制备并表征了具有温控功能的膦配体脂肪醇聚氧乙烯醚亚磷酸邻苯二酚酯(FAPEPP),将其与钯的配合物用于催化松香加氢反应的研究,考察了反应时间、反应温度、氢气压力、催化剂用量等因素对反应的影响。在松香5g、m(松香):m(甲苯):m(水)1:2:2、氯化钯0.090%、n(氯化钯):n(膦配体)l:10、氢气压力5MPa,反应温度160℃,反应时间3h的较佳工艺条件下,产物氢化松香中枞酸的质量分数小于1%,去氢枞酸的质量分数5.6%,符合GB/T14020—2006国家标准;并对催化剂的重复使用性能进行了考察,催化荆相不经过处理直接重复使用5次后,产品氢化松香仍然符合国家标准中关于枞酸和去氢枞酸的指标要求。
The fatty alcohol polyoxyethylene ether 1,2-phenylene phosphate ester (FAPEPP) was prepared, characterized and used as catalyst in the hydrogenation of rosin. Reaction time, reaction temperature, hydrogen pressure and amount of palladium chloride were studied. The optimum reaction conditions were as follows: rosin 5 g, m(rosin) : m(toluene) : m(water) 1 : 2: 2, palladium chloride 0. 090 % , n( palladium chloride) : n (ligands)1: 10, hydrogen pressure 5 MPa, reaction temperature 160 ℃ , reaction time 3 h, mass fraction of abietic acid could be under 1%, mass fraction of dehydroabietic acid was 5.6 % , which conforms to the national standards. The regeneration of catalyst was investigated. After cycling five times, the product of hydrogenated rosin still conforms to the national standards without any treatment of catalyst.