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A method of extracting 1,5-pentanediamine from a 1,5-pentanediamine salt solution system

A technology for pentamethylenediamine salt and pentamethylenediamine is applied in the field of extracting 1,5-pentamethylenediamine, which can solve the problems of complex process, high cost, low recovery rate and the like, and achieves a simple process, simple operation and strong applicability. Effect

Active Publication Date: 2017-08-15
CATHAY R&D CENT CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to overcome the defects of complex process, high cost and low recovery rate in the existing purification and extraction process of pentamethylenediamine, the object of the present invention is to provide a method for extracting 1,5-pentanediamine method

Method used

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  • A method of extracting 1,5-pentanediamine from a 1,5-pentanediamine salt solution system
  • A method of extracting 1,5-pentanediamine from a 1,5-pentanediamine salt solution system
  • A method of extracting 1,5-pentanediamine from a 1,5-pentanediamine salt solution system

Examples

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Effect test

Embodiment 1

[0088] Get the 1,5-pentamethylenediamine salt enzyme conversion solution of the carrier (wherein, the mass percentage concentration of 1,5-pentamethylenediamine salt is 35%, the sulfate content of 1,5-pentamethylenediamine is 70%, phosphoric acid The content of salt is 10%, the percentage is the molar percentage of 1,5-pentamethylenediamine salt), calcium oxide powder (purity above 90%) is added, and the molar ratio of calcium oxide to 1,5-pentamethylenediamine salt is 1.1: 1. Stir at a temperature of 40°C for 2 hours; then feed into the vacuum scraper drying device of the present invention at a feed rate of 20kg / m 2 / h, the speed of the vacuum scraper drying device is 0.8rpm, the thickness of the scraping film is 1mm, and the temperature of the heat transfer oil is 200°C;

[0089] In the vacuum scraper drying device, the solution system obtained above was evaporated, and the evaporation was carried out under the conditions of a vacuum degree of -0.09 to -0.095 MPa and a tempe...

Embodiment 2

[0092] Take the 1,5-pentanediamine sulfatase conversion solution of the bacteria (wherein, the mass percent concentration of 1,5-pentanediamine salt is 30%), add calcium oxide, calcium oxide and 1,5-pentanediamine The molar ratio of amine salt is 1.2:1, stirring at 40°C for 1.5h; then feeding into the vacuum scraper drying device of the present invention, the feeding speed is 18kg / m 2 / h, speed 2rpm, scraping film thickness 0.8mm, heat transfer oil temperature 200℃;

[0093] In the vacuum scraper drying device, the solution system obtained above was evaporated, and the evaporation was carried out under the conditions of a vacuum degree of -0.08MPa and a temperature of 190°C.

[0094] The yield of pentamethylenediamine is 98.9%.

Embodiment 3

[0096] Take the 1,5-pentamethylenediamine salinase conversion solution of the bacteria, and determine that the mass percent concentration of pentamethylenediamine is 20%. Evaporate on a pressure-0.095MPa rotary evaporator, control the temperature of the water bath at 90°C, concentrate until the mass percentage concentration of 1,5-pentamethylenediamine salt is 15%, add calcium hydroxide, calcium hydroxide 1.05:1, at 25°C Stir at high temperature for 1.5h; then feed into the vacuum scraper drying device of the present invention, feed rate 15kg / m 2 / h, speed 1rpm, scraping film thickness 0.6mm, heat transfer oil temperature 180℃;

[0097] In a vacuum scraper drying device, the above-mentioned solution system was evaporated, and the evaporation was carried out under the conditions of a vacuum degree of -0.08MPa and a temperature of 170°C.

[0098] The yield of pentamethylenediamine is 97.5%.

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Abstract

The invention provides a method of extracting 1,5-pentanediamine from a 1,5-pentanediamine salt solution system. An alkaline compound is added into the 1,5-pentanediamine salt solution system to form a solution system containing free-state 1,5-pentanediamine, and then the solution system containing the free-state 1,5-pentanediamine is distilled / evaporated in a vacuum scraping plate dryer. The degree of vacuum during distillation / evaporation is -0.015 to -0.05 MPa, and the temperature is 120-250 DEG C. The method is suitable for various salt forms of the 1,5-pentanediamine, and is higher in applicability and more cost-competitive. The vacuum scraping plate dryer is adopted as an evaporation device so that the final yield of the pentanediamine is greatly increased. Solid compounds do not influence a distillation / evaporation process. Solid liquid separation after the alkaline compound is added is not required and evaporation is performed directly, thus simplifying the process steps.

Description

technical field [0001] The invention relates to the field of separation and purification of chemical products, in particular to a method for extracting 1,5-pentanediamine from a solution system containing 1,5-pentanediamine salt. Background technique [0002] Pentamethylenediamine (ie, 1,5-pentanediamine, 1,5-diaminopentane, cadaverine, etc.) is an important polymer monomer. Starting from 1,5-pentamethylenediamine, a series of polyamides can be synthesized, such as polyamide 56, polyamide 510, etc., or polyester amide products, which are widely used in textiles, electronic appliances, mechanical equipment, automobiles and other fields. [0003] The production and purification patents of 1,5-pentanediamine include the following reports: [0004] In the patent CN101981202A, pentamethylenediamine is produced by direct fermentation. The fermented liquid was refluxed at 103°C for 5 hours to crack the by-products in the fermented liquid, then extracted with butanol several times...

Claims

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Application Information

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IPC IPC(8): C07C211/09C07C209/00C07C209/86
CPCC07C209/00C07C209/86C07C211/09
Inventor 戴端芳秦兵兵杨晨刘修才
Owner CATHAY R&D CENT CO LTD
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