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Process for preparing high-purity decanediol through side-stream vacuum rectification

A technology of vacuum distillation and decanediol, which is applied in the preparation of hydroxyl compounds, organic compounds, chemical instruments and methods, etc., can solve the problems of not specifically describing the purification method of high-purity decanediol, and reduce production costs , low energy consumption, and the effect of improving product yield

Active Publication Date: 2021-04-30
SINOPEC NANJING RES INST OF CHEM IND CO LTD +1
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  • Summary
  • Abstract
  • Description
  • 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] The process flow of sideline vacuum rectification: put the crude 1.10-decanediol into the rectification tower through the feed unit, and carry out rectification operation from the middle of the rectification tower, and the light components are extracted from the top of the rectification tower. Collect and process; take the intermediate material from the side line outlet of the rectification tower for collection and treatment; extract the heavy component from the bottom of the rectification tower for collection and treatment, which is the high-purity 1.10-decanediol product.

Embodiment 2

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

[0023] The rectification operating conditions are: vacuum degree 0.0012MPa, rectification tower top reflux ratio 7:1, tower top temperature 132~143.5°C, side line outlet temperature 158~162°C, tower bottom temperature 170~183°C °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 the crude product of decanediol is 95%;

[0026] The rectification operating conditions are: vacuum degree 0.002MPa, rectification tower top reflux ratio 3:1, tower top temperature 132~138.5°C, side outlet temperature 155~158°C, tower bottom temperature 172~190°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 from a decanediol crude product through side line vacuum distillation, which comprises the following steps: pumping the 1,10-decanediol crude product into a rectifying tower through a feeding unit, feeding a material flow from the middle of the rectifying tower, carrying out vacuum distillation separation and purification, and separating out the 1,10-decanediol from the bottom of the rectifying tower, the purity of the 1,10-decanediol being greater than or equal to 99.5%. The purity of the decanediol prepared by adopting the process is greater than or equal to 99.5%, meanwhile, the process is low in energy consumption, and the materials discharged from the side line of the rectifying tower can be put into a system to be recycled, so that the product yield is increased, and the production cost is reduced.

Description

technical field [0001] The invention belongs to the field of fine chemical industry 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 located at both ends of the carbon chain. It has high reactivity and can react with organic acids, isocyanates, anhydrides, etc. to produce different types of derivatives. . Due to its unique performance and the ability to produce a series of new fine chemical products, it is used more and more in the fields of spices, new polyurethanes, polyesters, plasticizers, pesticides, pharmaceuticals, and lubricant additives. [0003] The industrialization of 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 condition...

Claims

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Application Information

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Patent Type & Authority Applications(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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