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Process for producing diamine and polyamide

A manufacturing method and technology of polyamide, applied in the field of manufacturing polyamide, can solve the problems of increased environmental load, increased waste liquid treatment cost, low recovery rate of diamine and the like

Active Publication Date: 2014-09-03
TORAY IND INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when the diamine is separated from the salt by the extraction operation, a large amount of organic solvent (for example, aniline, chloroform, etc.) is required, and if it is a diamine with a small distribution coefficient, the recovery rate of the diamine in the organic solvent layer is low, The problem that the extraction operation must be repeated using an organic solvent
Also, after the extraction operation, the organic solvent and the aqueous solution containing the organic solvent are discharged as a large amount of waste liquid, so there are problems such as increased cost of waste liquid treatment and increased environmental load

Method used

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  • Process for producing diamine and polyamide
  • Process for producing diamine and polyamide
  • Process for producing diamine and polyamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～12

[0084] (preparation of 1,4-butanediamine sulfate aqueous solution separated by nanofiltration membrane)

[0085] In 10g / L 1,4-butanediamine sulfate aqueous solution (50L), add 1M calcium hydroxide aqueous solution (manufactured by Wako Pure Chemical Industries, Ltd.) to pH 9, 10, 11, and then Stir for 1 hour at °C. The precipitated calcium sulfate was filtered off by suction filtration with No. 2 qualitative filter paper (manufactured by Advantec), and 50 L of filtrate was recovered.

[0086] (Separation experiment using nanofiltration membrane)

[0087] Next, if figure 1 As shown, 50L of filtrate obtained above is injected into the raw water tank 1 of the membrane filtration device, and when passing through the nanofiltration membrane, the pressure of the high-pressure pump 3 is adjusted to 1MPa, and the permeated water 5 is recovered. Use an ion chromatograph (manufactured by DIONEX) to analyze the concentration of sulfate ions and calcium ions contained in the raw water ...

Embodiment 13～24

[0091] (Preparation of 1,5-pentanediamine sulfate aqueous solution separated by nanofiltration membrane)

[0092] In 10g / L 1,5-pentanediamine sulfate aqueous solution (50L), add 1M calcium hydroxide aqueous solution (manufactured by Wako Pure Chemical Industries, Ltd.) to pH 9, 10, 11, and then Stir for 1 hour at °C. The precipitated calcium sulfate was filtered off by suction filtration with No. 2 qualitative filter paper (manufactured by Advantec), and 50 L of filtrate was recovered.

[0093] (Separation experiment using nanofiltration membrane)

[0094] Next, if figure 1 As shown, 50L of filtrate obtained above is injected into the raw water tank 1 of the membrane filtration device, and when passing through the nanofiltration membrane, the pressure of the high-pressure pump 3 is adjusted to 1MPa, and the permeated water 5 is recovered. Use an ion chromatograph (manufactured by DIONEX) to analyze the concentration of sulfate ions and calcium ions contained in the raw wate...

Embodiment 25～36

[0098] (preparation of 1,6-hexamethylenediamine sulfate aqueous solution with nanofiltration membrane separation)

[0099] To 10 g / L 1,6-hexamethylenediamine sulfate aqueous solution (50 L), 1M calcium hydroxide aqueous solution was added to pH 9, 10, 11 respectively, and then stirred at 25° C. for 1 hour. The precipitated calcium sulfate was filtered off by suction filtration with No. 2 qualitative filter paper (manufactured by Advantec), and 50 L of filtrate was recovered.

[0100] (Separation experiment using nanofiltration membrane)

[0101] Next, if figure 1 As shown, 50L of filtrate obtained above is injected into the raw water tank 1 of the membrane filtration device, and when passing through the nanofiltration membrane, the pressure of the high-pressure pump 3 is adjusted to 1MPa, and the permeated water 5 is recovered. Use an ion chromatograph (manufactured by DIONEX) to analyze the concentration of sulfate ions and calcium ions contained in the raw water tank 1 and...

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Abstract

A method for producing diamine, comprising a process of purifying diamine from an aqueous solution containing diamine salts, including adding an alkaline substance to the aqueous solution, and then filtering the aqueous solution through a nanofiltration membrane to remove salt, thereby obtaining diamine The diamine production method in the amine aqueous solution step can obtain diamine suitable as a polyamide raw material by a simpler operation than the conventional extraction operation using an organic solvent.

Description

technical field [0001] The present invention relates to a method for producing diamine, including a step of purifying diamine from an aqueous solution containing a diamine salt, and a method for producing polyamide using diamine obtained by the method for producing diamine as a raw material. Background technique [0002] Represented by nylon, diamine is used in various fields as a raw material of polyamide. For example, polyamide can be obtained by thermal polycondensation reaction of diamine dicarboxylate with a molar ratio of diamine to dicarboxylic acid of 1:1, but due to the high volatility of diamine as a raw material, it will destroy Because of the molar balance of the dicarboxylic acid, it is necessary to add an excess amount of diamine to the dicarboxylic acid (for example, Patent Document 1). The diamine added here must be a high-purity product that does not damage the physical properties of the polyamide resin. Therefore, a technology that can easily purify diamin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/84C07C211/09
CPCB01D61/58B01D71/60C07C209/84B01D2317/022B01D61/027C08G69/26C08G69/28B01D61/025C07C211/09C07C211/12
Inventor 伊藤正照中川泉加藤公哉耳塚孝泽井健司峯岸进一泽井秀树山田胜成
Owner TORAY IND INC