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A kind of separation method of 1,5-pentanediamine

A separation method, the technology of pentamethylenediamine, applied in the direction of amino compound purification/separation, organic chemistry, etc., can solve the problems of high cost, low recovery rate, low yield, etc., to reduce pollution and separation cost, easy to handle, contain mixed low effect

Active Publication Date: 2020-09-22
CATHAY R&D CENT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the cost can be greatly reduced, a large amount of 1,5-pentanediamine will be encapsulated or entrapped in the solid inorganic salt, so that the free 1,5-pentanediamine cannot be effectively recovered, for example, vacuum filtration is used to remove the solid After the salt, the distillation recovery efficiency of 1,5-pentanediamine is only about 20%, the yield is low, and a large amount of products are wasted
[0011] The above-mentioned methods for the separation and recovery of 1,5-pentanediamine have the defects of low recovery rate, high impurity content in finished products, high cost, high energy consumption, serious environmental pollution, etc. The separation and recovery method of 1,5-pentanediamine with low cost and pollution has become a problem to be solved urgently in the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0167] (1) 50g of 1,5-pentanediamine enzyme conversion solution was added to a 250mL Erlenmeyer flask, the concentration of 1,5-pentanediamine was 2.5wt%, the pH value was 8.1, and the absorbance at 340nm was determined to be 2.7; in the solution Add 30mL732 strong acid cation exchange resin (pH3.0), stir for 10min at 25℃, filter with filter paper, and sample the obtained clear liquid for detection. The concentration of 1,5-pentanediamine in the solution is 2000ppm;

[0168] (2) The resin obtained by filtration was added to 150 mL of sodium hydroxide aqueous solution (concentration 2%), stirred at 60°C, and after 10 minutes, the concentration of 1,5-pentanediamine in the solution was determined to be 7000 ppm; The clear solution of 1,5-pentanediamine, the absorbance of the clear solution of 1,5-pentanediamine at 340nm was determined to be 0.15, and most of the color was removed during the adsorption and desorption process.

Embodiment 2

[0170] (1) Add 1g of 1,5-pentanediamine to a 250mL Erlenmeyer flask, add 30g of water, adjust the pH to pH 10 with 30% sulfuric acid, add water to the solution to a total of 50g; add 30mL D110 (Shanghai Huazhen) weak acidity to the solution Cation exchange resin (pH 7.1), stirred for 10 minutes at room temperature, filtered with filter paper, and the obtained clear liquid was sampled and tested. The concentration of 1,5-pentanediamine in the solution was 3000 ppm;

[0171] (2) The resin obtained by filtration was added to 150 mL of sodium hydroxide aqueous solution (concentration 2%), stirred at 60° C. for 10 min, filtered with filter paper, and the concentration of 1,5-pentanediamine in the filtrate was determined to be 7000 ppm.

Embodiment 3

[0173] (1) 100 mL of 1,5-pentanediamine enzyme conversion solution, centrifuged in a centrifuge at 4000 rpm for 15 minutes, separated the bacteria, and obtained the supernatant; take 60g of the supernatant and determine its 1,5-pentanediamine concentration At room temperature, the supernatant was added to a diameter of 3cm, a height of 60cm, and 200mL strong acid cationic resin (Su Qing, 001*7, styrene) at a feed rate of 2BV / h at room temperature. In a macroporous (pH3.5) separation column, after the addition is complete, wash the resin column with 2BV of water; combine the adsorption effluent and the washing solution, and determine 1,5-pentanediamine by gas chromatography;

[0174] (2) Use 60mL of 3% sodium hydroxide solution to flow through the resin at a rate of 1BV / h at 60°C, and then wash the resin with 600mL of water at a rate of 2BV / h. Collect all effluents totaling 653g, The content of 1,5-pentanediamine was determined to be 2700ppm;

[0175] (3) Evaporate the obtained fil...

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Abstract

The invention discloses a separation method for 1,5-pentanediamine. The separation method comprises the following steps: (1) contacting a 1,5-pentanediamine solution with cationic resin and carrying out adsorption; and (2) eluting 1,5-pentanediamine adsorbed onto the resin. Compared with the prior art, the separation and recovery method for 1,5-pentanediamine in the invention increases the yield of 1,5-pentanediamine; a treated solution obtained after adsorption by resin is basically free of 1,5-pentanediamine residues and the resin does not adsorb tetrahydropyridine, thalli, proteins and other impurities, so separated 1,5-pentanediamine is high in purity and low in impurity content; and the treated solution obtained after resin adsorption does not contain any polar organic solvent, so thesolution is free of harm to environment and easy to treat, and environmental pollution and separation cost are reduced. Meanwhile, a 1,5-pentanediamine diacid solution obtained after elution with diacid can be directly used as a raw material for synthesis of high-performance polyamide.

Description

Technical field [0001] The invention relates to the field of separation and purification of organic matter, in particular to a separation method of 1,5-pentanediamine. Background technique [0002] For a long time, the chemical industry has 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, the greenhouse effect caused by the production and use of petroleum products has become more and more serious. Looking for alternative products of petrochemical resources, especially green products based on renewable resources, has become an important development direction of today's chemical industry. [0003] Polyamide is a very important type of polymer material, which has important applications in many fields such as automobiles and high-end textiles. At present, the global annual output of polyamide polymers is more than 6 million t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/86C07C211/09
CPCC07C209/86C07C211/09
Inventor 李晓明秦兵兵刘修才
Owner CATHAY R&D CENT CO LTD
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