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Method for preparing ethyl acetoacetate
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A technology of ethyl acetoacetate and ethanol, which is applied in the field of preparation of ethyl acetoacetate, can solve the problems of high risk, many wastes, and high toxicity of diketene, and achieve the effect of low raw material price, good safety and simple process
Active Publication Date: 2013-11-13
吴江市曙光化工有限公司
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Among these two methods, the former has the disadvantages of serious corrosion of equipment, high toxicity of diketene, and serious environmental hazards, while the latter is too expensive, has a lot of three wastes and is very dangerous
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Embodiment 1
[0017] In a fixed-bed reactor with a diameter of 25mm and a length of 1000mm, catalysts such as copper, zinc, aluminum, nickel and other metals and aluminum oxide, copper oxide, zinc oxide, nickel oxide and other metal oxides are added, consisting of 20% copper, 28% zinc, aluminum 11%, nickel 16%, aluminum oxide 6%, copper oxide 4%, zinc oxide 8%, nickel oxide 7% by weight. The outer layer is heated with an electric heating wire, the temperature is controlled by a pressure regulator, and ethanol is introduced, the reaction temperature is 420°C, and the space velocity of the reactant is 5500h -1 , the molar ratio of ethanol and catalyst is 1.9: 1, and the molar yield of one reaction of ethyl acetoacetate reaches 63%.
Embodiment 2
[0019] In a fixed-bed reactor with a diameter of 20mm and a length of 800mm, add copper, zinc, aluminum, nickel and other metals and aluminum oxide, copper oxide, zinc oxide, nickel oxide and other metal oxide catalysts, consisting of 23% copper, 31% zinc, aluminum 13%, nickel 18%, aluminum oxide 3%, copper oxide 3%, zinc oxide 4%, nickel oxide 5% by weight. The outer layer is heated with an electric heating wire, the temperature is controlled by a pressure regulator, and ethanol is introduced, the reaction temperature is 390°C, and the space velocity of the reactant is 6500h -1 , the molar ratio of ethanol and catalyst is 2.7: 1, and the molar yield of one reaction of ethyl acetoacetate reaches 52%.
Embodiment 3
[0021] Add copper, zinc, aluminum, nickel and other metals and aluminum oxide, copper oxide, zinc oxide, nickel oxide and other metal oxide catalysts in a fixed-bed reactor with a diameter of 25 mm and a length of 1200 mm, consisting of 17% copper, 27% zinc, aluminum 10%, nickel 15%, aluminum oxide 7%, copper oxide 6%, zinc oxide 9%, nickel oxide 9% by weight. The outer layer is heated with a heating wire, the temperature is controlled by a pressure regulator, and ethanol is introduced, the reaction temperature is 450 °C, and the space velocity of the reactant is 4500h -1 , the molar ratio of ethanol to the catalyst is 2.2:1, and the molar yield of ethyl acetoacetate reaches 56%.
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Abstract
The invention relates to a method for preparing ethyl acetoacetate. The method comprises the following steps of: allowing gasified ethanol to continuously pass through a fixed bed reactor with a catalyst layer, and reacting to obtain the ethyl acetoacetate, wherein the reaction temperature is 200 to 700 DEG C; and the catalyst layer comprises the following components in percentage by weight: 10 to 25 percent of copper, 15 to 35 percent of zinc, 5 to 15 percent of aluminum, 4 to 20 percent of nickel, 2 to 8 percent of alumina, 1 to 6 percent of copperoxide, 3 to 9 percent of zincoxide and 4 to 10 percent of nickeloxide. The method is continuously operated; raw materials are cheap; three wastes are basically avoided; and the process is simple, low in cost and high in safety.
Description
technical field [0001] The present invention relates to a kind of preparation method of ethyl acetoacetate. Background technique [0002] Ethyl acetoacetate is a very important intermediate in organic synthesis, which can be used to prepare medicines, pesticides, dyes and spices. At present, there are two main industrial production methods of conventional ethyl acetoacetate: one is to use acetic acid in the presence of triethyl phosphate to crack to generate vinyl ketene, and then dimerize to generate diketene. Esterification is carried out under the catalysis of sulfuric acid to produce ethyl acetoacetate, and the obtained crude product is distilled under reduced pressure to obtain the finished product; the second is to prepare ethyl acetoacetate with ethyl acetate as raw material and sodiummetal or sodium ethoxide. Among these two methods, the former has the disadvantages of severe equipment corrosion, high toxicity of diketene, and serious environmental hazards, while t...
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