阅读说明：本技术 一种二环己醚的制备方法 (Preparation method of dicyclohexyl ether ) 是由 王存亮 许灵艳 严学文 黄焕军 王小桥 于 2018-06-27 设计创作，主要内容包括：本发明公开了一种二环己醚的制备方法,在装有环己醇的烧瓶中加入浓硫酸,油浴搅拌加热到134-138℃,分水器除水,反应1-1.5h后,冷却后加入氢氧化钠调节PH至中性,分液,加中性干燥剂除水,减压蒸馏,馏分即为二环己醚；本发明操作简单,收率高,适合企业化生产。(The invention discloses a preparation method of dicyclohexyl ether, which comprises the steps of adding concentrated sulfuric acid into a flask containing cyclohexanol, stirring and heating to 134 ℃ and 138 ℃ in an oil bath, dehydrating by a water separator, reacting for 1-1.5h, cooling, adding sodium hydroxide to adjust the pH value to be neutral, separating liquid, adding a neutral drying agent to remove water, and distilling under reduced pressure to obtain fraction dicyclohexyl ether; the method is simple to operate, high in yield and suitable for industrialized production.)

1. A method for preparing dicyclohexyl ether is characterized in that: adding concentrated sulfuric acid into a flask containing cyclohexanol, stirring in an oil bath, heating to 134 ℃ and 138 ℃, removing water in a water separator, reacting for 1-1.5h, cooling, adding sodium hydroxide to adjust the pH value to be neutral, separating liquid, adding a neutral drying agent to remove water, and distilling under reduced pressure to obtain a fraction, namely dicyclohexyl ether.

2. The method of claim 1, wherein: the cyclohexanol: the volume ratio of concentrated sulfuric acid is 10-12: 3-4.

3. The method of claim 1, wherein: the neutral drying agent is anhydrous calcium chloride, anhydrous sodium sulfate, anhydrous magnesium sulfate and the like.

Technical Field

The invention relates to the technical field of synthesis, in particular to a preparation method of dicyclohexyl ether.

Background

The dicyclohexyl ether is a chemical substance with the molecular formula C₁₂H₂₂O, molecular weight 182.30248, colorless transparent liquid, boiling point 243 ℃, relative density (water =1) 0.92, slightly soluble in water, melting point-3.6 ℃, currently common dicyclohexyl ether is a by-product in the process of preparing cyclohexene from cyclopropanol, and the purity is low, which is not beneficial to the industrialized production.

Disclosure of Invention

The invention aims to provide a preparation method of dicyclohexyl ether suitable for industrial production.

The technical scheme adopted by the invention is that concentrated sulfuric acid is added into a flask containing cyclohexanol, the concentrated sulfuric acid is stirred in an oil bath and heated to 134 ℃ and 138 ℃, a water separator is used for removing water, after the reaction is carried out for 1-1.5h, sodium hydroxide is added after the cooling to adjust the PH to be neutral, liquid separation is carried out, a neutral drying agent is added for removing water, and the fraction is dicyclohexyl ether after reduced pressure distillation.

The cyclohexanol of the present invention: the volume ratio of concentrated sulfuric acid is 10-12: 3-4.

The neutral drying agent in the invention is anhydrous calcium chloride, anhydrous sodium sulfate, anhydrous magnesium sulfate and the like.

The method has the advantages of simple operation, high yield and suitability for enterprise production.

Detailed Description