Acetylacetone synthesis method
A technology for the synthesis of acetylacetone, which is applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve the problems of product yield to be improved, many reaction by-products, complicated operation, etc., and achieve separation Recycling, less reaction by-products, good selectivity
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Embodiment 1
[0025] Preparation of catalyst γ-alumina: dehydration of aluminum hydroxide at low temperature to generate Al 2 o 3 , then Al 2 o 3 Dry at 90°C for 20 hours, then bake at 450°C for 1.5 hours, and then grind the baked alumina to obtain γ-alumina with a purity of 99% and a specific surface area of 170-185m 2 / g, particle size 30-35nm, bulk density 0.1-0.15g / cm 3 .
[0026] In a three-neck flask equipped with a rectification column, add ethyl acetoacetate and acetic anhydride at a molar ratio of 1:1, and simultaneously add γ-alumina with 0.5% acetic anhydride mass, control the reaction temperature at 125°C, and Ethyl acetate was distilled out from the reaction system. After reacting for 6 hours, γ-alumina was recovered by filtration, and fractions at 135-142°C were collected by rectification to obtain acetylacetone.
[0027] The acetylacetone collected by rectification was quantitatively and qualitatively analyzed by SP-3700 gas chromatography, and the yield of AA was calc...
Embodiment 2
[0029] Preparation of catalyst γ-alumina: dehydration of aluminum hydroxide at low temperature to generate Al 2 o 3 , then Al 2 o 3 Dry at 110°C for 28 hours, then calcined at 800°C for 2.5 hours, and then grind the calcined alumina to obtain γ-alumina with a purity of 99% and a specific surface area of 185-190m 2 / g, particle size 45-50nm, bulk density 0.15-0.2g / cm 3 .
[0030] In a three-neck flask equipped with a rectification column, add ethyl acetoacetate and acetic anhydride at a molar ratio of 1:1.1, and simultaneously add γ-alumina with 3.5% acetic anhydride mass, control the reaction temperature at 150°C, and Ethyl acetate was distilled out from the reaction system, and after 8 hours of reaction, γ-alumina was recovered by filtration, and fractions at 135-142°C were collected by rectification to obtain acetylacetone. Detection and analysis showed that the yield of AA was 94.5%, and the purity was 99.3%.
Embodiment 3
[0032] Preparation of catalyst γ-alumina: dehydration of aluminum hydroxide at low temperature to generate Al 2 o 3 , then Al 2 o 3 Dry at 100°C for 24 hours, then calcined at 600°C for 2 hours, and then grind the calcined alumina to obtain γ-alumina with a purity of 99% and a specific surface area of 180m 2 / g, particle size 35-45nm, bulk density 0.1-0.2g / cm 3 .
[0033] In a three-neck flask equipped with a rectification column, add ethyl acetoacetate and acetic anhydride at a molar ratio of 1:1.05, and at the same time add γ-alumina with 1.5% acetic anhydride mass, control the reaction temperature at 130°C, and remove the generated Ethyl acetate was distilled out from the reaction system, and after 6.5 hours of reaction, γ-alumina was recovered by filtration, and fractions at 138-140°C were collected by rectification to obtain acetylacetone. Detection and analysis showed that the yield of AA was 97.5%, and the purity was 99.9%.
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