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A kind of method for preparing anhydrous ethylenediamine from bisaminosilane by-product ethylenediamine hydrochloride

A technology for the production of ethylenediamine hydrochloride and ethylenediamine hydrochloride, which is applied in the field of producing anhydrous ethylenediamine, and achieves the effects of simple equipment and process, reduced production costs, and low moisture content in products

Active Publication Date: 2022-03-04
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 ethylenediamine produced can be directly used in The production of bisaminosilane reduces the consumption of raw materials, thereby improving the economic efficiency of the method for preparing anhydrous ethylenediamine from bisaminosilane by-product ethylenediamine hydrochloride

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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Abstract

The invention relates to a method for preparing anhydrous ethylenediamine from bisaminosilane by-product ethylenediamine hydrochloride, belonging to the technical field of fine chemicals. In the present invention, ethylenediamine hydrochloride and calcium oxide powder, the by-products of bisaminosilane, are stirred and neutralized at 80-115°C in the presence of ethylenediamine solvent, and directly distilled after the reaction to obtain a moisture content of 2%~ 3% water-containing ethylenediamine, then add water-containing ethylenediamine to calcium oxide powder under the action of a catalyst, stir and dehydrate at 100~115°C, and then distill to obtain anhydrous ethylenediamine with a moisture content of less than 0.2%. The invention has the advantages of simple equipment process, cheap and easy-to-obtain raw materials, safety and environmental protection, high product quality and low moisture content, can be directly used as raw materials, improves economic benefits, and is suitable 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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Patent Type & Authority Patents(China)
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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