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Hybrid polydimethylsiloxane-zirconium oxo nanocomposites. Part 1 Characterization of the matrix and the siloxane-zirconium oxo interface Ce ´line Guermeur,a Jacques Lambard,b Jean-Franc ¸ois Gerardc and Cle ´ment Sanchez*a

The paper presents an analysis of chemical production requirements in an exclusive synthesis market environment and describes how this analysis guided the development of a modular multi-injection reactor. Detailed engineering of a reactor in the light of the requirements of an organometallic reaction, as well as characterization of the reactor is reported. This reactor has provided the target chemistry result at Lonza Ltd. as detailed in a companion paper.

A Grignard reaction performed in a microreactor is presented. The reaction is of type A (highly exothermic and very rapid) and has a low yield which is attributed to a hot spot formed in the mixing zone of the reactor. The reaction yield could be significantly increased by applying the multi-injection principle, leading to better thermal control in the microreactor. Nevertheless, the microreactor plays a major role in reducing the magnitude of the hot spot. Knowing this, it was possible to design and construct an industrial microreactor with significant advantages such as modularity, high flow rate operation, and low investment expenditure (pumps and flow controller minimization).

The synthesis of transparent hybrid organic-inorganic coatings obtained from condensation between alkoxysilane containing grafted dyes (azo dyes or phthalocyanines) and metal alkoxides precursors has been performed. The Red 17 azo dye, known for its high second order polarisability, was bonded to the silicon oxide network following two procedures: a silylation reaction between Red 17 and triethoxysilane; a coupling reaction between Red 17 and 3-isocyanatopropyltriethoxysilane. Silicon phthalocyanines (known for their third order polarisability and inverse saturable absorption properties) were incorporated into the silicon oxide network by a silylation reaction. Phthalocyanine doped transparent hybrid organic-inorganic coatings were obtained from condensation between diethoxymethylsilane and zirconium propoxide precursors.