Process for preparing high-purity decanediol by side-line vacuum distillation

A technology of vacuum distillation and decanediol, which is applied in the preparation of hydroxyl compounds, organic compounds, organic chemistry, etc., can solve the problems that there is no special description of the purification method of high-purity decanediol, so as to reduce production costs and energy The effect of low consumption and high product yield

Active Publication Date: 2022-07-01
SINOPEC NANJING RES INST OF CHEM IND CO LTD +1
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] There is no specific description of the purification method of high-purity decanediol in the existing literature, and the purity of decanediol currently on the market is only 98%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Side-line vacuum distillation process flow: the crude 1.10-decanediol is injected into the rectification tower through the feeding unit, and the rectification operation is carried out from the intermediate feed of the rectification tower, and the light components are extracted from the top of the rectification tower, Collect and process; extract the intermediate substance from the side discharge port of the rectification tower, and collect and process; the heavy component is extracted from the bottom of the rectification tower and collect and process, which is a high-purity 1.10-decanediol product.

Embodiment 2

[0022] The content of 1,10-decanediol in crude decanediol is 90%;

[0023] The operating conditions of rectification are: the vacuum degree is 0.0012MPa, the reflux ratio at the top of the rectification tower is 7:1, the temperature at the top of the tower is 132~143.5°C, the temperature at the side outlet is 158~162°C, and the temperature at the bottom of the tower is 170~183°C ℃; the purity of 1,10-decanediol prepared at the bottom of the tower is 99.95%.

Embodiment 3

[0025] The content of 1,10-decanediol in crude decanediol is 95%;

[0026] The rectification operating conditions are: the vacuum degree is 0.002MPa, the reflux ratio at the top of the rectification tower is 3:1, the temperature at the top of the tower is 132~138.5°C, the temperature at the side outlet is 155~158°C, and the temperature at the bottom of the tower is 172~190°C °C. The purity of 1,10-decanediol prepared at the bottom of the column was 99.8%.

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Abstract

The invention relates to a process for preparing high-purity 1,10-decanediol by side-line vacuum rectification of crude decanediol products. The intermediate feed of the rectification column is subjected to vacuum distillation, separation and purification, and 1,10-decanediol is separated from the bottom of the rectification column, and the purity of 1,10-decanediol is ≥99.5%. The purity of the decanediol prepared by the process of the invention is greater than or equal to 99.5%, and at the same time, the process not only has low energy consumption, but also the materials from the side line of the rectifying tower can be put into the system for recycling, which improves the product yield and reduces the production cost.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and relates to a process for refining and purifying high-purity decanediol with crude decanediol. Background technique [0002] 1,10-Decanediol is an emerging fine chemical raw material. It has two hydroxyl groups at both ends of the carbon chain and has high reactivity. It can react with organic acids, isocyanates, acid anhydrides, etc. to form different types of derivatives. . Due to its unique properties and the ability to produce a series of new fine chemical products, it is increasingly used in the fields of fragrances, new polyurethanes, polyesters, plasticizers, pesticides, medicines and lubricant additives. [0003] The industrialized decanediol reported in the literature mainly adopts the catalytic hydrogenation method. Catalyst hydrogenation method, Jones used this method to prepare decanediol for the first time, using copper-chromium catalyst, under the conditions of 250 ℃, 35MPa, to ob...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/80C07C31/20
CPCC07C29/80C07C31/20
Inventor 袁俊秀黄冬储政逯贵广曾志强
Owner SINOPEC NANJING RES INST OF CHEM IND CO LTD
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