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A method for adsorbing and separating pentamethylenediamine by using ultra-high cross-linked resin

An ultra-high cross-linked resin, adsorption and separation technology, applied in the biological field, can solve the problems of difficult downstream separation, achieve large adsorption capacity, avoid environmental pollution problems, and have long service life

Active Publication Date: 2019-01-22
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a method for extracting pentamethylenediamine from the fermentation broth to solve the downstream separation problem in the pentamethylenediamine industry

Method used

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  • A method for adsorbing and separating pentamethylenediamine by using ultra-high cross-linked resin
  • A method for adsorbing and separating pentamethylenediamine by using ultra-high cross-linked resin
  • A method for adsorbing and separating pentamethylenediamine by using ultra-high cross-linked resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Preparation and pretreatment of pentamethylenediamine fermentation broth

[0043] The source of the aqueous solution of the crude product of pentamethylenediamine is not particularly limited, and it can be any fermentation broth 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. The transformation solution was centrifuged to remove the bacteria, and the supernatant was added with 1.5% (g / L) activated carbon and stirred at 20°C for 1 hour to decolorize, then centrifuged at 6000-8000rpm for 5-10 minutes, and then filtered to remove the activated carbon , and then add enough NaOH to free pentamethylenediamine, and adjust the pH to 12.5-13.5.

[0044] The content of pentamethylenediamine in the pentamethylenediamine fermentation broth after the above pretreatment is about 70g / L.

Embodiment 2

[0046] Preparation and pretreatment of ultra-high cross-linked resin HD-6

[0047]The preparation method of the ultra-high cross-linked resin can be found in the patent CN105884956A, that is, polystyrene-divinylbenzene is used as the skeleton, and it is obtained through the Friedel-Crafts cross-linking reaction. The ultra-high cross-linked resin has weak polarity and hydrophilicity Good; the average particle size is 0.5-0.8mm, the water content is 43wt%, the average pore size is 4.94nm, the porosity is 30%-40%, and the wet density is 1.09g / cm 3 , with an average specific surface area of ​​806m 2 / g, average pore volume 0.995cm 3 / g, the functional group is carbonyl, named HD-6.

[0048] figure 2 To prepare the pore size distribution figure of the resulting ultra-high cross-linked resin HD-6; image 3 To prepare the BET figure of the super high cross-linked resin HD-6.

[0049] Pretreatment of ultra-high cross-linked resin HD-6: wash the resin with 2BV 1mol / L HCL solution...

Embodiment 3

[0051] Fixed bed resin column separation

[0052] The pentamethylenediamine fermentation broth after the pretreatment of Example 1 is passed through the adsorption column equipped with the ultra-high cross-linked resin after the pretreatment of Example 2 from top to bottom at a flow rate of 4BV / h, using fixed bed adsorption, and the resin column The aspect ratio is 15, pentamethylenediamine is selectively adsorbed, stop feeding when the feed volume reaches 4BV, and drain the liquid in the column; wash impurities with deionized water at a flow rate of 2BV / h until the effluent No inorganic salts, residual sugar and other impurities, then drain the deionized water; add 0.5mol / L adipic acid aqueous solution to the top of the adsorption column at a flow rate of 0.5BV / h, after desorption, there is basically no glutaric acid in the effluent Amines, desorption is complete. Desorption curve see Figure 4 . Then, deionized water is fed at a flow rate of 1BV / h to clean the adipic acid...

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Abstract

The invention discloses a method for separating pentamethylene diamine by utilizing ultrahigh crosslinking resin absorption. The method comprises the following steps: causing a preprocessed pentamethylene diamine fermentation liquor pass by an adsorption column filled with ultrahigh crosslinking resin, absorbing, cleaning impurities and desorbing, thereby acquiring a pentamethylene diamine adipic acid solution. According to the method provided by the invention, the adsorption column is adopted for separating the pentamethylene diamine from the fermentation liquor; all the operations can be performed under room temperature; the energy consumption in the separating process and the dosage of the organic extraction agent are greatly reduced; the selected adsorbing medium has the advantages of high adsorption capacity for pentamethylene diamine, high physical-chemical property stability, high adsorptive selectivity, mild desorbing condition, easiness in regeneration, long service life, and the like; the used adsorption column can be regenerated by using water; the acid-base or organic solvent need not be consumed; the energy consumption can be reduced and the wastewater discharge can be reduced; the problem of environmental pollution is avoided; the method is a more clean and environment-friendly production technique.

Description

technical field [0001] The invention belongs to the field of biotechnology, in particular to a method for adsorbing and separating pentamethylenediamine by using an ultra-high cross-linked resin. Background technique [0002] The chemical industry has always relied on oil and natural gas as raw materials to produce polymer products, which has become an important pillar of modern civilized society. However, with the gradual depletion of oil and natural gas resources and the increasing greenhouse effect caused by the production and use of petroleum products, finding alternatives to petrochemical resources, especially green products based on renewable resources, has become an important development direction of the chemical industry today. Nylon is a very important polymer material, which has important uses in many fields such as automobiles and high-grade textiles. At present, the annual output of nylon polymers in the world is more than 6 million tons, and China's consumption ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/00B01J20/26B01J20/28C07C209/86C07C211/09
CPCB01D15/00B01J20/267B01J20/28016B01J20/28064B01J20/28073B01J20/28076B01J20/28083C07C209/86C07C211/09
Inventor 应汉杰姜康康吴菁岚杨朋朋陈可泉陈勇朱晨杰柳东
Owner NANJING TECH UNIV
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