Preparation of Acetylacetone and Calcium Acetylacetonate

Abstract: In this paper, the synthesis process of acetylacetone has been studied, using ethyl acetoacetate and acetic anhydride as raw materials,.magnesium oxide as catalyst. The effects of raw material ratio, reaction temperature, reaction time, stirring speed, heating method, catalyst species, catalyst dosage, side reaction, purification method, precipitant, acidifier, extractant on synthesis yield have been analyzed. In single factor experiments, the effects of main factors including reaction time, material ratio, catalyst dosage on synthesis yield have been studied. In orthogonal experiment, the interaction of main factors on synthesis yield has been verified. Single factor and orthogonal analysis of experimental results speculated the optimum conditions. The verification experiments showed that the optimum conditions of acetylacetone synthesis were:reaction time was 15.3h, molar ratio of ethyl acetoacetate and acetic anhydride was 1.1, weight ratio of catalyst and acetic anhydride was 3%.Under the conditions, the synthesis yield of reaction steps was 99.28%.Purified product identified as acetylacetone by UV spectrophotometry qualitatively. Quantitative analysis showed product purity was 99.27% by HPLC, and the whole yield was 82.89%. The catalysts were also characterized.The thermal-solid synthesis process of calcium acetylacetonate has been studied, using acetylacetone and calcium hydroxide as raw materials. The effects of raw material ratio, reaction temperature, reaction time, purification method, diluent dosage, detergent dosage on synthesis yield have been analyzed. In single factor experiments, the effects of main factors including raw material ratio, diluent dosage, detergent dosage on synthesis yield have been studied. Single factor experimental results speculated the optimum conditions. The verification experiments showed that the optimum conditions of calcium acetylacetonate synthesis were:molar ratio of acetylacetone and calcium hydroxide was 3.76, weight ratio of diluent and calcium hydroxide was 13.5, weight ratio of detergent and calcium hydroxide was 24.0. Under the conditions, the single synthesis yield of calcium acetylacetonate was 93.41%. Through the recovery of calcium acetylacetonate which lost in washing step, the cyclic synthesis yield increased to 99%. Qualitative analysis showed that the product characteristics and spectra of FTIR, TGA-DTA, XRD and melting point determination were as same as standard sample, and identified as calcium acetylacetonate.The paper was innovative in the preparation process of acetylacetone and calcium acetylacetonate, as well as the characterization of acetylacetone.
Key words: ethyl acetoacetate; acetic anhydride; acetylacetone; thermal-solid method; calcium acetylacetonate;

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