Continuous synthesis method for acetylacetone metallic compound

Abstract

The invention relates to a continuous synthesis method and a synthesis device for an acetylacetone metallic compound. The method comprises the following steps of: adding a metallic compound and acetylacetone into a reactor; adding the acetylacetone into a product collector; uninterruptedly distilling the acetylacetone in the product collector into the reactor in the heating process, and reacting the distilled acetylacetone with the metallic compound; when a liquid level in the reactor is higher than a siphon, siphoning liquid comprising the acetylacetone metallic compound generated during reaction in the reactor into the product collector to separate a product from a reactant; distilling the acetylacetone which is not reacted in a product separator into the reactor, and continuously reacting the acetylacetone with the metallic compound; and reacting and refluxing for a certain period of time, stopping heating, cooling a solution in the product collector, precipitating, filtering, drying, and thus obtaining the product. The method has a simple process and universality, is high in product yield and is environment-friendly.

Description

technical field [0001] The invention relates to a method for continuously synthesizing metal acetylacetonate compounds and a synthesis device thereof, in particular to a method for continuously synthesizing metal acetylacetonate compounds using metal compounds and acetylacetone as raw materials and a synthesis device thereof. Background technique [0002] Metal acetylacetonate is a common organometallic complex, which has a wide range of applications in catalysts, catalyst preparation, organic synthesis, and material preparation. For example, vanadyl acetylacetonate can be combined with tert-butyl hydroperoxide (TBHP), and can be rapidly oxidized into a homogeneous pentavalent vanadium compound under the reaction system, which can effectively oxidize various organic functional groups; nickel acetylacetonate catalyst can not only be used as Oligomerization and polymerization catalysts for non-polar monomers such as propylene, styrene, dienes, and cycloolefins, and can also be...

AI Technical Summary

Problems solved by technology

The disadvantages of this type of method are: (1) the yield is low, and salt is generated in the reaction process, resulting in low product purity; (2) to obtain a pure product, the product must be recrystallized, and the process is complicated; (3) Due to the introduction of a large amount of water during the adoption process, a large amount of waste liquid will be generated in the later stage, which will easily cause environmental pollution

The disadvantages of this type of method are: (1) the operation process is complicated, time-consuming, and the production cost is high; (2) for metals that are difficult to prepare hydroxides, or are difficult to obtain pure hydroxides, this method does not Not applicable, such as vanadium, iron (II), etc.

[0006] (3) Step-by-step synthesis reaction method (Rowe RA, Jones M M., et al.Vanadium(IV)Oxy(Acetylacetonate)[Bis(2,4-Pentanediano)Oxovanadium(IV)][J].Inorg.Synth. , 1957, 5:113~116): For some metals, their hydroxides are not easy to obtain, and when the pure metal salts or metal oxides are very expensive, the synthesis of acetylacetonate compounds is more complicated

A large amount of concentrated sulfuric acid needs to be used in the reaction process, which requires high equipment, and the complexation reaction is carried out in aqueous solution, which causes serious loss of reactants and serious pollution

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