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Purifying method for 3-methyl-3-butene-1-ol

A purification method and technology of butene, applied in the separation/purification of hydroxyl compounds, chemical instruments and methods, preparation of hydroxyl compounds, etc., can solve problems such as solvent pyrolysis, yield drop, equipment blockage, etc., and achieve high purification efficiency, Simple operation effect

Inactive Publication Date: 2018-07-20
SHANDONG CHENGTAI CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Embodiment 1, a kind of purification method of 3-methyl-3-buten-1-ol, comprises the following steps:

[0012] 1. Add 1wt% ethylene oxide and 2wt% polyphosphoric acid to the raw material containing 3-methyl-3-butene-1-ol and isoamyl alcohol, and stir at 80°C for 1.5 hours to obtain an organic solution ;

[0013] 2. Add 1wt% zinc powder to the organic solution obtained in step 1, and stir to obtain a suspension;

[0014] 3. Distill the suspension obtained in step 2 under reduced pressure. The pressure of the distillation tower is -0.08MPa, and the fraction at 130°C is collected to obtain 3-methyl-3-butene-1-ol; The yield of 3-buten-1-ol was 99.97%.

Embodiment 2

[0015] Embodiment 2, a kind of purification method of 3-methyl-3-buten-1-ol, comprises the following steps:

[0016] 1. Add 1.5wt% ethylene oxide and 2.5wt% polyphosphoric acid to the raw material containing 3-methyl-3-buten-1-alcohol and isoamyl alcohol, and stir at 90°C for 1.8 hours to obtain organic solution;

[0017] 2. Add 1.5wt% zinc powder to the organic solution obtained in step 1, and stir to obtain a suspension;

[0018] 3. Distill the suspension obtained in step 2 under reduced pressure. The pressure of the distillation tower is -0.08MPa, and the fraction at 131°C is collected to obtain 3-methyl-3-butene-1-ol; The yield of 3-buten-1-ol was 99.98%.

Embodiment 3

[0019] Embodiment 3, a kind of purification method of 3-methyl-3-buten-1-ol, comprises the following steps:

[0020] 1. Add 2wt% ethylene oxide and 3wt% polyphosphoric acid to the raw material containing 3-methyl-3-butene-1-ol and isoamyl alcohol, stir at 100°C for 2 hours to obtain an organic solution ;

[0021] 2. Add 2wt% zinc powder to the organic solution obtained in step 1, and stir to obtain a suspension;

[0022] 3. Distill the suspension obtained in step 2 under reduced pressure. The pressure of the distillation tower is -0.08MPa, and the fraction at 132°C is collected to obtain 3-methyl-3-butene-1-ol; The yield of 3-buten-1-ol was 99.99%.

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Abstract

The invention discloses a purifying method for 3-methyl-3-butene-1-ol. The purifying method for the 3-methyl-3-butene-1-ol comprises the following steps: (a), adding 1 to 2 weight percent of ethyleneoxide and 2 to 3 weight percent of polyphosphoric acid in a raw material which contains the 3-methyl-3-butene-1-ol and isoamylol, and stirring for 1.5 to 2 hours at the temperature of 80 to 100 DEG Cto obtain an organic solution; (b) adding 1 to 2 weight percent of zinc powder into the organic solution which is obtained in the step (a), and stirring uniformly to obtain suspension liquid; (c) distilling the suspension liquid which is obtained in the step (b) under reduced pressure, and collecting fraction at 130 to 132 DEG C to obtain the 3-methyl-3-butene-1-ol, wherein the pressure in a distilling tower is -0.08 MPa; the purifying method which adopts the scheme disclosed by the invention is high in purifying efficiency; the yield of the 3-methyl-3-butene-1-ol can reach 99.99 percent.

Description

technical field [0001] The invention relates to a purification method, in particular to a purification method of 3-methyl-3-buten-1-ol. 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 alkanes and olefins mixtures can be extractive distillation, usually using strong polar solvents such as ethylene glycol, dimethyl sulfoxide, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/74C07C29/80C07C29/94C07C33/03
CPCC07C29/74C07C29/80C07C29/94C07C33/03
Inventor 文斌刘明久张国华王杰兴
Owner SHANDONG CHENGTAI CHEM IND