Purification method of 3-methyl-3-butene-1-ol

Abstract

The invention discloses a purification method of 3-methyl-3-butene-1-ol. According to the method, a solvent is added, and an extractive distillation technology is adopted for separation, wherein the added solvent is high-boiling-point fatty alkane or fatty alkane containing fatty alcohol; the solvent is added from the middle upper area of a rectifying column, and raw materials containing 3-methyl-3-butene-1-ol and isoamyl alcohol are added from the middle area of the rectifying column; a part of a column bottom liquid is gasified by a heater, and obtained gas is returned into the column from agas phase inlet of the column bottom; gas at the column top is totally condensed into a liquid by a condenser and then sent into a column top return tank, and a part of liquid is sent into the columnfrom a return port at the column top by a return pump. The rectifying column is operated under the condition of reduced pressure, a pure product of 3-methyl-3-butene-1-ol is obtained at the column top, and a mixture of isoamyl alcohol and the solvent exists at the column bottom. The method has the advantages that the adopted solvent is relatively stable at the high temperature, and the product of3-methyl-3-butene-1-ol obtained from the column top is favorable for avoiding self-polymerization loss of the product.

Description

field of invention [0001] The invention belongs to the field of separation of fine chemical water reducer intermediates, and relates to a method for separating and purifying enol from a mixture of enol and saturated alcohol by adding a solvent and extracting and rectifying. Background technique [0002] 3-Methyl-3-buten-1-ol is a water reducer intermediate, which can further synthesize isopentenol (3-methyl-2-butene-1- alcohol). During hydroisomerization, in addition to mainly obtaining prenol, part of 3-methyl-3-buten-1-ol will be converted into isoamyl alcohol. In order to obtain a higher yield of isopentenol, it is necessary to separate 3-methyl-3-buten-1-ol from isopentenol in production. Since the boiling points of 3-methyl-3-buten-1-ol and isoamyl alcohol are very close, it is difficult to achieve the ideal separation effect by conventional separation means, and an effective separation method needs to be developed. [0003] The traditional method for separating alka...

AI Technical Summary

Problems solved by technology

Since olefins enter the bottom of the rectification tower with the solvent, and the temperature at the bottom of the tower is often high, it is easy to cause problems such as yield drop and equipment blockage for unsaturated hydrocarbons that are easy to self-polymerize. When nitrogen-containing or sulfur-containing solvents are used There are also unfavorable factors such as solvent pyrolysis

[0004] For the separation problem containing polyolefins, a suitable alternative is to choose a solvent with a strong interaction with saturated bonds, so that polyolefins become volatile components and enter the top of the column, but such solvents are generally difficult to choose

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