Preparation method of 5-ethyl-1, 3-dioxane-5-methanol

Abstract

The invention discloses a preparation method of 5-ethyl-1, 3-dioxane-5-methanol, which comprises the following steps: by using an acidic catalyst, reacting trimethylolpropane and formaldehyde as raw materials in a condensation reaction kettle in an atmosphere with nitrogen or air protection, and neutralizing after the reaction to obtain a neutral reaction solution; sending the neutral reaction solution to a light component rectifying tower for further separation, extracting materials from the tower top to obtain water and light components, extracting materials from the tower bottom to obtain 5-ethyl-1, 3-dioxane-5-methanol and heavy components, sending the 5-ethyl-1, 3-dioxane-5-methanol and the heavy components to a product rectifying tower, and extracting materials from the tower top toobtain a 5-ethyl-1, 3-dioxane-5-methanol product. The rectification yield of the 5-ethyl-1, 3-dioxane-5-methanol can reach 95% or above, and the mass concentration of the 5-ethyl-1, 3-dioxane-5-methanol can reach 99.5% or above. According to the method, a condensation reaction kettle with a simple structure is used, no solvent is used, no solvent residue is left, the process is simple, the economyis good, and the obtained product is high in quality and good in chromaticity.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of 5-ethyl-1,3-dioxane-5-methanol. Background technique [0002] 5-ethyl-1,3-dioxane-5-methanol, commonly known as cyclic trimethylolpropane formal, its English name is 5-ethyl-1,3-dioxane-5-methanol, referred to as CTF, CAS No. 5187-23-5. The synthesis route of 5-ethyl-1,3-dioxane-5-methanol in the prior art is: by-product 5-ethyl during the condensation of trimethylolpropane (aldol condensation + Cannizzaro reaction) -1,3-dioxane-5-methanol, the conversion rate varies with different process conditions, and the conversion rate of 5-ethyl-1,3-dioxane-5-methanol is about 3 in terms of n-butyraldehyde ~21%, due to the low conversion rate, complex components in the condensation liquid, low content of 5-ethyl-1,3-dioxane-5-methanol, difficult separation, high separation cost and poor production process economy. [0003] Patents US4076727,...

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Problems solved by technology

The synthesis route of 5-ethyl-1,3-dioxane-5-methanol in the prior art is: by-product 5-ethyl during the condensation of trimethylolpropane (aldol condensation + Cannizzaro reaction) -1,3-dioxane-5-methanol, the conversion rate varies with different process conditions, and the conversion rate of 5-ethyl-1,3-dioxane-5-methanol is about 3 in terms of n-butyraldehyde ~21%, due to the low conversion rate, complex components in the condensation liquid, low content of 5-ethyl-1,3-dioxane-5-methanol, difficult separation, high separation cost, and poor production process economy

[0003] Patents US4076727, CN89103420.X and CN108383826A respectively disclose the preparation methods of 5-ethyl-1,3-dioxane-5-methanol, all of which require the use of solvents, which makes the process complicated, the production cost rises, and the economy is not good

Patent CN200710055700.0 discloses a method for synthesizing trimethylolpropane cyclic formal, but requires a reactive distillation device, and is intermittently operated, the process is complicated, the reaction temperature is high, and the product quality is poor, so it is not suitable for continuous industrial production

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