Method for preparing anhydrous ethylenediamine from double-amino silane byproduct ethylenediamine dihydrochloride

A technology for the production of ethylenediamine hydrochloride and ethylenediamine hydrochloride, which is applied in the field of producing anhydrous ethylenediamine to achieve the effects of reducing production costs, low moisture content of products, and reducing raw material consumption

Active Publication Date: 2019-08-27
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to: provide a kind of process equipment is simple, the raw material is cheap and easy to obtain, solves the by-product problem of existing diaminosilane, has the characteristics of safety and environmental protection, and the anhydrous

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In the 3-ton rake reactor, first pump in 1 ton of diaminosilane by-product ethylenediamine hydrochloride, 0.8 tons of ethylenediamine solvent, turn on the stirring, the stirring speed is 40 rpm, and then add 0.4 tons of oxidation calcium powder. After feeding the materials, the rake reactor was first heated to 70°C, and the stirring speed was 40 rpm for neutralization reaction for 2 hours, and then the temperature of the kettle was raised to 115°C to continue the heat preservation reaction for 6 hours. After the reaction was completed, the neutralization reaction device was changed to an ordinary distillation device, and distillation was carried out under vacuum at -0.09MPa. The maximum distillation temperature was 160°C, and 1.48 tons of ethylenediamine containing water was obtained. The detected moisture content was 2.4%, and the product yield was 95.2%. Give out 718 kilograms of calcium salt powder mixture.

[0022] Pump 1.48 tons of distilled ethylenediamine with a...

Embodiment 2

[0025] In the 3-ton rake reactor, first pump in 0.92 tons of bisaminosilane by-product ethylenediamine hydrochloride, 0.8 tons of ethylenediamine solvent, turn on the stirring, the stirring speed is 40 rpm, and then add 0.4 tons of oxidation calcium powder. After feeding the materials, the rake reactor was first heated to 80°C, and the stirring speed was 40 rpm for neutralization reaction for 2 hours, and then the temperature of the kettle was raised to 110°C to continue the heat preservation reaction for 6 hours. After the reaction was completed, the neutralization reaction device was changed to an ordinary distillation device, and distillation was carried out under vacuum at -0.1MPa. The maximum distillation temperature was 160°C, and 1.40 tons of ethylenediamine containing water was obtained. The detected moisture content was 2.1%, and the product yield was 93.8%. Give out 712 kilograms of calcium salt powder mixture.

[0026] Pump 1.4 tons of distilled ethylenediamine wit...

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PUM

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Abstract

The invention relates to a method for preparing anhydrous ethylenediamine from double-amino silane byproduct ethylenediamine dihydrochloride, and belongs to the technical field of fine chemical engineering. The method comprises the following steps: using double-amino silane byproduct ethylenediamine dihydrochloride and calcium oxide powder, under the condition that an ethanediamine solvent exists,stirring at the temperature of 80 to 115 DEG C for a neutralization reaction, directly distilling after the reaction is completed to obtain water-containing ethanediamine with the water content of 2%to 3%, then adding calcium oxide powder into the water-containing ethanediamine under the effect of a catalyst, stirring at the temperature of 100 to 115 DEG C for a dehydration reaction, and then distilling to obtain anhydrous ethanediamine with the water content of smaller than 0.2%. The equipment technology is simple, the raw materials are cheap and easy to get, the method is safe and environmentally-friendly, the product quality is high, the product is low in water content, the product can be used as a raw material directly, the economic benefit is improved, and the method is applicable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing anhydrous ethylenediamine from bisaminosilane by-product ethylenediamine hydrochloride, belonging to the technical field of fine chemicals. Background technique [0002] Diaminosilane is an important industrial additive, it can be used to couple organic polymers and inorganic substances, used as glass fiber finishing agent, used as crosslinking agent and curing agent for silicone rubber and silicone resin, used as It can be used as textile finishing agent, coating additive, amino-modified silicone oil, etc., with an annual global output of more than 200,000 tons, and its representative products are N-(β-aminoethyl)-3-aminopropyltrimethoxy Silane (KH-792) and N-(β-aminoethyl)-3-aminopropylmethyldimethoxysilane (KH-602), these two products accounted for 90% of the total bisaminosilane production above. The industrial synthesis methods of diaminosilane are all prepared by using ethylenediamine and chlorohy...

Claims

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Application Information

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IPC IPC(8): C07C209/00C07C209/84C07C211/10C07F7/18
CPCC07C209/00C07C209/84C07F7/1892C07F7/1804C07C211/10
Inventor 胡江华罗晗晗甘俊甘书官陈圣云
Owner JINGZHOU JIANGHAN FINE CHEM
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