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Method for recovering 1,4-butanediol from waste liquor generated in production of 1,4-butanediol through Reppe method

A technology of butanediol and Rapper method, which is applied in the field of organic waste liquid recycling, can solve the problems of unsuitable treatment of small batches of waste liquid recycling and utilization, high equipment investment and operating costs, and long process, so as to facilitate popularization and application , Conducive to environmental protection and low recycling cost

Inactive Publication Date: 2012-09-12
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] German patent DE 19950991 discloses a method for continuous rectification recovery and purification of 1,4-butanediol with three rectification and vacuum towers, through which a high-purity 1,4-butanediol with a mass percentage of 99% is obtained Alcohol products, but this method adopts a continuous rectification process and requires three rectification towers, which has a long process, high equipment investment and high operating costs, and is not suitable for the recovery and utilization of small batches of waste liquid

Method used

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  • Method for recovering 1,4-butanediol from waste liquor generated in production of 1,4-butanediol through Reppe method
  • Method for recovering 1,4-butanediol from waste liquor generated in production of 1,4-butanediol through Reppe method

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Embodiment 1

[0022] To the waste liquid (raw material) of 1,4-butanediol produced by the Rapper method, add the additive sodium carbonate according to the mass ratio of the additive to the raw material as 3:600, stir and mix evenly, and put the mixture into the still of the batch rectification tower , the batch distillation is operated under the following conditions:

[0023] (1) When the temperature of the tower bottom is 66-105°C, the temperature of the tower top is 47-100°C, the normal pressure, and the reflux ratio are 0.1-0.14, the light components mainly composed of water are extracted from the top of the tower, which contains a small amount of Tetrahydrofuran, methanol;

[0024] (2) When the temperature at the bottom of the tower is 105-200°C, the temperature at the top of the tower is 100-185°C, the absolute pressure at the top of the tower is 91.33kPa, and the reflux ratio is 0.2-0.35, extract the dihydric fusel alcohol from the top of the tower;

[0025] (3) When the temperature...

Embodiment 2～4

[0028] Operating conditions are identical with embodiment 1, and difference is that sodium carbonate and raw material mass ratio are respectively 1: 600, 5: 600, 7: 600, respectively extract 1, the mass percent of 4-butanediol product and reclaim Efficiency is also not the same, and the mass percent of the 1,4-butanediol product that embodiment 2, embodiment 3, embodiment 4 are extracted is respectively 89.38%, 93.39%, 93.41%, and the rate of recovery is respectively 74.48%, 77.83% %, 77.84%.

Embodiment 5～8

[0030] Operating conditions are identical with embodiment 1, and difference is that additive is sodium hydroxide, and the mass ratio of sodium hydroxide and raw material is respectively 3: 600, 5: 600, 7: 600, 9: 600, respectively extracts 1 , the mass percent of 4-butanediol product and the rate of recovery are also not the same, and the mass percent of the 1,4-butanediol product of embodiment 5, embodiment 6, embodiment 7, embodiment 8 mining is respectively 72.84% , 75.67%, 80.09%, 78.05%, the recoveries were 60.70%, 63.06%, 66.74%, 65.04%, respectively.

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Abstract

The invention discloses a method for recovering 1,4-butanediol from a waste liquor generated in production of 1,4-butanediol through a Reppe method. The method comprises the following steps: (1) adding an alkaline substance serving as an additive into a raw material, namely the waste liquor generated in production of 1,4-butanediol, ensuring that the mass ratio of the additive to the raw material is (1-9):600, and stirring and mixing uniformly; and (2) putting the mixture into an intermittent rectifying tower for intermittent rectification, and recovering the 1,4-butanediol. The method has the advantages that: (1) a small amount of additive is added, so that the mass percentage of a 1,4-butanediol product and the recovery rate of the 1,4-butanediol are obviously improved; (2) only one piece of intermittent rectifying equipment is used, and the technological operation is flexible, simple and convenient; (3) the additive is cheap and readily available, low in recovery cost and high in economy; (4) the process application range is wide, the method is suitable for recovering and purifying the 1,4-butanediol from waste liquors in different concentration generated in the production of the 1,4-butanediol through the Reppe method, and the recovery rate can reach 80 percent; and (5) the waste liquor resource is fully utilized, the waste emission is reduced to the greatest extent, and the method is favorable for protecting environment and convenient to promote and apply.

Description

Technical field [0001] The invention belongs to the technical field of organic waste liquid recovery and utilization in industrial production, and in particular relates to a method for recovering 1,4-butanediol from the waste liquid of 1,4-butanediol produced by the Rapper method. Background technique [0002] 1,4-Butanediol, also known as 1,4-dihydroxybutane, butylene glycol, English name 1,4-Butanediol, 1,4-Dihydroxybutane, referred to as BDO, is an important organic fine chemical product, Widely used in solvents, medicines, cosmetics, plasticizers, curing agents, pesticides, herbicides, foam artificial leather, fibers, engineering plastics, etc., mainly used in the production of tetrahydrofuran (THF), γ-butyrolactone (GBL), Polyurethane (TPU), polybutylene terephthalate (PBT), plasticizers and pharmaceutical intermediates have broad market prospects. [0003] The methods for industrial production of 1,4-butanediol mainly include: (1) the Reppe method (Reppe method) using...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/80C07C29/94
Inventor 刘跃进张光文李勇飞陈桂夏迪
Owner XIANGTAN UNIV
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