过硫脲法和硫化氢法制备了 2,2-二巯基乙基硫代丙硫醇, 折射率达到 1.63,纯度 99%。此外,我们合成了含硅的四元 硫醇——四(2-巯基乙基)硅烷。以四乙烯基硅烷和硫代乙 酸为原料,偶氮二异丁腈为催化剂,并结合采用硅胶过柱提 纯方法,制备了高纯度的四(乙酰硫代乙基)硅烷。然后采 用锂铝氢还原方法,合成了较高纯度的四(2-巯基乙基)硅 烷。从分子结构设计角度开发高含硫量且折射率可调的聚氨 酯镜片专用聚硫醇,探索了多硫化合物扩链技术,开发出系 列化二元、三元、聚硫醇,性能指标达到考核要求。 用 DSC 和 FTIR 研究了原料分子结构、催化剂、复配工艺等 与短流程加工的关联调控技术,为后续理论基础及技术开发 奠定基础。 研究了 H6XDI/BES 体系的固化动力学方程,探 讨了光学聚氨酯转化率-时间-温度的关系。在保证制备的光 学材料具有高的折射率的前提下,通过引入具有双硫键,制 备了高折射率光学自修复材料,不仅具有良好的自修复效 果,显示出良好的光学性质,拓展了高折射光学材料研究的 范畴。对光学聚氨酯镜片专用抗氧化、防紫外等添加剂进行 了系统的研究评价,筛选出最佳复配工艺配方。
The sulfur element, which has both high RI and low dispersion, should be incorporated as much as possible. 2,2-dimercaptoethyl thiopropyl mercaptan(BES) was prepared by thiourea method and hydrogen sulfide method,respectively, with the refractive index 1.63 and the purity 99%. Besides, tetra(2-mercaptoethyl)silane was designed in our project. From the perspective of molecular structure design, we developed special polythiols for polyurethane lenses with high sulfur content and adjustable refractive index, explored the chain extension technology of polysulfide compounds, and developed a series of binary, ternary and polythiols, and the performance indexes met the assessment requirements.DSC and FTIR were used to study the correlation between the molecular structure of raw materials, catalysts, compounding process and short process processing, so as to lay a foundation for the follow-up theoretical basis and technical development. The curing kinetic of H6XDI / BES system was studied, and the relationship between conversion-time-temperature of optical polyurethane was discussed. The optical self-repairing materials with high refractive index were prepared by introducing the double sulfur bond, which have good self-repairing ability and good optical properties. The antioxidant and anti ultraviolet additives for optical polyurethane lenses were systematically studied and evaluated, and the best compounding process formula was selected.