Preparation method of amyl 3-pentyloxy propionate

Abstract

The invention relates to a preparation method of amyl 3-pentyloxy propionate, which comprises the following steps: carrying out transesterification and addition reaction on n-amyl alcohol and an acrylate compound under the action of a basic catalyst to obtain a product containing amyl 3-pentyloxy propionate, and carrying out primary reduced pressure distillation treatment on the product containing amyl 3-pentyloxy propionate under specific conditions to obtain amyl 3-pentyloxy propionate. Distilling off a mixture of an alcohol compound and an acrylate compound, wherein the kettle liquid is a first crude product containing 3-pentyloxy amyl propionate; then carrying out secondary reduced pressure distillation treatment on the first crude product containing amyl 3-pentyloxypropionate under specific conditions, distilling out a fraction at 65-125 DEG C to obtain n-amyl alcohol, and taking a kettle liquid as a second crude product containing amyl 3-pentyloxypropionate; and neutralizing a second crude product containing the amyl 3-pentyloxy propionate by using acid, layering, taking an oil phase, and carrying out third reduced pressure distillation treatment under specific conditions to distill out a fraction at 110-153 DEG C to obtain the amyl 3-pentyloxy propionate, thereby enhancing the yield and purity of the amyl 3-pentyloxy propionate.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of 3-pentyloxypentyl propionate. Background technique [0002] Amyl 3-pentoxypropionate is an environment-friendly high-boiling solvent with a boiling point above 250°C, almost no odor, and low toxicity. Compared with traditional high-boiling-point solvents such as propylene carbonate, 3-pentyloxypentyl propionate has better solubility for high-temperature resins, ceramic raw materials, inks and other materials, thereby improving the surface fluidity of the prepared ceramics and paint films. It is regarded as an ideal solvent for high-temperature resins, ceramic raw materials, inks and other materials. [0003] In the traditional technical scheme for preparing 3-pentyloxypentyl propionate, there are many side reactions, the product and the reactant cannot be separated in time, and it is difficult to separate the impurities in the follow-up, result...

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Problems solved by technology

[0003] In the traditional technical scheme for preparing 3-pentyloxypentyl propionate, there are many side reactions, the product and the reactant cannot be separated in time, and it is difficult to separate the impurities in the follow-up, resulting in low purity and low yield of the obtained product

For example, in Patent Publication No. CN109734594A, the patent uses a traditional tank reactor to prepare pentyl 3-pentoxypropionate. Due to the limitations of the equipment itself, the mass transfer of the entire reaction system is relatively slow, and the back-mixing of the reactants is serious, and the product Can not be separated from the reactants in time, resulting in low conversion rate of raw materials, long reaction time, many side reactions, unfavorable for continuous production and other shortcomings

When preparing the same type of product, as related to the preparation of tert-amyl 3-tert-amyloxypropionate in the patent CN109734596A, it also adopts the traditional kettle reaction, which also has the inherent defects of the kettle reaction; It relates to the method for preparing ethyl 3-ethoxypropionate, which uses a fixed bed reactor to prepare ethyl 3-ethoxypropionate, and the catalyst is fixed in the fixed bed. The method has the advantages of simple synthesis, mild conditions and few side reactions , the catalyst can be recycled and regenerated, which is convenient for continuous production, etc., but this method also has shortcomings, such as the product and reactant cannot be separated in time, which will reduce the conversion rate of raw materials

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