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Separation method for 1,5-pentanediamine

A separation method, pentamethylenediamine technology, applied in 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, high purity high effect

Active Publication Date: 2018-07-13
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) 50 g of 1,5-pentanediamine enzyme conversion solution was added into a 250 mL Erlenmeyer flask, the concentration of 1,5-pentanediamine was 2.5 wt %, the pH value was 8.1, and its absorbance at 340 nm was determined to be 2.7; in the solution Add 30mL732 strongly acidic cation exchange resin (pH3.0), stir at 25°C for 10min, filter with filter paper, and take a sample of the obtained supernatant, the concentration of 1,5-pentanediamine in the solution is 2000ppm;

[0168] (2) Add the resin obtained by filtration into 150mL sodium hydroxide aqueous solution (concentration 2%), stir at 60°C, and after 10min, measure the concentration of 1,5-pentanediamine in the solution to be 7000ppm; filter through filter paper to obtain The serum of 1,5-pentanediamine, the absorbance of the serum of 1,5-pentanediamine at 340nm was determined to be 0.15, and most of the color was removed during the process of adsorption and desorption.

Embodiment 2

[0170] (1) Add 1g of 1,5-pentanediamine into a 250mL Erlenmeyer flask, add 30g of water, adjust the pH to pH10 with 30% sulfuric acid, add water to a total of 50g of the solution; add 30mL of D110 (Shanghai Huazhen) weak acid to the solution Cation exchange resin (pH7.1), stirred at room temperature for 10 minutes, filtered through filter paper, and the obtained clear liquid was sampled for detection, and the concentration of 1,5-pentanediamine in the solution was 3000ppm;

[0171] (2) Add the filtered resin to 150mL sodium hydroxide aqueous solution (concentration: 2%), stir at 60°C for 10min, filter through filter paper, and measure the concentration of 1,5-pentanediamine in the filtrate to be 7000ppm.

Embodiment 3

[0173] (1) 100mL of 1,5-pentanediamine enzyme conversion solution was centrifuged in a centrifuge at 4000rpm for 15min to separate the bacteria to obtain a supernatant; take 60g of the supernatant and measure its 1,5-pentanediamine concentration 3.1wt%, pH 7.8; under room temperature, the supernatant was added to a diameter of 3cm, a height of 60cm, filled with 200mL strong acid cationic resin (Su Qing, 001*7, styrene In the separation column of macroporous pH3.5), after the feeding is finished, the resin column is washed with 2BV of water; the adsorption effluent and washing liquid are combined, and gas chromatographic determination shows that 1,5-pentanediamine cannot be detected;

[0174] (2) Use 60mL of 3% sodium hydroxide solution to flow through the resin at a speed of 1BV / h at 60°C, then wash the resin with 600mL of water at a speed of 2BV / h, and collect all the effluents to a total of 653g, Measure its 1,5-pentanediamine content to be 2700ppm;

[0175] (3) Evaporate t...

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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] 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, the greenhouse effect caused by the production and use of petroleum products is becoming more and more serious. Finding alternatives to petrochemical resources, especially green products based on renewable resources, has become an important development direction of the chemical industry today. [0003] Polyamide is a very important polymer material, which has important uses in many fields such as automobiles and high-end textiles. At present, the annual output of polyamide polymers in the world is more than 6 million tons, and China's consu...

Claims

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Application Information

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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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