Separation method for mixture of triethylene-diamine and ethanolamine

A technology of triethylenediamine and separation method, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of amino hydroxyl compounds, etc., to achieve the effect of simple separation operation process

Inactive Publication Date: 2012-07-18
山西玉龙化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Separation method for mixture of triethylene-diamine and ethanolamine
  • Separation method for mixture of triethylene-diamine and ethanolamine
  • Separation method for mixture of triethylene-diamine and ethanolamine

Examples

Experimental program
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Embodiment 1

[0020] The feed material containing triethylenediamine and ethanolamine and the entrainer recycle stream are fed from the middle of the azeotropic rectification tower. The azeotropic rectification tower is a packed tower with a diameter of Φ25mm and a built-in Φ3*3θ ring stainless steel filler. The packing layer Height 0.8m. The top of the azeotropic distillation column is the azeotrope of the entrainer and ethanolamine, which enters the phase separator, and the distillate in the bottom of the tower is triethylenediamine product; the operating pressure of the phase separator is 100kPa, and the operating temperature is 30°C. The upper layer is the p-xylene phase, which is recycled to the middle of the azeotropic distillation column for feeding, and the lower layer is the crude product of ethanolamine, which enters the ethanolamine refining tower; the lower layer of the phase separator is fed from the middle of the ethanolamine refining tower, which is a packed tower , the tower...

Embodiment 2

[0028] The operation process of Example 2 is similar to that of Example 1, except that the operating parameters of the azeotropic distillation column and the ethanolamine refining column are different. The operating parameters are shown in Table 3, and the stream composition of Example 2 is shown in Table 4.

[0029] Tower operation parameter in the embodiment 2 of table 3

[0030]

[0031] The logistics composition in the embodiment 2 of table 4

[0032]

Embodiment 3

[0034] The operation process of Example 3 is similar to that of Example 1, except that the mass ratio of entrainer to ethanolamine is 15:1, and the stream composition of Example 3 is shown in Table 5.

[0035] The logistics composition in the embodiment 3 of table 5

[0036]

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Abstract

Provided is a separation method for a mixture of triethylene-diamine and ethanolamine. In the method, dimethylbenzene or ethylbenzene serves as an entrainer, and the mixture of triethylene-diamine and ethanolamine is separated through heterogeneous azeotropic rectification. The method includes the following steps: 1 the mixture and the entrainer of triethylene-diamine and ethanolamine enter an azeotropic rectifying tower, overhead fraction is an azeotrope of the entrainer and ethanolamine, and tower kettle fraction is triethylene-diamine product; 2 the overhead fraction of the azeotropic rectifying tower enters a phase segregator for phase segregation, the upper layer is the entrainer and circulated to the azeotropic rectifying tower, and the lower layer is ethanolamine crude product and enters an ethanolamine refining tower; and 3 overhead fraction of the ethanolamine refining tower is an azeotrope of the entrainer and ethanolamine and circulated to the azeotropic rectifying tower, and tower kettle fraction is ethanolamine product. The method is suitable for separating the triethylene-diamine and ethanolamine mixture obtained through amination reaction with ethanolamine and liquid ammonia as raw materials.

Description

technical field [0001] The invention relates to a method for separating a mixture of triethylenediamine and ethanolamine, in particular to a method for separating a mixture of triethylenediamine and ethanolamine obtained by amination reaction using ethanolamine and liquid ammonia as raw materials. Background technique [0002] Triethylenediamine is an important fine chemical, which is widely used as a blowing agent for polyurethane soft, semi-rigid and rigid foams, as well as ethylene polymerization catalysts, acrylonitrile polymerization catalysts, epoxy catalysts, and epoxy resin curing agents etc., and its derivatives can also be used in the production of petroleum additives, corrosion inhibitors, emulsifiers, etc. [0003] 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 ethanola...

Claims

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Application Information

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IPC IPC(8): C07D487/08C07C215/08C07C213/10
Inventor 吕剑曾纪珺张伟郝志军王博王伟赵锋伟孙道安袁俊
Owner 山西玉龙化工有限公司
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