A method for separating and purifying pentamethylenediamine

A technology for separation and purification of pentamethylenediamine, which is applied in the fields of purification/separation of amino compounds, organic chemistry, etc. It can solve problems such as salt, pigment, and impurity proteins, and achieve the effects of mild desorption conditions, high product quality, and avoiding environmental pollution

Active Publication Date: 2021-02-12
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the present invention is to provide a method for separating and purifying pentamethylenediamine using an adsorption resin to solve the ubiquitous problems of salt, pigment and miscellaneous proteins in the pentamethylenediamine industry

Method used

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  • A method for separating and purifying pentamethylenediamine
  • A method for separating and purifying pentamethylenediamine
  • A method for separating and purifying pentamethylenediamine

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Preparation and pretreatment of pentamethylenediamine conversion solution

[0044] The source of the aqueous solution of the crude product of pentamethylenediamine is not particularly limited, and it can be any conversion solution containing pentamethylenediamine prepared by any biological method, for example, the pentamethylenediamine obtained after lysine or lysine salt is catalyzed by lysine decarboxylase Crude conversion solution. Add one or more of calcium oxide, calcium hydroxide, and sodium hydroxide to the conversion solution to adjust the pH of the system to 12-13.0, and then centrifuge at 6000-8000 rpm for 15-20 minutes to obtain an aqueous solution of pentamethylenediamine.

[0045] The content of pentamethylenediamine in the fermentation broth after the above pretreatment is about 110-120 g / L.

Embodiment 2

[0047] Preparation and pretreatment of modified adsorption resin

[0048] That is, a weakly polar adsorption resin with styrene as a monomer and divinylbenzene as a crosslinking agent is modified with methylamine. The modified adsorption resin has high polarity, good hydrophilicity, and an average particle size of 0.4~0.8mm, water content 41~47wt%, average pore diameter 4.6~6.3nm, porosity 30%~40%, wet density 1.12g / cm 3 , the average specific surface area is 786~862m 2 / g, average pore volume 0.97~1.12cm 3 / g, the functional group is an amine group.

[0049] figure 2 To prepare the breakthrough curve of the resulting modified adsorption resin; image 3 To prepare the infrared spectrum of the modified adsorption resin.

[0050] Pretreatment of the modified adsorption resin: wash the resin with ethanol at a flow rate of 2BV / h, wash away the ethanol with deionized water, and set aside.

[0051] Table 1 Adsorption performance parameter table of adsorption resin

[0052] ...

Embodiment 3

[0054] Fixed bed resin column separation

[0055] The concentration of the pentamethylenediamine conversion liquid after the pretreatment of Example 1 is 118g / L, and the adsorption column equipped with the modified adsorption resin after the pretreatment of Example 2 is passed from top to bottom at a flow rate of 4BV / h, using a fixed bed Adsorption, the ratio of height to diameter of the resin column is 15, pentamethylenediamine is selectively adsorbed, and the feeding is stopped after the adsorption is saturated; the liquid in the column is drained, and the impurities are washed with deionized water at a flow rate of 2BV / h until the effluent is It does not contain impurities such as inorganic salts and residual sugar. The consumption of detergent is 1.5BV, and then the deionized water is drained; deionized water is added dropwise to the top of the adsorption column at a flow rate of 0.5BV / h for desorption. When the desorption effluent When the concentration of pentamethylened...

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Abstract

The invention discloses a method for separating and purifying pentamethylenediamine. The pretreated pentamethylenediamine conversion solution is passed through an adsorption column equipped with an adsorption resin. After the adsorption is saturated, water is used as a washing agent to wash impurities, and water is used as a desorbing agent. Desorb the pentamethylenediamine solution to obtain an aqueous solution of pentamethylenediamine, and then directly enter the aqueous solution of pentamethylenediamine into a rectification tower for rectification to obtain pure pentamethylenediamine; wherein, the adsorption resin is based on styrene or acrylate body, divinylbenzene is used as a cross-linking agent to obtain a weakly polar adsorption resin; or, a polar adsorption resin obtained by using an aminating agent to modify the weakly polar adsorption resin with amine groups; the resin Stable physical and chemical properties, insoluble in acid, alkali and organic solvents, not affected by inorganic salts and strong ionic low-molecular compounds; the above-mentioned adsorption resin has an average particle size of 0.4-0.8mm and a water content of 41-47wt%. The average pore diameter is 4.6-6.3nm, the porosity is 30%-40%, and the wet density is 1.12g / cm 3 , with an average specific surface area of ​​786‑862m 2 / g, average pore volume 0.97~1.12cm 3 / g.

Description

technical field [0001] The invention belongs to the field of biotechnology, in particular to a method for separating and purifying pentamethylenediamine. Background technique [0002] 1,5-pentamethylenediamine, similar to hexamethylenediamine, is polymerized with dibasic acid to produce nylon 5X (nylon 54, nylon 56, etc.), the performance is comparable to or even surpasses the classic nylon 66, and its main application fields are fibers (such as clothing, automobiles, etc.) Tire cords, carpets and pipes, etc.) and engineering plastics (such as electronic instrument products and automotive parts, etc.). 1,5-Pentanediamine, which can be produced from biomass through biological methods, can be polymerized with adipic acid to obtain nylon 56, which is considered to be the most likely to replace or supplement nylon 66 due to its good performance. product. Bio-based nylon 56 is polymerized from adipic acid and pentamethylenediamine, of which pentamethylenediamine is produced by ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/84C07C211/09
Inventor 应汉杰崔琳琳代坤吴菁岚杨朋朋李子涵曹翰飞庄伟
Owner NANJING TECH UNIV
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