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Method for separating triethylene diamine and ethanolamine

A technology of triethylenediamine and separation method, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as triethylenediamine and ethanolamine not being retrieved, and achieves reduced energy consumption and simple steps. Effect

Active Publication Date: 2013-03-20
山西玉龙格兰特化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] According to the information search done by the applicant, no information about the method of extracting and rectifying the separation of triethylenediamine and ethanolamine was found

Method used

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  • Method for separating triethylene diamine and ethanolamine

Examples

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Embodiment 1

[0023] The azeotrope of triethylenediamine and ethanolamine (mass percentage: triethylenediamine 70%, ethanolamine 30%) is fed from the lower part of the extraction tower at a flow rate of 100kg / h and a temperature of 90°C. The fresh extractant DMSO is After the flow rate of 197.95kg / h is mixed with the circulating extractant stream from the rectification tower, it is added from the upper part of the extraction tower at a temperature of 25°C. The two are in reverse contact in the extraction tower filled with packing. The pressure of the extraction tower is 30kPa. The top temperature is 112.6°C, the temperature of the tower kettle is 132.2°C, the material in the tower kettle is a mixture of DMSO and ethanolamine, and the mass percentage of the mixture of DMSO and ethanolamine is: ethanolamine 9%, DMSO 91%, and the mixture enters the refinery at 712.87kg / h Distillation tower; the mixture of triethylenediamine and DMSO is extracted from the top of the tower, and the recovery rate ...

Embodiment 2

[0025] The azeotrope of triethylenediamine and ethanolamine (mass percentage composition is: triethylenediamine 68%, ethanolamine 32%) with 100kg / h flow velocity, temperature is that 60 ℃ are fed from the lower part of extraction tower, fresh extraction agent 1, After mixing 3-dimethylimidazolinone with the circulating extractant stream from the rectification tower at a flow rate of 57.99kg / h, it is added from the upper part of the extraction tower at a temperature of 25°C, and the two are in reverse contact in the extraction tower filled with packing , the pressure of the extraction tower is 20kPa, the temperature at the top of the tower is 103.2°C, and the temperature of the tower kettle is 126.2°C. The material in the tower kettle is a mixture of 1,3-dimethylimidazolinone and ethanolamine, wherein the mass percentage of the mixture is: ethanolamine: 21%, 1,3-dimethylimidazolinone: 79%, the mixture enters the rectification tower at 299.64kg / h; the mixture of triethylenediamin...

Embodiment 3

[0028]The azeotrope of triethylenediamine and ethanolamine (mass percentage: triethylenediamine 70%, ethanolamine 30%) is fed from the lower part of the extraction tower at a flow rate of 100kg / h and a temperature of 60°C. Fresh extractant N- After methylpyrrolidone is mixed with the circulating extractant stream from the rectification tower at a flow rate of 176.45kg / h, it is added from the upper part of the extraction tower 1 at 25°C, and the two are in reverse contact in the extraction tower filled with packing. The pressure is 15kPa, the temperature at the top of the tower is 97.2°C, and the temperature at the bottom of the tower is 118.13°C. The material in the bottom of the tower is a mixture of N-methylpyrrolidone and ethanolamine, and the mass percentage of the mixture is: ethanolamine 9%, N-methylpyrrolidone 91%, the mixture enters the rectifying tower at 612.18kg / h; the mixture of triethylenediamine and N-methylpyrrolidone is produced at the top of the tower, and the ...

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Abstract

The invention relates to a method for separating triethylene diamine and ethanolamine. The equipment adopted for separating the triethylene diamine and the ethanolamine comprises an extracting tower, a rectifying tower and a heat exchanger. The method comprises the following steps of: feeding the azeotrope of the triethylene diamine and ethanolamine from the lower part of the extracting tower, and feeding an extracting agent from the upper part of the extracting tower, wherein the azeotrope of the triethylene diamine and ethanolamine and the extracting agent are in reverse contact in the extracting tower filled with a filler, and the extracting agent is one of the N-methylpyrrolidone, 1,3-dimethyl-imidazolidinone, DMSO and N, N-dimethyl acetamide; extracting the mixture of the triethylene diamine and the extracting agent from the top of the extracting tower; cooling, filtering and collecting a solid to obtain the pure triethylene diamine; adjusting the temperature of the mixture of the extracting agent in the extracting tower and the ethanolamine to the bubble point temperature; feeding from the middle part of the rectifying tower; rectifying and separating in the rectifying tower; and separating from the top of the rectifying tower to obtain the ethanolamine; and making the extracting agent flow out of the bottom of the rectifying tower, wherein one part of the extracting agent is made to circulate into the extracting tower, and the other part is discharged.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for separating triethylenediamine and ethanolamine. Background technique [0002] Triethylenediamine is a foaming agent for the production of polyurethane soft, semi-rigid, and rigid foams, and is also used in ethylene polymerization catalysts, coatings, and plastic products. [0003] At present, the main raw materials for the preparation of triethylenediamine are N-hydroxyethylpiperazine, ethylenediamine, ethanolamine, piperazine and the like. When ethanolamine and liquid ammonia are used as raw materials to catalyze amination to synthesize ethylenediamine or piperazine, triethylenediamine can be co-produced. Since the boiling points of triethylenediamine (boiling point: 174°C) and ethanolamine (boiling point: 170°C) are very close, the two are easy to form an azeotrope, and it is difficult to separate them by conventional distillation methods. T...

Claims

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Application Information

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IPC IPC(8): C07D487/08C07C215/08C07C213/10
Inventor 杨建明吕剑梅苏宁王伟余秦伟王为强赵锋伟刘亚妮马贺
Owner 山西玉龙格兰特化工有限公司