Preparation of Acetylacetone and Calcium Acetylacetonate
|Keywords||Ethyl acetoacetate Acetic anhydride Acetylacetone The hot solid phase method Calcium acetylacetonate|
To of acetyl ethyl acetate and acetic anhydride as raw material, magnesium oxide as a catalyst, the process of synthesis acetylacetone. Analysis of the raw material ratio, reaction temperature, reaction time, stirring speed, the heating method, catalyst type, catalyst dosage, side effects, purification methods, precipitating agents, acidifiers, extraction, etc. on the synthesis rate; through the single factor experiment , the main factors of the reaction time, the ratio of raw materials, the amount of catalyst synthesis yield; verified by orthogonal experiments, the interaction of the main factors of the synthesis rate. Single factor and orthogonal experiment results, suggesting that the optimum conditions, and validation. The verification experiments showed that the optimum conditions for synthesis of acetyl acetone: reaction time 15.3h, of acetyl ethyl acetate and acetic anhydride molar ratio of 1.1, the amount of catalyst is 3% acetic anhydride. Under the process conditions, the reaction step of the synthesis of acetylacetone was 99.28%. The purified product with UV spectrophotometry qualitative analysis, recognized as acetylacetone. Quantitative analysis by HPLC, the purity of the product was 99.27%. After calculation, the overall yield of 82.89%. Addition of the catalysts were characterized. Synthesized above acetylacetone and calcium hydroxide as a raw material, synthetic calcium acetylacetonate thermal solid-phase process. Analysis of the ratio of reactants, reaction temperature, reaction time, purification methods, amount of diluent, the amount of detergent synthesis rate; through the single factor experiment, the ratio of raw materials, the amount of diluent, the amount of detergent and other major synthetic yield; through the analysis of the experimental results of the single factor, suggesting that the optimum conditions, and verified. Verification experiments showed that the optimum conditions of the synthesis of calcium acetylacetonate: Acetylacetone and calcium hydroxide mole ratio of 3.76, the diluent and the mass ratio of calcium hydroxide to 13.5, detergent and the mass ratio of calcium hydroxide 24.0 . Under the process conditions, calcium acetylacetonate single synthesis rate was 93.41%. By recovery loss of calcium acetylacetonate, the circulation rate is increased to 99%. Products by FTIR, TGA-DTA, XRD and melting point determination and other means of qualitative analysis, the results showed that: the product spectrum characteristics consistent standard to prove Calcium acetylacetonate. Papers in acetylacetone, acetylacetone calcium preparation process and acetylacetone characterization methods to be innovative.