,五硫化二磷、异丙醇、氢氧化钾、三氧化二镧为原料,制备了O,O′-二异丙基二硫代磷酸镧(LaDiPDP),考察了反应物用量、乙醇用量、反应温度和反应时间对LaDiPDP纯度的影响,通过傅里叶变换红外光谱(FTIR)、气相色谱质谱联用(GC-MS)及X射线衍射(XRD)对产物进行了表征,且研究了LaDiPDP对天然橡胶(NR)的硫化促进效果。结果表明,在LaCl3.6 H2O用量为化学计量的1.1倍、乙醇/KDiPDP(质量比)为24、反应温度为70℃、反应时间为35 min的条件下,LaDiPDP质量分数可达到96.2%;随着LaDiPDP用量的增加,NR的硫化速率和交联程度逐渐提高,LaDiPDP对NR具有良好的硫化促进作用。

Lanthanum O, O′-diisopropyldithiophosphate （LaDiPDP） was prepared with phosphorus pentasulfide, isopropyl alcohol, potassium hydroxide and lanthanum trioxide in ethanolic. Effects of reactant amount, ethanolic amount, reaction temperature and reaction time on purity of LaDiPDP were investigated systematically. The product was characterized by FTIR, GC-MS and XRD, and its effect on vulcanizing property for natural rubber （NR） was studied. The results showed that optimum reaction conditions was as follows：the amount of LaCl3·6 H2O was 1. 1 times stoichiometric amount, the mass ratio of ethanol to KDiPDP was 24, reaction temperature was 70 ℃ and reaction time was 35 min,and the purity of product was 96.2%. With LaDiPDP amount increased, the vulcanizating rate of NR and total crosslinking density of vulcanizates increased. LaDiPDP could act as effective accelerator.