Synthesis, characterization and catalytic performance of tri-nuclear copper complex

doi:10.16085/j.issn.1000-6613.2017-2271

Abstract

Abstract: A complex catalyst with tetrahedron structure copper(I) iodide (CuI) as active center has been synthesized by solvent-thermal method, which is then used in hydrosilylation. The effect of the material ratios on the product yield has been discussed in depth. The results show that when the molar ratio of ligand to CuI is 1:6, the highest yield is obtained. The chemical composition, spatial structure and properties of the catalyst have been studied by elemental analysis, Fourier transform infrared spectroscopy analysis, X-ray photoelectron spectroscopy analysis, X-ray single crystal diffraction analysis, UV-visible spectroscopy analysis and thermogravimetric analysis, respectively. Furthermore, the catalytic performance has been tested by the hydrosilylation reaction of methylphenyl vinyl resin and methylphenyl hydro-silicone oil. The results indicate that the curing effect is the best when the blending system reacts for 24h under the addition of 0.04% complex at 150℃. The complex shows very good catalytic performance in hydrosilylation, and can be synthesized with the advantages of low-cost raw materials, simple preparation method and convenient storage. It is promising to solve the problem of the high cost of traditional precious metal catalysts in hydrosilylation.

Key words: complex, catalyst, hydrosilylation, copper(I) iodide, crystal, synthesis

摘要： 采用溶剂热法合成了以三核碘化亚铜（CuI）四面体结构为活性中心的硅氢加成反应催化剂，探讨了物料比对产物收率的影响。结果说明了当配体与碘化亚铜的摩尔比为1：6时，产物收率最高。通过元素分析、傅里叶红外光谱分析、X射线光电子能谱分析、X射线单晶体衍射分析、紫外可见光光谱分析、热失重分析对配合物的化学组成、空间结构及性能进行表征，并进一步通过甲基苯基乙烯基树脂和甲基苯基含氢硅油的硅氢加成反应进行催化固化效果验证。结果说明了在催化剂填加量为0.04%、固化温度为150℃的优化条件下反应24h，共混体系固化效果最佳。该配合物对硅氢加成反应具有很好的催化性能，并且原料成本低、制备方法简单、晶体颗粒方便储存，有望解决硅氢加成反应中贵金属催化剂的高成本问题。

关键词: 配合物, 催化剂, 硅氢加成, 碘化亚铜, 晶体, 合成

CLC Number:

LENG Shuai, LI Yuntao, DENG Jianguo. Synthesis, characterization and catalytic performance of tri-nuclear copper complex[J]. Chemical Industry and Engineering Progress, 2018, 37(10): 3879-3884.

冷帅, 李云涛, 邓建国. 三核铜配合物的合成、表征及其催化性能[J]. 化工进展, 2018, 37(10): 3879-3884.

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