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Preparation method and product of ethylenediamine

A technology of ethylenediamine and ethylenediamine hydrochloride, which is applied to the preparation of amino compounds from amines, the purification/separation of amino compounds, organic chemistry, etc., can solve the problems of difficult operation, cumbersome operation, and high toxicity of solvents, and achieve The effect of reducing the difficulty of the process, improving the economic efficiency and reducing the workload

Active Publication Date: 2019-08-02
安徽工业大学科技园有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Ethylenediamine is extremely water-soluble, and its boiling point is close to that of water. During the distillation process, water and ethylenediamine will azeotrope, so it is impossible to separate ethylenediamine and water by means of distillation.
Regarding the reuse of ethylenediamine hydrochloride, there have been many literature studies, such as sodium methoxide being used as a neutralizing agent to remove HCl, and the generated methanol is easily separated from sodium chloride to obtain a purity of 98%. ethylenediamine, but the cost of sodium methoxide is too high; under the condition of temperature 80±10°C, n-propanol is used as the extractant, and after several extraction operations, the product is rectified, and the product containing sodium chloride and hydrogen is successfully purified The ethylenediamine aqueous solution of sodium oxide, obtains the ethylenediamine of purity 99%, and the main shortcoming of this method is that operation is loaded down with trivial details
Tanaka, etc. used toluene as an entrainer to separate ethylenediamine and water through azeotropic distillation to form toluene, H 2 The O mixture is then phase separated to recover toluene. Although this process can realize the separation of ethylenediamine and water, there are many operating steps and the toxicity of the solvent is high, which reduces the market competitiveness of the technology.
Wang Wei and others used double-tower continuous extraction and rectification to realize the separation of ethylenediamine and water, but the energy consumption is high and the operation is difficult

Method used

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  • Preparation method and product of ethylenediamine
  • Preparation method and product of ethylenediamine
  • Preparation method and product of ethylenediamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1.1 Reagents and instruments

[0037] The test drugs and test equipment used in this embodiment are shown in Table 1 and Table 2.

[0038] Table 1 Experimental drugs

[0039]

[0040] Table 2 Experimental equipment

[0041]

[0042] 1.2 Composition and property analysis of ethylenediamine hydrochloride

[0043] First of all, it is necessary to analyze the approximate content of ethylenediamine in the sample salt, estimate and compare the difference in economic benefits between the finished product ethylenediamine and the sample salt, and provide an economic basis for the entire ethylenediamine hydrochloride reuse project. At the same time, it is necessary to do some property analysis on the sample salt to find the optimum temperature for its dissolution so that it can directly react with solid sodium hydroxide.

[0044] Because ethylenediamine is a dibasic base, the ethylenediamine hydrochloride sample contains C 2 h 8 N 2·HCl and C 2 h 8 N 2 · 2HCl two h...

Embodiment 2

[0095] In Example 1, the highest purity of 97% ethylenediamine was obtained, but this purity ethylenediamine cannot be used in some specific processes, so it is necessary to explore a more efficient dehydration method.

[0096] In this example, 200 g of ethylenediamine with a water content of 16.10% prepared in Example 1 is directly added to the still of the rectification column, the extractant is 600 g of 1,4-butanediol, and the initial value of the reflux ratio is 0.5. Vacuum distillation operation. Record the water output at the top of the tower and the content of ethylenediamine and extractant at different temperatures and time periods as shown in Table 8.

[0097] Table 8 batch distillation experimental data

[0098]

[0099] It can be seen from Table 8 that substances start to be extracted from 65°C after feeding, and between 65°C and 95°C, there is a lot of water and a part of ethylenediamine is extracted at the same time. The process takes 1.5h, and the process is ...

Embodiment 3

[0101] The difference between this example and Example 2 is that the oil bath is heated to 60°C, and the rest of the steps and parameters are the same as in Example 1. The mass of the crude product finally obtained in this example is 75g, and the mass of the crude product ethylene glycol is 75g. The water content is 16.1%, then the yield of ethylenediamine is 75×83.90% / 140×60.86%×100%=73.85%. The crude product of ethylenediamine was dehydrated and purified by batch rectification, and the treatment steps were the same as in Example 1. The purity of the finally obtained ethylenediamine was 97.8%.

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Abstract

The invention discloses a preparation method and a product of ethylenediamine. The preparation method comprises steps as follows: industrial ethylenediamine hydrochloride is utilized as a raw materialand subjected to heating melting, then solid sodium hydroxide is taken as a neutralizer, a waterproof reaction and atmospheric distillation are performed, and ethylenediamine is obtained; the obtained ethylenediamine product is subjected to physical absorption dewatering and / or batch fractionating dewatering by a molecular sieve, anhydrous magnesium sulfate or sodium hydroxide solids for dewatering purification, and purity of the finally prepared product can reach 99%. The operation difficulty of an ethylenediamine recovery process is reduced, economic benefit is increased, and the problem about recovery of ethylenediamine by a factory is solved to a certain degree.

Description

technical field [0001] The invention belongs to the technical field of compound production, and in particular relates to a preparation method of ethylenediamine and a product thereof. Background technique [0002] Ethylenediamine belongs to diamines, and it can form ethylenediamine hydrochloride with hydrochloric acid. Ethylenediamine has a wide range of functions. In many domestic industrial production links, ethylenediamine used as catalyst, stabilizer, curing agent, etc. is usually recovered in the form of ethylenediamine hydrochloride, while industrially recovered ethylenediamine Amine hydrochloride is often sold at a low price, which has a huge price gap with finished ethylenediamine. [0003] Ethylenediamine is extremely water-soluble, and its boiling point is close to that of water. During the distillation process, water and ethylenediamine will azeotrope, so it is impossible to separate ethylenediamine and water by means of distillation. Regarding the reuse of ethy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/10C07C209/68C07C209/84
CPCC07C209/68C07C209/84C07C211/10
Inventor 叶明富夏国威许立信宋丰发沈博文万超贾志刚
Owner 安徽工业大学科技园有限公司
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