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首页> 外文期刊>Combinatorial Chemistry & High Throughput Screening >Optimisation of Polystyrene Resin-supported Pt Catalysts in Room Temperature, Solvent-less, Oct-l-ene Hydrosilylation using Methyldichlorosilane
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Optimisation of Polystyrene Resin-supported Pt Catalysts in Room Temperature, Solvent-less, Oct-l-ene Hydrosilylation using Methyldichlorosilane

机译：甲基二氯硅烷在室温下，无溶剂，Oct-l-烯氢化硅烷化中优化聚苯乙烯树脂负载的Pt催化剂

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Six precursor resins with systematic variation of porous parameters were prepared by suspension polymerisation using specific compositions of divinylbenzene, styrene vinylbenzyl chloride (VBC) and 2- ethylhexan-l-ol (a porogen). Surface areas from N2 sorption and BET analysis were ∼2-170 m2g-1. The VBC content in each case was 38 mol% and these groups were aminated using the sodium salt of trimethylethylene diamine. Pt was introduced onto each resin at three different loadings (∼0.03, ∼ 0.2 and ∼ 0.4 mmol g-1) by appropriate manipulation of K2PtCl6.nnThe matrix of 18 resin-supported Pt complexes was then assessed for catalytic activity in the room temperature, solvent-less, hydrosilylation of oct-l-ene using methyldichlorosilane such that alkene: silane: Pt ratio was fixed at 2:1:1x10-3. Though all the catalysts showed activity lower than that of homogeneous Speier's catalyst, most were sufficiently active to be potentially valuable heterogeneous catalysts in the laboratory, and indeed the plant. The most lightly loaded resins proved to be the least active. The remainder were recycled 5 times, and the best performers, the most highly loaded species, a further 5 times making 10 consecutive uses in all. A strong dependence on the porous structure of the resins was demonstrated with the activity rising systemically with the surface area. The two highest surface area highest loaded species displayed good activity even when used for the tenth time. The level of concurrent alkene isomerisation observed was very low throughout ( < 1%) making these heterogeneous species very selective as well as highly active. Overall the derived catalysts are excellent candidates for use in the research laboratory, and with further development could also be valuable in continuous processes.
机译：通过使用二乙烯基苯，苯乙烯乙烯基苄基氯（VBC）和2-乙基己-1-醇（致孔剂）的特定组成的悬浮聚合，制备了六种具有多孔参数系统变化的前体树脂。 N2吸附和BET分析得出的表面积约为2-170 m2g-1。每种情况下的VBC含量为38mol％，并且使用三甲基乙二胺的钠盐将这些基团胺化。通过适当地控制K2PtCl6.nn，以三种不同的负载量（〜0.03，〜0.2和〜0.4 mmol g-1）将Pt引入每种树脂中。然后在室温下评估18种树脂负载的Pt配合物的基质的催化活性，使用甲基二氯硅烷在无溶剂的情况下对辛-1-烯进行氢化硅烷化，以使烯烃：硅烷：Pt的比例固定为2：1：1x10-3。尽管所有催化剂的活性均低于均相Speier催化剂，但大多数催化剂的活性足以使其成为实验室乃至工厂中潜在有价值的非均相催化剂。负载最轻的树脂被证明是活性最低的。其余的被回收了5次，性能最好的，负载最大的物种又被回收了5次，总共10次连续使用。证明了其对树脂多孔结构的强烈依赖性，其活性随表面积而整体增加。即使在第十次使用时，表面积最高的两个最高负载物种也显示出良好的活性。观察到的同时发生的烯烃异构化水平非常低（<1％），这使得这些异质物种具有很高的选择性和高活性。总体而言，衍生的催化剂是用于研究实验室的极佳候选者，并且随着进一步的发展，在连续过程中也可能是有价值的。

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