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Preparation Of Micelle-like Complex Containing Nickel(Ⅱ) And Catalytic Hydrogenation Of Dimmer Acid

Posted on:2013-11-21Degree:MasterType:Thesis
Country:ChinaCandidate:Y Z LuoFull Text:PDF
GTID:2251330401460325Subject:Materials engineering
Abstract/Summary:PDF Full Text Request
As a oil chemical product with low toxicity, dimmer acid is a sort of good raw materialfor the synthesis of new polymeric materials. It comes from a variety of sources, which can berenewable. Hydrogenated dimmer acid is produced by unsaturated dimmer acid thoughcatalytic hydrogenation reaction. Without C=C bonds, the hydrogenated dimmer acid hasbetter thermal stability, which makes it to be widely used in the synthesis of polyamide,polyester, mineral oil additives, surface active agent, waterproofing agent etc..In this paper,aimed at combining the excellent dispersion and high reaction rate ofmicellar catalysis and metal cataysis, a kind of micelle-like metal complex is designed andsynthesized. Then the imitating micelle metal catalyst is used in hydrogenation of dimmeracid. The study is divided into three parts.Part one: The synthesis of amphiphilic ligand1,2-bis{bis [4-(N-(N-hydroxyethyl-piperazine) methylene)phenyl]phosphine}ethane. The experiment is classified into two steps.The first step is synthesis of the intermediate1,2-bis[bis(4-chlorinemethylphenyl)-phosphine]ethane: With AlCl3as catalyts,1,2-bis(bis-phenylphosphine)ethane reflux withchlorine methyl ethyl ether. The relationship between reaction conditions, such time andreaction temperature, and the product yield was studied. The second step is to use the productof first step react with N-hydroxyethyl piperazine. By means of FT-IR spectroscopy, the majorfunctional groups were determined, and using~1H-NMR to analyse the hydrogen atom indifferent chemical environment, which make the molecular composition, connecting modeand spatial structure can be determined.Part two: The synthesis of micelle-like metal catalyst. The reaction is between hydratednickel perchlorate and self-made ligand1,2-bis{bis [4-(N-(N-hydroxyethyl-piperazine)methylene)phenyl]phosphine}ethane, according to molar ratio of2:1at room temperature. ByFT-IR,~1H-NMR and EDS energy spectroscopy analysis, the species of H atomics, the ratio ofeach element and each group are basically the same with prediction. That means eachsynthesis step is successful.Part three: Hydrogenating the dimmer acid in high pressure, the self-made Ni metalcomplex as catalyst, after several experiments, the optimum conditions for the hydrogenationreaction were determined. The hydrogenated effect was characterized by iodine. Andthe selective property of the catalyst was discussed by comparison of FT-IR spectroscopy.Study of catalyst s reusability was also done by determining the elemental composition of the catalyst and hydrogenation degree of the dimmer acid, after recycling used three times.
Keywords/Search Tags:hydrogenation of dimmer acid, micelle catalyst, Ni metal complex
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