Method for preparing 1,5-pentanediamine

A technology for pentamethylenediamine and pentamethylenediamine salt, which is applied in the field of preparation of 1,5-pentamethylenediamine, can solve the problems of low product purity, high production cost, high environmental protection pressure, etc., achieves high overall yield and reduces environmental protection Pressure, the effect of reducing the cost of raw materials

Active Publication Date: 2018-12-14
河北美邦工程科技股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a preparation method of 1,5-pentanediamine to solve the problems of high environmental protection pressure, high production cost and relatively low product purity in the existing method

Method used

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  • Method for preparing 1,5-pentanediamine
  • Method for preparing 1,5-pentanediamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A, 250g lysine hydrochloride is dissolved in water, obtains the lysine hydrochloride aqueous solution that pH value is 6.6;

[0031] b. Add lysine decarboxylase and pyridoxal phosphate to the lysine hydrochloride aqueous solution obtained in step a, and perform enzymatic decarboxylation of lysine at 32°C to obtain 1,5-pentanediamine Hydrochloride solution, adding hydrochloric acid solution during the reaction to maintain a pH value of 6.6;

[0032] Among them, the dosage of lysine decarboxylase is 3% of the mass of lysine salt, the dosage of vitamin B6 coenzyme is 6.5‰ of the mass of lysine salt, and the conversion rate of lysine is 99.96%.

[0033] c, using an ultrafiltration membrane with a molecular weight cut-off of 5000 to filter the 1,5-pentanediamine hydrochloride solution obtained in step b to obtain a 1,5-pentanediamine hydrochloride ultrafiltrate containing pyridoxal phosphate and lysine decarboxylase solution, the separated lysine decarboxylase solution is r...

Embodiment 2

[0041] A, 340g lysine sulfate is dissolved in water, obtains the lysine sulfate aqueous solution that pH value is 6.1;

[0042] b. Add lysine decarboxylase and pyridoxal to the lysine sulfate aqueous solution obtained in step a, and perform enzymatic decarboxylation of lysine at 36° C. to obtain 1,5-pentamethylenediamine sulfate Solution, add sulfuric acid solution in reaction process and maintain pH value to be 6.1;

[0043] Wherein, the dosage of lysine decarboxylase is 4% of the mass of lysine sulfate, the dosage of pyridoxal is 5‰ of the mass of lysine sulfate, and the conversion rate of lysine is 99.91%.

[0044] c, the 1,5-pentanediamine sulfate solution obtained in step b is filtered using an ultrafiltration membrane with a molecular weight cut-off of 6000 to obtain the 1,5-pentanediamine sulfate ultrafiltrate containing pyridoxal and lysine Acid decarboxylase solution, the separated lysine decarboxylase solution is recycled after treatment;

[0045] d, using LXT-021 ...

Embodiment 3～4、 comparative example 1～2

[0052] The current density and temperature of the two-chamber bipolar membrane electrodialysis device were changed (see Table 1 for details), and other conditions were the same as in Example 1. The test results are shown in Table 1.

[0053] Table 1:

[0054]

[0055] It can be seen from Table 1 that the present invention adopts the bipolar membrane electrodialysis desalination technology with specific conditions to significantly improve the product purity, and under the current density and temperature conditions of the present invention, it can ensure that the obtained product has a higher purity (>99.5%) and Yield (>99.2%), beyond the current density and temperature range limited by the present invention, the product purity and yield are obviously reduced.

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Abstract

The invention provides a method for preparing 1,5-pentanediamine. The method comprises the steps of: a, dissolving lysine salt to obtain an aqueous solution of lysine salt; b, adding lysine decarboxylase and vitamin B6 coenzyme to the aqueous solution of lysine salt for a decarboxylation reaction of lysine; c. filtering a 1,5-pentanediamine salt solution obtained in step b by using an ultrafiltration membrane having a interception molecular weight being 3000-6000; d. selectively adsorbing vitamin B6 coenzyme in a 1,5-pentanediamine salt ultrafiltrate obtained in step c by using macroporous adsorption resin; e, sending the enzyme-removed 1,5-pentanediamine salt solution obtained in step d to a two-chamber bipolar membrane electrodialysis device for desalting; and f. performing concentrationand dehydration on the 1,5-pentanediamine aqueous solution obtained in the step e, then performing vacuum distillation, and performing condensation on a light phase to obtain a 1,5-pentanediamine product. The preparation method of the invention has the advantages of low cost, small environmental protection pressure, and high product purity, and is suitable for industrial application.

Description

technical field [0001] The invention relates to the technical field of organic chemistry, in particular to a preparation method of 1,5-pentanediamine. Background technique [0002] 1,5-pentamethylenediamine (pentamethylenediamine) can be used in the preparation of high polymers, as intermediates in organic synthesis, curing agents for epoxy resins, etc., and can also be used in biological research. Among them, the synthesis of nylon polymers is an important application of pentamethylenediamine, and 1,5-pentamethylenediamine can be used to synthesize nylon 56 and fully bio-based nylon 510. These products can be widely used in electronic appliances, mechanical equipment, automotive parts, etc. field. At present, the annual output of nylon polymer in the world is more than 6 million tons, and China's consumption accounts for 30% of the global nylon output, so the consumption of 1,5-pentanediamine is also very large. [0003] At present, the main raw material for the productio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/84C07C209/86C07C211/09C12P13/00
CPCC07C209/84C07C209/86C12P13/001C07C211/09
Inventor 刘东闫利军卢远峰魏朝帅张玉妹高文杲张玉新金作宏刘永英李彦欣
Owner 河北美邦工程科技股份有限公司
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