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Preparation method of diethylene triamine

A technology of diethylenetriamine and iminodiacetonitrile, applied in the chemical industry, can solve the problems of difficulty in obtaining high-quality diethylenetriamine, serious equipment corrosion, increase in equipment cost, etc., so as to avoid fluctuation of product components and three wastes. Low emissions, ensuring the effect of process control

Inactive Publication Date: 2014-11-05
CHONGQING HAIZHOU CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the wide distribution of components and the difficulty of separation, it is difficult to obtain high-quality diethylenetriamine by this method
In addition, due to the cumbersome process, a large amount of sodium chloride wastewater is produced during the production process, the equipment is severely corroded, and the environmental pollution is worrying.
In contrast, the ethanolamine method has less environmental pollution and higher value-added by-products, but due to the high pressure used, the cost of the device has increased significantly

Method used

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  • Preparation method of diethylene triamine

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Using iminodiacetonitrile and hydrogen as raw materials, liquid ammonia as a solvent, and Pd / C as a catalyst, diethylenetriamine was synthesized as follows:

[0029] (1) Add 7kg of liquid ammonia and 500g of iminodiacetonitrile into a 10L stainless steel autoclave, turn on magnetic stirring, and then add 20g of supported Pd / C catalyst after the iminodiacetonitrile is dissolved;

[0030] (2) Pass nitrogen into the kettle to replace the air until the oxygen content reaches below 0.5%, and then replace the nitrogen with hydrogen;

[0031] (3) Heating the materials in the kettle, the temperature in the kettle is 100°C, the pressure is 12MPa, and the hydrogen gas is passed in, and the ventilation rate is about 220Nm 3 / h, half an hour after the hydrogen is no longer absorbed is the end point of the reaction, and the reaction material is obtained;

[0032] (4) The reaction material is input into a sedimentation separator for separation, and the separated catalyst is recycled...

Embodiment 2

[0036] Using iminodiacetonitrile and hydrogen as raw materials, ammonia as a solvent, and Pt / C as a catalyst, synthesize diethylenetriamine as follows:

[0037] (1) Add 8 kg of ammonia water to a 10L stainless steel autoclave, start magnetic stirring, then add 450 g of iminodiacetonitrile, and then add 20 g of supported Pt / C catalyst after the iminodiacetonitrile is dissolved;

[0038] (2) In the kettle, first feed nitrogen to replace the air, then replace the nitrogen with hydrogen;

[0039] (3) Heat the material in the kettle, the temperature in the kettle is 140°C, and the hydrogen gas is fed under the condition of 8MPa, and the ventilation rate is 230Nm 3 / h, half an hour after the hydrogen is no longer absorbed is the end point of the reaction, and the reaction material is obtained;

[0040] (4) The reaction material is input into a sedimentation separator for separation, and the separated catalyst is recycled after regeneration, and the sedimentation liquid is desolvate...

Embodiment 3

[0044] Using iminodiacetonitrile and hydrogen as raw materials, ammonia as a solvent, and Pt-Pd / C as a catalyst, synthesize diethylenetriamine as follows:

[0045] (1) Add 7kg of solvent to a 10L stainless steel autoclave, turn on magnetic stirring, then add 500g of iminodiacetonitrile, and then add 24g of catalyst;

[0046] (2) feed nitrogen in the kettle to replace the air, then replace the nitrogen with hydrogen;

[0047] (3) Heating the materials in the kettle, the temperature in the kettle is 120°C, the pressure is 12MPa, and the hydrogen gas is passed into it, and the ventilation rate is 220Nm 3 / h, stop feeding half an hour after the hydrogen is no longer absorbed, to obtain the reaction material;

[0048] (4) The reaction material is input into a sedimentation separator for separation, and the separated catalyst is recycled after regeneration, and the sedimentation liquid is desolvated from the normal pressure tower to obtain a crude product;

[0049] (5) Send the cr...

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Abstract

The invention discloses a preparation method of diethylene triamine. The preparation method comprises the following steps: adding liquid ammonia or ammonia water, iminodiacetonitrile and a hydrogenation catalyst into a reaction kettle, uniformly mixing the materials, introducing nitrogen into the reaction kettle for replacing air in the reaction kettle, heating the reaction kettle, controlling the temperature and the pressure of the reaction kettle at 100-140 DEG C and at 8-12MPa respectively, introducing hydrogen, and stopping the introduction of the hydrogen half an hour after the hydrogen is not absorbed to obtain a reaction material; separating the obtained material in a sedimentation separator, collecting sedimentation liquid, removing a solvent from the sedimentation liquid to obtain crude diethylenetriamine; and rectifying the crude diethylenetriamine under the condition that the temperature is 180-190 DEG C and the vacuum degree is between -0.085MPa and -0.095MPa to obtain fine diethylenetriamine. The method is simple in process, and can be applied to industrial production of the diethylenetriamine. The composition profile of the product is simple, and the purity of the product is high and can be over 90 percent. Moreover, a small number of three wastes are discharged, so that environmental pollution can be lowered.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of diethylenetriamine. Background technique [0002] Diethylene triamine is mainly used for synthesizing polyamide resin, surfactant, lubricant, epoxy resin curing agent, etc., and the existing technology is mainly produced by dichloroethane ammoniation method or ethanolamine method. The products synthesized by dichloroethane ammoniation method are mainly mixtures of ethylenediamine, diethylenetriamine, triethylenetetramine, tetraethylenepentamine, pentaethylenehexamine, etc., of which ethylenediamine accounts for 55%, and diethylene Triamine accounts for 23%, triethylenetetramine accounts for 10%, tetraethylenepentamine accounts for 4%, and the remainder is other components. Due to the wide distribution of components and the difficulty of separation, it is difficult to obtain high-quality diethylenetriamine by this method. In addition...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/14C07C209/48
CPCY02P20/584
Inventor 郭汝轩
Owner CHONGQING HAIZHOU CHEM