Preparation method of 1,2-propane diamine

A technology for the preparation of propylenediamine, which is applied in the field 1, can solve problems such as expensive raw material costs, high pressure, and outdated processes, and achieve the effects of reducing investment and production efficiency, no pollution discharge, and simplifying process steps

Inactive Publication Date: 2013-04-03
张家港市大伟助剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Mainly imported by foreign companies such as BASF, the price is expensive
At present, the market demand for 1,2-propanediamine in the Chinese market is 1000-2000 tons per year, but there are few manufacturers in China. The technology is backward and the product quality is not high. At present, the traditional art is to use 1,2-diamine Chloropropane ammonolysis production, the method yield is low, and organic chlorine compounds seriously pollute the environment
It is also reported that acrylonitrile method is useful abroad for synthesis, but this method has high pressure and expensive raw material cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add 112.99g (1.0mol) 1,2-dichloropropane, 225mL water, 102.24g (169.5mL, 6.0mol) liquid ammonia, 22.5g CuO-Co 2 o 3 / Al 2 o 3 - Diatom catalyst, heat up to 160~180°C, pressure 8MPa-12MPa, and maintain this condition for 4~5h; sampling GC detection, 1,2-dichloropropane reaction is complete, the reaction system is cooled to 20~25°C, discharge Excessive ammonia gas produced a mixture of 1,2-propanediamine as the main component, and then obtained 66.19g of the product through rectification, with a yield of 89.3%;

Embodiment 2

[0016] Add 112.99g (1.0mol) 1,2-dichloropropane, 22.60mL water, 136.32g (226mL, 8.0mol) liquid ammonia, 10.0g CuO-Co 2 o 3 / Al 2 o 3 - Diatom catalyst, heat up to 175~180°C, pressure 8MPa-12MPa, and keep this condition for 4~5h; sampling GC detection, 1,2-dichloropropane reaction is complete, the reaction system is cooled to 20~25°C, discharge Excessive ammonia gas produced a mixture of 1,2-propanediamine as the main component, and then obtained 64.86g of the product through rectification, with a yield of 87.5%.

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PUM

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Abstract

The invention discloses a preparation method of 1,2-propane diamine, which comprises the following steps of: adding 1,2-dichloropropane, water, liquid ammonia and a catalyst in a high-pressure reactor, raising the temperature to 160-180 DEG C and the pressure to 8-12MPa, and keeping the conditions for reacting for 4-5h; and sampling for carrying out GC (Gas Chromatograph) detection, completely reacting the 1,2-dichloropropane, cooling a reaction system to 20-25 DEG C, discharging excessive ammonia gas, preparing a mixture using the 1,2-propane diamine as a main component, and rectifying the 1,2-propane diamine to obtain a finished product. According to the preparation method, the process steps are greatly simplified, pollution emission does not exist basically, and the cost is lowered. Excessive ammonia after the reaction is ended can be recycled, and the preparation process can be completed in one high-pressure reactor, so that the investment and production efficiency of equipment are greatly reduced. According to the invention, complete reaction can be completed by adopting one catalyst, and low distillates obtained after rectification can be used as raw materials for recycling, so that the selectivity of the 1,2-propane diamine is greatly increased.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of 1,2-propanediamine. Background technique [0002] 1,2-Propylenediamine (DAP) is an important fine chemical intermediate, widely used in the fields of organic synthesis, medicine, dyestuff, pesticide, chemical additives, rubber plastic additives and epoxy resin curing agent, etc. . Compared with ethylenediamine, DAP has good oil solubility and can be used as an oil passivator. After splitting DAP, dextro-DAP can be obtained, and then propylimine (dex-rotatory dexrazoxane) can be synthesized. In the production of spandex elastic fibers, DAP can be used as a chain extender. DAP can also be used to prepare anionic surfactants. [0003] The market demand for this product is increasing year by year. It is mainly imported by foreign companies such as BASF, and the price is expensive. At present, the market demand for 1,2-propanediamine in the Ch...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/11C07C209/08
Inventor 龚卫良黄德周
Owner 张家港市大伟助剂有限公司
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